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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a connection element for connecting mounting rails.
[0003] 2. Description of the Prior Art
[0004] Connection elements for connecting mounting rails found a particular application in the pipe suspending systems. In order to suspend a pipe from a ceiling so that the pipe occupies a predetermined position, the mounting rails have to be connected with each other with sufficient flexibility. For flexibly connecting mounting rails with each other conventionally rail nuts with angles are used. An angle or angle element has a plurality of connection openings for attachment to a mounting rail at a predetermined position.
[0005] A drawback of using angle elements consists in that different angle elements need to be used for attachment of two or more rails at attachment point in different attachment positions. Therefore, a large number of different angle elements is required. This is associated with substantial expenses and a need in a large storage space. This is because a large number of angle elements should be stocked. Furthermore, the necessity to use different angle elements for attachment of mounting rails in different positions limits the mounting flexibility at a site when, e.g., a suspension system requires an angle element or a bend other than originally planned.
[0006] Accordingly, an object of the present invention is to provide a connection element for mounting rails suitable for different applications and which can be economically produced.
SUMMARY OF THE INVENTION
[0007] This and other objects of the present invention, which will become apparent hereinafter, are achieved by providing a connection element for at least two mounting rails and including a base member at least one attachment member having at least one connection opening, and connection means for reasleasably connecting the attachment member with the base member.
[0008] Because the connection element is formed as a modular element, a small number of parts is sufficient for forming a plurality of different connections. The base member is so formed that one or more attachment members can be secured thereto with the connection means. The connection means is formed as releasable means, permitting a correction of a position of the attachment member relative to the base member. The connection means, according to the present invention, significantly facilitate handling of the inventive connection element. This is because the positions of the members are predetermined. The connection means prevents rotation of the connected members relative to each other in their locked position. The manufacturing of the connection elements is significantly simplified in comparison with the prior art because instead of a number of different angle elements, only two parts for a connection element that provides for a plurality of different positions of the mounting rails should be produced. Storage is also significantly simplified. The invention connection element provides for more flexibility on a site.
[0009] According to the present invention, to facilitate the assembly of the connection element, the connection means includes a plurality of openings formed in the base or attachment member, a plurality of pegs provided on another of the base and attachment members and engaging in respective openings, and thread elements for fixedly connecting the base and attachment members together.
[0010] The openings in one of the member and the pegs on another member can be formed simply and economically. The number of openings and pegs determines the number of possible positions. The greater is the number the more positions of the attachment member relative to the base member can be obtained.
[0011] According to an advantageous embodiment of the present invention, the openings are formed in the base member, and there are provided at least four openings symmetrically arranged about a bore formed in the base member for receiving a thread element, e.g., a screw or a bolt. The pegs are provided on the attachment member and include at least four pegs symmetrically arranged about a bore formed in the attachment member through which the thread element extends. With the above-described embodiment, there are provided four positions of the attachment member relative to the base member offset relative to each other by 90°. The central arrangement of the bore for the locking element of the connection means insures a uniform engagement of the pegs in respective openings and a uniform distribution of a load in the connection means. The bores are formed transverse to a longitudinal extent of the respective members, providing for a number of positions of the attachment and base members relative to each other.
[0012] Advantageously, the base member has two side walls and a connection or bottom wall that connects two side wall, whereby a U-shaped profile is formed. The U-shaped profile insures an easy manufacture of the base member and its reliable attachment on mounting rail, without a possibility of rotation relative thereto.
[0013] According to the present invention, the base member is provided, on one of its end surfaces, with a web and, on another of its end surfaces, with a pocket complementary to the web. The webs and the pockets insure that a row of base members can be formed by connection of several base members with each other, with the web of one base member engaging in the pocket of another base member.
[0014] Advantageously, the central bore formed in the base member has an inner thread which forms part of the thread means that provides for a fixed connection between the attachment and base members. Naturally, the inner thread can be provided in the central bore of the attachment member. However, from the economical point of view, it is preferable to provide the bore of the base member with the inner thread as, generally, a greater number of attachment members than of base members is produced.
[0015] According to a particularly advantageous embodiment of the present invention, the attachment member is formed of mutually perpendicular attachment plate and a connection plate. The connection opening is formed in the attachment plate and the pegs are provided on the connection plate.
[0016] Preferably, the connection plate is formed as a square plate, with the bore being formed in the center of the plate, and with the length of a side of the plate corresponding somewhat to the height of a mounting rail. This shape of the connection plate insures that it can be easily secured to the base member in any of four, offset relative to each other by 90°, positions. While, preferably, the angle between the connection and attachment plates is a right angle, it can be arbitrary changed, dependent on the requirements to a particular connection element. For some applications, it may be advantageous to form the connection plate as a circular plate.
[0017] According to the present invention, preferably, the side wall of the base member is formed as a rectangular wall having a width corresponding to a double of a height of an attachable mounting rail and to a double of distance between the side walls. This insures that the connection element can be used for connecting two mounting rails, with the rail openings facing each other or facing away from each other.
[0018] An economic manufacturing is insured when the attachment and base members are formed as stamped bent parts.
[0019] The novel features of the present invention, which are considered as characteristic for the invention, are set forth in the appended claims. The invention itself, however, both as to is construction and its mode of operation, together with additional advantages and objects thereof, will be best understood from the following detailed description of preferred embodiments, when read with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] The drawings show:
[0021] [0021]FIG. 1 a perspective view of a connection element according to the present invention;
[0022] [0022]FIG. 2 a perspective view, at an increased scale, of a base member of the connection element shown in FIG. 1;
[0023] [0023]FIG. 3 a perspective view, at an increased scale, of an attachment member of the connection element shown in FIG. 1;
[0024] [0024]FIG. 4 a perspective view, at an increased scale, of the connection element shown in FIG. 1;
[0025] [0025]FIG. 5 a perspective view of the connection element shown in FIG. 4, with the attachment member being pivoted by 90°;
[0026] [0026]FIG. 6 a perspective view is illustrated one of the applications of a connection element according to the present;
[0027] [0027]FIG. 7 a perspective view showing a mounting rail with a plurality of base members of connection element according to the present invention;
[0028] [0028]FIG. 8 a perspective view showing a connection element according to the present invention with a mounting rail passing therethrough;
[0029] [0029]FIG. 9 a perspective view showing mounting of the attachment member of a connection element according to the present invention at an end of a mounting rail;
[0030] [0030]FIG. 10 a perspective view of another embodiment of a connection element according to the present invention;
[0031] [0031]FIG. 11 a perspective view of the connection element shown in FIG. 10, but with the mounting rail being pivoted 90°;
[0032] [0032]FIG. 12 a perspective view illustrating a possible use of the attachment member a connection element according to the present invention; and
[0033] [0033]FIG. 13 a perspective view similar to that of FIG. 12 with two cross-braces.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0034] A connection element according to the present invention for connecting two mounting rails 1 and 2 , which is shown in FIGS. 1 - 6 , is designated generally with a reference numeral 3 . The connection element 3 has a base member 4 and the attachment member 5 . Each of the connection member 4 and the attachment member 5 has at least one connection opening 6 for attachment of the respective members 4 and 5 to corresponding mounting rails 1 and 2 . The attachment member 5 is releasably connected with the base member 4 by connection means 7 , as it is particularly shown in FIG. 1.
[0035] The connection means 7 includes a plurality of openings 8 , which are provided in one of the members 4 and 5 , and a plurality of pegs 9 which are provided on another of the members 4 and 5 and which cooperate with the opening 8 for connecting the two members 4 and 5 together. The connection means 7 further includes thread means 10 for fixedly securing the base member 4 and the attachment member 5 together.
[0036] In the embodiment shown in FIGS. 1 - 6 , the base member 4 has four openings 8 symmetrically arranged about a bore 11 for a bolt or a screw that forms part of the thread means 10 . The attachment member 5 has four pegs 9 which are symmetrically arranged about a bore 12 and which engage in respective openings 8 as it is shown in FIGS. 4 and 5. The base member 4 has two, extending parallel to each other walls 13 and a bottom or connection wall 14 , forming together a U-shaped profile. Each of the parallel walls 13 and the connection wall 14 has, a one of its free end surfaces, a web 15 and has, at another of its free end surfaces, a pocket 16 complementary to the web 15 . The webs 15 and pockets 16 provide for a formlocking connection of a plurality of a base members 4 with each other, as it is shown in FIG. 6. Each of the walls 13 and 14 has the connection opening 6 and an element of the connection means 7 . The thread means 10 includes a screw with a polygonal head 17 . The screw cooperates with an inner thread 19 provided in the bore 11 for securing the attachment member 5 to the base member 4 .
[0037] The attachment member 5 has an attachment plate 21 and a connection plate 22 extending transverse to the attachment plate 21 . The connection opening 6 is formed in the attachment plate 21 . The pegs 9 of the connection means 7 are provided on the connection plate 22 .
[0038] As it is particularly shown in FIGS. 4 and 5, the base member 4 and the attachment member 5 can be pivoted relative to each other in their non-connected position. In the embodiment of FIGS. 1 - 6 , the base member 4 and the attachment member 5 have four connection positions displaced by 90° to each other. Naturally instead of being attached to the connection wall 14 as it is shown in FIGS. 4 - 5 , the attachment member 5 can be secured to one of the parallel walls 13 . Further, several attachment member 5 can be secured to the base member 4 .
[0039] [0039]FIG. 6 illustrates one of possible applications of a connection element according to the present invention. Each of the mounting rails 1 and 2 has a mounting opening 24 and are so arranged relative to each other that the mounting openings 24 face in opposite directions. Two base members 4 and 20 are formlockingly connected with each other, with the web 15 of the base member 4 engaging in the pocket 16 of the base member 20 . Two attachment members 5 are secured to respective connection walls of the base members 4 and 20 with respective connection means 7 . The attachment members 5 are secured to the mounting rails 1 , 2 with respective rail nuts (not shown). The bottom 26 , 27 of the rails 1 , 2 about each other. To insure an appropriate mounting, the width (t) of the connection wall of the base member 5 should be equal to a double height (h) of the mounting rails 1 and 2 and be twice of the distance (a) between the parallel walls 13 of the base member 4 , 20 .
[0040] [0040]FIG. 7 shows a plurality of base members 4 secured on a mounting rail 1 . The base members 4 are connected to the mounting rail 1 with respective rail nuts 29 , one of which is shown before being inserted in the mounting opening of the base member 4 .
[0041] For using the connection element according to the present invention with a passing-through rail, two attachment members 31 , 32 are secured to a mounting rail 30 at a distance from each which corresponds to the width of a base member 34 , as shown in FIG. 8. A further mounting rail 33 extends through the base member 34 . The attachment members 31 , 32 are secured to the parallel walls of the base member 34 with respective connection means 35 , 36 .
[0042] [0042]FIG. 9 illustrates another possibility of using an attachment member. In FIG. 9, an attachment member 37 is secured at the end of a mounting rail 38 . The attachment member 37 is secured to the rail 38 with a rail nut (not shown) extendable through the connection openings 39 .
[0043] The parts, which are shown in FIGS. 1 - 9 , are formed of sheet metal as stamped bent parts.
[0044] FIGS. 10 - 13 shown another embodiment of an attachment member and its possible use. The shown attachment member 40 has, contrary to the attachment member 5 shown in FIG. 3, at least one bore 44 with an inner thread 45 and formed in a connection web 41 that connects mutually perpendicular connection plate 42 with attachment plate 43 . The base member 46 connects the attachment member 40 with a mounting rail 47 . The base member 46 has a side wall 48 with a connection opening 49 and a bore 50 with an inner thread 51 . In order to be able to mount a second mounting rail 42 pivoted with respect to the first mounting 47 by 90°, as it is shown in FIG. 11, the side wall 48 of the base member 46 should lie in the same plane in which the connection web 41 of the attachment member 46 lies. At least the second mounting rail 52 has a plurality of elongate openings 53 equidistantly spaced from each other. The openings 53 are formed in the bottom 54 of the second mounting rail 52 . The length of the elongate openings 53 should be so selected that each opening 53 encompasses both bores 44 and 45 formed in the connection web 41 of the attachment member 40 and the side wall 48 of the base member 46 , respectively. For the sake of clarity, the connecting screw means is not shown.
[0045] FIGS. 12 - 13 illustrate a further application of the attachment member 40 as an attachment point for cross-braces designated generally with a reference numeral 61 . The cross-brace 61 has a base plate 63 with two connection brackets 64 , 65 provided at opposite longitudinal ends of the plate 63 . The connection bracket 64 , which is secured to the attachment member 40 , has a bore 66 for receiving a screw 67 . The opposite bracket 65 has a guide bore 68 for receiving an end of a brace bar 69 . At its receivable end, the brace bar 69 has an engaging peg 70 the diameter of which is slightly larger than the diameter of the bar 69 and which formlockingly engages from behind in the guide bore 68 . For insertion of the peg 70 in the guide bore 68 , the base plate 63 of the brace 61 has an insertion opening 71 interconnected with the guide bore 68 . A cross-brace 61 serves for receiving tension load acting within an installation system formed, e.g., by a plurality of mounting rails, e.g., rails 47 and 52 .
[0046] Though the present invention was shown and described with references to the preferred embodiments, such are merely illustrative of the present invention and are not to be construed as a limitation thereof, and various modifications of the present invention will be apparent to those skilled in the art. It is, therefore, not intended that the present invention be limited to the disclosed embodiments or details thereof, and the present invention includes all variations and/or alternative embodiments within the spirit and scope of the present invention as defined by the appended claims.
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A connection element for at least two mounting rails ( 1, 2, 30, 33, 38 ) and including a base member ( 4, 20, 28, 34 ) at least one attachment member having at least one connection opening ( 6, 39 ), and connection elements ( 7, 35, 36 ) for reasonably connecting the attachment member ( 5, 25, 31, 32, 37 ) with the base member ( 4, 20, 28, 34 ).
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BACKGROUND
The invention pertains to the attribution to and effectiveness of single known data points and their effect on other single, but unknown data points, in a massive secondary, tertiary or higher linked system. One example of this is the attribution to and effectiveness of public relations or other marketing events on revenue. It is commonly accepted that public reputation and consumer awareness are key drivers of corporate revenue and brand value. However, the effects of particular public relation or marketing events on the reputation or public awareness of a firm or product is difficult to attribute quantitatively.
Traditionally, public relations and marketing professionals analyze paper or electronic sources to determine what effect, if any, their efforts to drive company reputation and consumer awareness through the media can have any measurable effect. And any subsequent measured effects deduced have been limited to a narrow set of metrics such as share-of-voice, number of impressions, etc. No further conclusions have been made to quantitatively link these already limited set of metrics and its effect on sales or revenue—the ultimate measure of corporate health.
Whereas earlier ages were hampered by the lack of paper sources, current analysts may be overwhelmed by the amount of data that are electronically available through search engines or third-party aggregated press databases. This information overload has made it harder, rather than easier to determine the cause and effect of public relations and marketing efforts and the effect of reputation and consumer awareness campaigns have in driving corporate revenue. Further, current methods of measuring PR and marketing performance have been limited to efficiencies on a per-impression acquisition or per-campaign basis. For example, cost per impression or cost per click through various media channels. A company with a far larger market share (or indeed PR and advertising budget) will naturally have wider media exposure than a smaller competitor, yet this in itself does not quantitatively indicate how effectively the available resources to impart consumer awareness in the media are being utilized as contributor to corporate revenue. There is a need, fulfilled by this invention, to resolve this massive data dump into coherent, graphical results.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a method to use statistical modeling to establish discovery, trending and predictive relationships between any data sets.
It is an object of the present invention to provide a method of performance measurement for public relations and marketing events.
It is an object of the present invention to provide a method for consolidating information regarding events for evaluation of corporate key performance relevance from public relations and marketing events.
It is an object of the present invention to provide a method to integrate and compare on an equivalent basis the effectiveness of a variety of public relations events and marketing levers.
It is a further object of the present invention to provide a method of evaluating multiple external events to determine their public relations and marketing efforts with revenue significance.
It is a further object of the present invention to provide a relationship between data sets working from a finish-to-start methodology (Finish Line Approach) to determine the relationship.
It is a further object of the present invention to provide a scalable, Software-as-a-Service (SaaS) solution that uses statistical modeling to establish relationships between any data. The system has the ability to digest any data, establish a mathematic relationship between the data, and identify the actions that the data was measured against to show which has the most quantitative impact on business, and finally, use this information to build a predictive model.
It is a further object of the present invention to provide this information dynamically in real-time.
Thus according to the principles of the invention, there is provided a method of doing business and a system for gathering a plurality of external promotional events having significance to a customer, indexing the external events for an electronic database and abstracting predefined portions thereof for inclusion in the database, evaluating the influence of each of the external references to the defined customer and generating at least one report summarizing the influence or return that each of the external events has on revenue.
The following describes an exemplary data set from the automotive industry that may be utilized in the present invention. The data set may include, without limitation: (i) media car loans, (ii) story requests, (iii) press/marketing events, (iv) published/advertising content, (v) PR/marketing spend, (vi) key performance indicators such as car sales, and (vii) a custom field. These options may then be combined and packaged to provide a graphical result.
The exemplary data set headers are defined as:
Media Car Loans: Car manufacturers provide automobiles to the media for test drives and pre-release evaluation. Story Requests: Media queries to car manufactures regarding interest to publish stories. Press/Marketing Events: Media or consumer invited to events sponsored by car manufacturers for new product introduction and tests. Published/Advertising Content: Media coverage or advertising on TV, in magazines, on Internet, or in any other emerging media such as social networks. PR/Marketing Spend: The cost associated with PR and marketing levers. Key Performance Indicators (KPI): Important metrics describing the ultimate company goals determined and selected by the software user. Examples: car sales, unit sales, etc. Custom: Placeholder for one or more Key Performance Indicators (KPI) such as share-of-voice, conquests buys, brand awareness or reputation measures common to PR and
Further features and advantages of the invention as well as the structure and operation of the preferred embodiments of the present invention are described in detail below with reference to the accompanying drawings. In the drawings, like numbers indicate identical or functionally similar elements.
BRIEF DESCRIPTION OF THE DRAWINGS
Preferred embodiments of the present invention will now be described, by way of example only, with reference to the accompanying drawings in which:
FIG. 1 is an exemplary block diagram that depicts the structure of the system embodying the present invention.
FIG. 2 is a graphical representation showing the detail of the flow of information in the Modeling Engine operation.
FIG. 3 is an exemplary graphical representation of the flow of information and decision making of the present invention.
FIG. 4 is an exemplary graphical representation of the iterative process in determining the Dynamic Sphere of Influence.
FIG. 5 is a graphical representation showing the Software flow of information from a User standpoint.
FIG. 6 is an exemplary graphical representation that depicts the results of the present invention's analysis of the relationship between several external variables and revenue.
DETAILED DESCRIPTION OF THE INVENTION
With respect to FIG. 1 , system 100 of the present invention is utilized as follows: a query is sent via a User Interface 102 using the Graphical User Interface (GUI) module 104 for input. Relevant information from one or more of a plurality of databases 106 a , 106 b , 106 c and 106 d , containing one or more data strings, 107 a , 107 b , 107 c , 107 d , will be assessed and collected through a Data Ingestion Module 108 . This information, along with information from the existing database 110 is sorted in the Indexing Engine 112 and forwarded to the Data Query Engine 114 . The data is then sent to the Quantitative Analysis Method Module 120 , specifically to the Data Input/Choose Analysis 122 . Based on the analysis chosen, information is fed to the Discovery Modeling Engine 124 the Trending Modeling Engine 126 and Predictive Modeling Engine 128 . The Discovery Modeling Engine 124 , Trending Modeling Engine 126 and Predictive Modeling Engine 128 can request more data (new or updated) from the Data Input/Choose Analysis 122 . Alternatively, data from the Discovery Modeling Engine 124 can be sent to Trending Modeling Engine 126 , and to Predictive Modeling Engine 128 if complete analysis utilizing all Modeling Engines is desired. Data from the Modeling Engines 124 , 126 and 128 may then go directly to Test Significance 130 . If the result of Test Significance 130 is No, Data Input/Choose Analysis 122 is repeated. If the result of Test Significance 130 is Yes, information is fed into the Decision Engine 132 , and results are may be forwarded to the Dashboard 134 for display, and/or to Actions Items 136 for additional analysis or to obtain additional required information. The information may then be graphically represented through the Visualization module 138 , and fed through the GUI Output 140 back to the User Interface 102 .
With respect to FIG. 2 , the Modeling Engine System 200 , is shown in detail. The Modeling Engine system comprises a Data Input/Choose Analysis module 122 . Based on user selection, Data Input/Choose Analysis 122 transfers data to Discovery Math Modeling 124 , Trending Math Modeling 126 , or Predictive Math Modeling 128 .
When Data is fed into Discovery Math Modeling 124 , Pattern Statistical Engine 222 performs pattern recognition calculations. Analysis executed here may include existing pattern recognition math techniques, but not limited to descriptive statistics, correlation, time series, etc. If any there are no desired patterns within, or between the data at the Patterns of Interest module 224 , the data is examined again, looping back to Data Input/Choose Analysis 122 for additional or updated data. If Pattern of Interest 224 is detected, information is forwarded to Trending Math Modeling 126 for next step of analysis, or can be sent to Test Significance 130 .
When Data is fed into Trending Math Modeling 126 , Trending Statistical Engine 242 performs comparative calculations. Analysis executed here may include existing comparative math techniques, but not limited to correlation, principle component, cluster, boot-strapping, etc. If any there are no desired relationships within, or between the data at the Data Relationship module 244 , the data is examined again, looping back to Data Input/Choose Analysis 122 for additional or updated data. If Data Relationship 224 is detected, information is forwarded to Predictive Math Modeling 128 for next step of analysis, or can be sent to Test Significance 130 .
When Data is fed into Predictive Math Modeling 128 , Forecasting Statistical Engine 262 performs future projection calculations. Analysis executed here may include existing prediction math techniques, but not limited to regression, discriminate functions, etc. If any there are no predictive models established within, or between the data at the Data Forecasting module 264 , the data is examined again, looping back to Data Input/Choose Analysis 122 for additional or updated data. If Data Forecasting 264 is established, information is forwarded to Test Significance 130 .
With respect to FIG. 3 , a graphical representation of the “Finish-Line Approach” system 300 of the present invention is exemplified. Taken Data Input from outside of system 300 , and/or the Customer Defined KPI (Key Performance Indicator) (End Goal) 302 is selected. The KPI is used as a Benchmark/Filter for Data Analysis 304 . The data set or sets are then entered into the Quantitative Analysis module 120 along with Upstream Measured Data A 306 a , Upstream Measured Data B 306 b , Upstream Measured Data C 306 c , Upstream Measured Data N 306 d . The output of the Quantitative Analysis Method 120 is then analyzed to determine if a Statistical Relationship 308 exists. If No, then More Data and Analysis Needed 310 is flagged and additional Upstream Measured Data 360 a , 306 b , 306 c , 306 d is required. If Yes, then Identified Data Influence on KPI is flagged and the Updated Data Test 314 is considered. Data Input from outside of system 300 can also be fed into Updated Data Test 314 for consideration. If the result of Updated Data Test 314 is Yes, More Data and Analysis 310 is flagged. If Updated Data Test is No, Data Identified to Drive KPI 318 is confirmed, and the output may be iteratively applied back through the Customer Defined KPI (End Goal) module 302 for continuous improvement, and/or sent as Data Output to outside of system 300 .
With respect to FIG. 4 , a graphical representation of the Sphere of Influence (SOI) Index system 400 is depicted. From Input Data outside of SOI Index System 300 , and/or the user initially identifies Sphere Of Index (SOI) Relevant to a Business Function 402 , that data is entered into Customer Defined KPI (End Goal) 302 within “Finish-Line Approach” system 300 . If Data Identified to Drive KPI 318 is detected, the result is used to Define the Number of Influence Data in the SOI Index 404 . The data is then analyzed to determine the Weighting of Individual Data in SOI Index 406 . A check is made to determine if there Real-Time Update SOI 408 is needed. If Yes, the data is checked for Updated Data Test 314 in the “Finish-Line Approach” system 300 . If No, SOI Index Snapshot 410 is created, and can be forwarded to optimize, modify and/or refine SOI Relevant to Business Function 402 , and/or sent as Output Data to outside SOI Index System 300 .
With respect to FIG. 5 , Software User Execution system includes a User Login 502 and an Authentication Module 504 . Upon authentication, the user may Select Data for Analysis 506 . The system may query if the selected data is New Data 508 . If the data is new, the user may choose a Data File/Type/Location 510 , Upload/Parse Data for Database 514 .
If the data is already resident in the database, either one, multiple or combinations of, Quantitative Analysis Method, Finish Line Method or Dynamic Sphere of Index (SOI), may be pursued. In the first, the Quantitative Analysis Method 120 performs Discovery, Trending and Predictive functions on the data. The results may then be sent to Graphical Output 526 for the user to view, and may be saved, transmitted, printed or deleted. The user may also exit the system through the User Logout 528 .
Alternatively, separately, in concert or combination with, to the above data manipulation, may be sent to the Finish Line Method 300 , where the user can define Key Performance Indicators (KPIs)/Benchmarks, test all relevant data, and identify the data are key drivers of the said KPIs/benchmarks. The results may then be sent to Graphical Output 526 for the user to view, and may be saved, transmitted, printed or deleted. The user may also exit the system through the User Logout 528 .
Alternatively, separately, in concert or combination with, to the above data manipulation, may be sent to the Dynamic Sphere of Influence (SOI) Index, where the user can detect, select and customize a Sphere of Influence (SOI) Index that is relevant and complements a specific business goal(s). The results may then be sent to Graphical Output 526 for the user to view, and may be saved, transmitted, printed or deleted. The user may also exit the system through the User Logout 528 .
If the Authentication 504 fails, the user may be prompted to a Sign Up/Password Retrieval module 530 . If the user has an account does not wish to create a new account, they will be sent a Password Recovery Email 534 and returned to the User Login 502 .
If the user wishes to sign up, they may do so and a Sign Up Confirmation Email 538 will be generated and sent to the user, who is then returned to the User Login 502 .
With respect to FIG. 6 , the Output GUI 140 of FIG. 1 may be represented in the manner of the Software Graphical User Interface system screen 600 . Function Bar 610 contains multiple functions that may be selected through an input device, for example, a mouse, a pen, a touch screen or by voice command. One embodiment of the present invention includes a New/Open Analytics tab, a Custom Data tab, Standard Editing Functions, Benchmark Data Configuration, Standard/Favorite Analytic Scenarios, Share/Publish Report and Help Functions. Additional or alternative functions may be configured as necessary or appropriate for different embodiments. A Filter or Search by Keyword Box 612 allows a user to search for particular data, results or other elements of the database by text, keyword or other search strings. Both the Search and Filter function may be contextual, literal or employ Boolean arguments to generate results. Display Tabs 630 allow the user to select the type of analysis that he or she wishes to have displayed.
In one embodiment of the present invention a Trending Analysis tab shows the relationship between several plotted variables in a graphical output display. There are additional Discovery, Predictive and Dashboard tabs also shown. These tabs are exemplary and are not to be considered limiting.
Key Performance Indicators (KPIs)/Benchmarks variables selectable by user, shown as Select KPI Data 642 . Relationship variables are shown as Select Test Data 644 . In one embodiment of the present invention, Sales is chosen as KPI data, Media Car Loan, Consumer Confidence Index (CCI) and Web Traffic are chosen as Test Data. As with the display tabs above, these categories are exemplary and not to be considered limiting. Analysis Date Range 640 allows the user to identify the start and end date for the analysis to be performed.
In the graphical visualization 650 , plots are displayed based on user selection of KPI and Test data. A Time Slider tab 652 is available to scroll chronologically through a display showing the effect of different test data over time against KPI data. A custom View Date range 654 option is also available to display results between a specific start and end date. The types charting presented, line plots, scatter, bar, etc., are exemplary and are not to be considered limiting.
Tables are available to show Discovery Results 660 , Trending Results 662 and Predictive Results 664 corresponding to the types of analysis chosen based on Display Tab 630 . Action Items 670 presents the recommended actions to be taken also based aon the corresponding analysis chosen with Display Tab 630 .
While various embodiments of the disclosed system, software, and method have been described above, it should be understood that they have been presented by way of example only, and should not limit the claimed invention. Likewise, the various diagrams may depict an example architectural or other configuration for the disclosed system, software, and method. This is done to aid in understanding the features and functionality that can be included in the disclosed system, software, and method. The claimed invention is not restricted to the illustrated example architectures or configurations, rather the desired features can be implemented using a variety of alternative architectures and configurations. Indeed, it will be apparent to one of skill in the art how alternative functional, logical or physical partitioning and configurations can be implemented to implement the desired features of the disclosed system, software, and method. Also, a multitude of different constituent module names other than those depicted herein can be applied to the various partitions. Additionally, with regard to flow diagrams, operational descriptions and system or method claims, the order in which the steps are presented herein shall not mandate that various embodiments be implemented to perform the recited functionality in the same order unless the context dictates otherwise.
Although the disclosed system, software, and method is described above in terms of various exemplary embodiments and implementations, it should be understood that the various features, aspects and functionality described in one or more of the individual embodiments are not limited in their applicability to the particular embodiment with which they are described. Thus, the breadth and scope of the claimed invention should not be limited by any of the above-described exemplary embodiments.
Terms and phrases used in this document, and variations thereof, unless otherwise expressly stated, should be construed as open ended as opposed to limiting. As examples of the foregoing: the term “including” should be read as meaning “including, without limitation” or the like; the term “example” is used to provide exemplary instances of the item in discussion, not an exhaustive or limiting list thereof; the terms “a” or “an” should be read as meaning “at least one,” “one or more” or the like; and adjectives such as “conventional,” “traditional,” “normal,” “standard,” “known” and terms of similar meaning should not be construed as limiting the item described to a given time period or to an item available as of a given time, but instead should be read to encompass conventional, traditional, normal, or standard technologies that may be available or known now or at any time in the future. Likewise, where this document refers to technologies that would be apparent or known to one of ordinary skill in the art, such technologies encompass those apparent or known to the skilled artisan now or at any time in the future.
A group of items linked with the conjunction “and” should not be read as requiring that each and every one of those items be present in the grouping, but rather should be read as “and/or” unless expressly stated otherwise. Similarly, a group of items linked with the conjunction “or” should not be read as requiring mutual exclusivity among that group, but rather should also be read as “and/or” unless expressly stated otherwise. Furthermore, although items, elements or components of the disclosed method and apparatus may be described or claimed in the singular, the plural is contemplated to be within the scope thereof unless limitation to the singular is explicitly stated.
The presence of broadening words and phrases such as “one or more,” “at least,” “but not limited to” or other like phrases in some instances shall not be read to mean that the narrower case is intended or required in instances where such broadening phrases may be absent. The use of the term “module” does not imply that the components or functionality described or claimed as part of the module are all configured in a common package. Indeed, any or all of the various components of a module, whether control logic or other components, can be combined in a single package or separately maintained and can further be distributed in multiple groupings or packages or across multiple locations.
Additionally, the various embodiments set forth herein are described in terms of exemplary block diagrams, flow charts and other illustrations. As will become apparent to one of ordinary skill in the art after reading this document, the illustrated embodiments and their various alternatives can be implemented without confinement to the illustrated examples. For example, block diagrams and their accompanying description should not be construed as mandating a particular architecture or configuration.
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A system and method for the identification, analysis, attribution, and graphical display pertaining to the effectiveness of public relations is described. The methodology is based on a massively quantitative approach suitable for numerical processing. This method provides a computer-based means of consolidating both internal and external data and producing a graphical representation of the quantitative results to attribute individual contributions of separate data sources.
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BACKGROUND OF THE INVENTION
The present invention relates generally to a machine for joining two members at a miter joint, a clamping head assembly for use in such a machine, and a method of retrofitting an existing joining machine to include the present clamping head assembly. More particularly, the preferred embodiment of the present invention relates to a frame making machine used for joining two frame members at a miter joint, where the machine includes a clamping head assembly with two fence members, at least one of which is movable, which are used to align the frame members in the proper orientation. The present invention also relates to such a clamping head assembly, as well as to retrofitting a machine that includes a conventional head assembly with the present head assembly. It should be noted that although the preferred embodiments of the present invention will be shown and described as being intended for use in the frame making industry, uses of the present invention in other industries that require members to be joined together at a miter joint are also contemplated as being within the scope of the invention, for example the woodworking industry.
A miter joint is a corner joint formed by fitting two members together at their respective edges, wherein each edge is cut at some angle; the line defined at the joint between the adjacent edges is the miter angle. Conventionally, for adjacent edges cut at the same angle, if the included angle between the two members is 90 degrees, the miter angle will be 45 degrees, and if the included angle is 60 degrees, the miter angle will be 30 degrees. Therefore, a miter angle by definition is an oblique angle.
Machines for joining two frame members at a miter joint are known in the art. One popular machine, which is shown in an exploded view in FIG. 1, is the “Mitre-Mite VN 4 Electronic,” which is manufactured and distributed by Alfamachine-ITW/AMP of Vernon Hills, Ill. The frame making machine 10 includes a work table 12 with a preferably horizontal work surface 14 . Briefly, as known to those of ordinary skill in the art, the machine 10 operates as follows. First, one frame member is aligned along each one of the two fence members ( 22 , 24 ) with a miter joint therebetween. Next, the frontal clamp 18 (optional) moves horizontally in a direction that is generally coincident with the miter joint, and pushes each of the two frame members against its respective fence member ( 22 , 24 ). Third, the vertical clamp ( 20 ) engages the frame members from the top, pushing them downwardly against the work surface 14 . Finally, the two frame members are nailed together at the miter joint by one or more nails (e.g., V-nails, corrugated fasteners or other fasteners) that are driven upwardly into the miter joint from a nail driving mechanism that is seated below the work surface 14 . After the nailing operation, the two frame members (which are now a single unit) can be removed from the machine since they have been joined together at the miter joint.
Since the present invention relates primarily to the methods and apparatuses used to clamp the frame members in place, these features of the prior art machine will be described next in more detail. The machine 10 includes three primary clamping subassemblies: (1) a stationary clamping assembly 16 ; (2) a movable frontal clamp assembly 18 ; and (3) a movable vertical clamp assembly 20 . It should be noted that since these features are known to those of ordinary skill in the art, only the major components of each subassembly will be described below.
The stationary clamping assembly consists primarily of two stationary fence members 22 and 24 that are relatively rigidly affixed to the work surface 14 by a plurality of screws 26 extending through a plurality of associated holes 28 . The holes 28 are in the form of elongated slots to allow for some adjustment of the positioning of the stationary fence members 22 , 24 . Knobs 30 are useful for adjusting the vertical angle of the edge of the fence members to better accommodate and achieve a tight fit between frame members having angled or non-uniform edges. A shown in the FIG. 1 view, the inner (or left) side of each of the stationary fence members defines a positioning edge upon which a respective edge of one of the frame members intended to be joined together is seated against.
The second subassembly, the movable frontal clamp assembly 18 , includes a movable frontal clamp member 32 , which is configured to move within track 34 . The position of the frontal clamp member 32 may be varied by moving the securing knob 36 to another one of the holes 38 . In operation, the movable front clamp member 32 is moved from a first position in which it is drawn backward (toward the left-hand side of FIG. 1) to a second position (toward the right-hand side of FIG. 1) in which it is clamping against the frame members intended to be joined together. The direction of travel of the frontal clamp member 32 is essentially coincident with the miter between the two frame members being joined together.
The third subassembly, the movable vertical clamp assembly 20 , includes a pressure plate 37 that is attached to a rod 39 . The rod 39 is attached to a support structure 40 , which is in turn connected to two cylinders 42 . The cylinders 42 are rigidly affixed to the work surface 14 from below so that the attachment plates 44 are below the work surface 14 and the cylinders 42 extend through holes 45 to be situated above the work surface. If necessary, the horizontal location of the pressure plate 37 may be adjusted by loosening handle 46 , and then sliding the threaded dowel 48 within the slot 50 . The vertical height of the pressure plate 37 may be adjusted by manipulating the other handle 52 . In operation, the cylinders 42 are withdrawn to push the pressure plate 37 downwardly upon the top of the frame members being joined together at the miter joint. In this manner, the frame members are firmly held down when the fastener(s) (e.g., V-nails, corrugated fasteners) are inserted from below.
One common problem with many frame assembly machines of the prior art, such as the one described above, is that the two frame members being joined together may not be properly held together at the miter joint. There may be a slight space between the two frame members at the miter joint prior to nailing. If this is the case, when the frame members are nailed together, there will be an unsightly gap between the two frame members at the joint. That is, the miter joint may be too wide along its entire length, resulting in a visible air space along the entire length of the miter joint, or the miter joint may be uneven, whereby a portion of the joint has a visible air space and another portion is tight with no visible air space. Neither of these two situations is desirable since the intent is to arrive at a tight miter joint with no visible gap between the two frame members.
Accordingly, one object of the present invention is to provide an improved frame assembly machine which is capable of consistently making a tight miter joint.
Another object of the present invention is to provide a clamping head assembly for use with a frame assembly machine whereby the resulting miter joints are tight.
A third object of the present invention is to provide a clamping head assembly for use with a frame machine where the assembly includes at least one movable fence member for properly positioning the frame member within the machine prior to the nailing operation.
A fourth object of the present invention is to provide a clamping head assembly that applies a force to the frame members being joined together at a miter joint, where that force is applied in a direction that is approximately perpendicular to the miter joint.
An additional object of the present invention is to provide a method of retrofitting an improved clamping head assembly upon an existing frame assembly machine.
These and other objects of the present invention are discussed or will be apparent from the following detailed description of the present invention.
BRIEF SUMMARY OF THE INVENTION
The above-listed objects are met or exceeded by the present frame assembly machine, which features a clamping head assembly that provides an additional clamping force for maintaining the frame members in position prior to being joined together at a miter joint, where that additional clamping force is applied in a direction that is approximately perpendicular to the miter joint. In the preferred embodiments, the additional clamping force is realized by providing a movable fence member that cooperates with a stationary fence member to retain the two frame members in the proper position prior to being nailed together.
More specifically, the present invention provides a clamping head assembly for clamping a first member to a second member at a miter joint, where the clamping head assembly includes a first fence member with a first positioning edge for positioning an edge of the first member and a second fence member that is movable and includes a second positioning edge for positioning an edge of the second member. The second positioning edge is arranged at an approximately right angle with respect to the first positioning edge. Additionally, the first fence member and the second fence member are configured and arranged to that the approximately right angle is approximately bisected by the miter joint formed between the first and second members. The second fence member is movable in a direction that is approximately perpendicular to the miter joint, whereby a normal force is generated upon the miter joint. Furthermore, the present invention also relates to a frame making machine that includes the clamping head assembly just described.
Another aspect of the present invention relates to retrofitting an existing frame making machine with an improved clamping head assembly. In particular, the invention relates to a method of retrofitting a frame making machine that originally includes a primary work surface (preferably generally horizontal) and two stationary fence members for positioning first and second frame members intended to be joined together at a miter joint, where the two stationary fence members are seated upon the primary work surface. The first step of the method involves removing at least one of the stationary fence members from the frame making machine. The second step involves installing at least one movable fence member upon the frame making machine, where the movable fence member is capable of being moved in a direction that is generally perpendicular to the miter joint between the first and second frame members.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
Preferred embodiments of the present invention are described herein with reference to the drawings wherein:
FIG. 1 is an exploded view of a prior art frame assembly machine, including a prior art clamping head assembly consisting of two stationary fence members;
FIG. 2 is a top perspective view of the first embodiment of the clamping head assembly of the present invention;
FIG. 3 is schematic view of a second embodiment of the clamping head assembly of the present invention; and
FIG. 4 is a schematic view of a third embodiment of the clamping head assembly of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to FIG. 2, a first embodiment of the present clamping head assembly will be described. It should be noted that features of FIG. 2 that are also found in the prior art device of FIG. 1 will be numbered with the same numbers used in FIG. 1 . It should also be noted that in FIG. 2 a portion of the pressure plate 37 has been cut away to allow for a better view of the components below this plate.
In the FIG. 2 embodiment, the clamping head assembly 52 includes two fence members—a stationary fence member 54 and a movable fence member 56 . The stationary fence member 54 includes a positioning edge 58 for aligning the edge of one of the frame members intended to be joined at a miter joint, and the movable fence member 56 also includes a positioning edge 60 for aligning the other frame member. The stationary fence member 54 is preferably rigidly affixed to the work surface 14 via several bolt and slot arrangements, only one of which is shown. These arrangements each include a bolt, such as bolt 62 , and a slot, such as slot 64 . The elongated slots 64 allow for some adjustment of the position of the stationary fence member 54 .
In this preferred embodiment, the movable fence member 56 is attached to a cylinder rod 66 of a pneumatic cylinder 68 via a pivotable connection 70 made through a block 72 . The block 72 is rigidly affixed to the top of the movable fence member 56 . One end of the cylinder 68 is preferably affixed to a cylinder base 73 such that the cylinder extends horizontally from the base so that the cylinder rod 66 is aligned with the pivotable connection 70 . Instead of using a pneumatic cylinder to move the movable fence member 56 , it is also contemplated that electromechanical means, e.g., electronic, mechanical, pneumatic controls and parts, may be used.
Two guide rods 74 , each of which are slidable between a corresponding guide block 76 , are preferably provided to guide the movable fence member 56 along a straight horizontal path that is perpendicular to the miter joint that will be found between the two frame members being joined together. The guide rods 74 are preferably notched at areas 75 , which is a simple method of affixing them to the raised shoulder 79 of the movable fence member 56 . A stop bar 78 is preferably provided on the ends of both guide rods 74 in order to prevent the rods from extending too far. The guide blocks 76 and the cylinder base 73 are preferably rigidly affixed to a supplemental work surface 77 .
Optionally, additional guidance for the movable fence member 56 may also be provided by a pair of bearings 80 seated within a pair of slots 82 (only one of which are shown). It should be noted that each bearing 80 passes through one of the slots 82 , and is affixed to the work surface 14 , and this bearing/slot combination allows for the movable fence member 56 to slide across the work surface 14 .
Another optional feature of the present invention is the inclusion of a ridge 84 on the stationary fence member 54 . The ridge functions to align the frame members prior to clamping and fastening the members together. The ridge further facilitates the centering of the fastener with respect to the miter joint. A notch 86 may also be included the movable fence member 56 . The notch provides clearance for the moveable fence to move inwardly toward the stationary fence, while applying pressure perpendicularly to the miter joint. This notch/ridge configuration thereby facilitates the formation of the miter joint.
In operation, the steps related to the clamping head assembly of the present invention are simply incorporated into the operating steps of prior art frame making machines. Thus, first the operator sets one frame member against each of the positioning edges 58 and 60 . Next, the movable frontal clamp 32 moves towards the frame members in a direction that is essentially coincident with the miter joint. Third, the cylinder 68 activates to move the movable fence member 56 in the direction of the arrow, creating a force upon the frame members that is approximately perpendicular to the miter joint. Such a force is useful in reducing the size of the gap between frame members at the miter joint. Next, the pressure plate 36 is lowered, creating a downward force upon the frame members. Finally, the frame members are affixed together at the miter joint, for example, by one or more fasteners that are driven upwardly from below the work surface 14 . Accordingly, the two frame members are now affixed together at a miter joint, and can be removed from the machine.
Another important aspect of the present invention is that the present clamping head assembly may be retrofitted to a frame making machine with two stationary fence members, such as that shown and described above while referring to FIG. 1 . The basic retrofitting procedure is as follows. First, one of the stationary fence members, such as fence member 22 of FIG. 1, is removed from the machine. Then, the movable fence member 56 is positioned upon the primary work surface 14 in the appropriate area. The movable fence member 56 preferably includes the block 72 , but the fence member is not connected to the cylinder rod 66 or the guide rods 74 yet. Either before or after the movable fence 56 is installed, a supplemental work surface (such as surface 77 of FIG. 2) is affixed to the machine. Upon the supplemental work surface 77 are seated the components used to move the movable fence member 56 , such as the pneumatic cylinder 68 , the guide blocks 76 , etc. At this point the guide rods 74 are connected to the movable fence member 56 via the notched area 75 and the raised shoulder configuration 79 mentioned above. The cylinder rod 66 is connected as well, via the pivotable connection 70 . The pneumatic tubes 81 are then connected to the cylinder 68 , and the machine is in condition to be operated. If desired, the other stationary fence member (member 24 of FIG. 1) may also be replaced by a fence member with a ridge (such as member 54 of FIG. 2 with ridge 84 ) in order to facilitate the substantial alignment of the frame members prior to clamping and fastening operations.
A second embodiment of the present invention will now be described while referring to the schematic view of the top of the machine shown in FIG. 3 . Once again, like components from FIGS. 1 and 2 will be numbered with the same index numbers in FIG. 3 .
One of the main features of the FIG. 3 embodiment is that the work surface 14 is split into two sections—section 14 A and section 14 B. In this embodiment, the movable fence member 56 is rigidly affixed to work surface section 14 A, and the entire section 14 A of the work surface is configured to move in the direction of the arrow, i.e., in a direction that is approximately perpendicular to the miter joint between the two frame members.
In order to be able to move, the movable section 14 of the work surface is connected to a support structure 88 that is situated below the work surface 14 . The support structure 88 preferably includes four mounting blocks 90 , which are used to mount two rods 92 . A bearing 94 , such as a Thompson bearing, is slidably mounted upon each rod 92 . The tops of the bearings 94 are rigidly connected to the bottom of section 14 A of the work surface. The bearings 94 are preferably connected to each other via a bar 96 , which is connected near a center portion thereof to a cylinder 98 . The cylinder 98 is configured to move the bar 96 in the direction of the arrow, and accordingly also moves the bearings 94 and work surface section 14 A in the same direction, since these components are all rigidly connected to the bar 96 .
In the FIG. 3 embodiment, as well as in the FIG. 2 embodiment, only a slight movement of fence member 56 is required to provide sufficient pressure upon the miter joint. For example, travel of approximately 0.25 inches is sufficient. Since only a minimal amount of movement required, it is also contemplated that section 14 A of the work surface may be hingedly mounted to a mechanism for moving it with respect to the other section (section 14 B). Although movable fence member 56 would then be moved in an arc (instead of perfectly perpendicular to the miter joint as in the embodiments of FIGS. 2 and 3 ), the movement distance is so minimal that it can be considered to be moving in a straight line.
In the FIG. 3 embodiment, the movable vertical clamp assembly 20 , which includes the pressure plate 37 , is preferably configured in a similar manner to that shown in FIG. 1 . However, since section 14 A of the work surface is movable (along with the associated cylinder 42 ), the left side of the horizontal bar 41 of the support structure 40 needs to be connected to the left cylinder 42 with a horizontally slidable connection, such as with a bearing. In the alternative, the components supporting the pressure plate 37 may all be positioned upon the movable section 14 A, in which case a horizontally slidable connection between horizontal bar 41 and the left cylinder 42 is unnecessary.
The FIG. 3 embodiment may also be retrofitted to an existing frame making machine, such as machine 10 shown in FIG. 1 . Basically, the work surface 14 (FIG. 1) is removed from the work table 12 , and is divided into two sections 14 A and 14 B (FIG. 3) along a line that is coincident with the location of the miter joint between the two frame members intended to be joined together. The support structure 88 is installed within the work table 12 , section 14 A of the work surface is seated above the support structure, and the bottom of section 14 A is connected to the tops of bearings 94 . The other section of the work surface, section 14 B, is then reinstalled upon the work table 12 so that it remains stationary with respect to the work table. The fences 54 and 56 may be installed upon their respective sections ( 14 A and 14 B) of the work surface either before or after the work surface is reinstalled upon the table 12 . The movable vertical clamp assembly 20 (FIG. 1) may also be reinstalled upon the appropriate work surface section 14 A (or upon both sections 14 A and 14 B if desired) either before or after the section(s) have been reinstalled upon the table 12 .
Referring now to FIG. 4, a schematic view of the top of the machine of a third embodiment is shown. In this embodiment, both fences 54 and 56 are fixed to the work surface 14 , and the additional pressure is applied by pads 100 . In this schematic, arrows 102 represent cylinders, or other similar pressure means, that apply pressure to the pads 100 in the direction of the arrows. As in the other embodiments, each of the pads 100 apply pressure in a direction that is approximately perpendicular to the miter joint between the two frame members being joined together. In this way, the frame members are moved together to form the miter joint, while being held against the work surface, resulting in a tighter miter joint. Preferably, the cylinders 102 are arranged to apply forces in the vertical direction as well as in the horizontal direction. This combination force can be accomplished by arranging the cylinders 102 at an angle with respect to the work surface 14 . The suggested range for the angle is between 30° and 60°, with 45° being most preferred. This embodiment may also be retrofitted upon an existing machine, such as the machine of FIG. 1 .
While particular embodiments of the clamping head assembly and method of retrofitting a frame making machine to include the assembly have been shown and described, it will be appreciated by those skilled in the art that changes and modifications may be made thereto without departing from the invention in its broader aspects and as set forth in the following claims.
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A clamping head assembly for clamping a first member to a second member at a miter joint, where the clamping head assembly includes a first fence member with a first positioning edge for positioning an edge of the first member and a second fence member that is movable and includes a second positioning edge for positioning an edge of the second member. The second positioning edge is arranged at an angle with respect to the first positioning edge. Additionally, the first fence member and the second fence member are configured and arranged so that the angle is approximately bisected by the miter joint formed between the first and second members. The second fence member is movable in a direction that is approximately perpendicular to the miter joint, whereby a normal force is generated upon the miter joint. Furthermore, the present invention also relates to a frame making machine that includes the clamping head assembly just described.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of and is a continuation-in-part of U.S. Provisional Patent Application Ser. No. 61/069,083 entitled “Spacer instrumentation system with deployment indicator” filed on Mar. 12, 2008 which is incorporated herein by reference in its entirety. This application also claims priority to and is a continuation-in-part of U.S. patent application Ser. No. 12/354,517 entitled “Interspinous spacer” filed on Jan. 15, 2009 which is a non-provisional of U.S. Provisional Patent Application No. 61/011,199 entitled “Interspinous spacer” filed on Jan. 15, 2008 both of which are incorporated by reference herein in their entireties. This application also claims priority to and is a continuation-in-part of U.S. patent application Ser. No. 12/338,793 entitled “Spacer insertion instrument” filed on Dec. 18, 2008, which issued as U.S. Pat. No. 8,613,747 on Dec. 18, 2008, which is a non-provisional of U.S. Provisional Patent Application Ser. No. 61/008,418 entitled “Spacer insertion instrument” filed on Dec. 19, 2007 both of which are incorporated herein by reference in their entireties. This application also claims priority to and is a continuation-in-part of U.S. patent application Ser. No. 12/205,511 entitled “Interspinous spacer” filed on Sep. 5, 2008, which issued as U.S. Pat. No. 8,123,782 on Feb. 28, 2012, which is a non-provisional of U.S. Provisional Patent Application Ser. No. 60/967,805 entitled “Interspinous spacer” filed on Sep. 7, 2007 and a continuation-in-part of U.S. patent application Ser. No. 12/220,427 entitled “Interspinous spacer” filed on Jul. 24, 2008, which issued as U.S. Pat. No. 8,277,488 on Oct. 2, 2012, which is a non-provisional of U.S. Provisional Patent Application Ser. No. 60/961,741 entitled “Interspinous spacer” filed on Jul. 24, 2007 and is a continuation-in-part of U.S. patent application Ser. No. 12/217,662 entitled “Interspinous spacer” filed on Jul. 8, 2008, which issued as U.S. Pat. No. 8,273,108 on Sep. 15, 2012, which is a non-provisional of U.S. Provisional Patent Application No. 60/958,876 entitled Interspinous spacer” filed on Jul. 9, 2007 and a continuation-in-part of U.S. patent application Ser. No. 12/148,104 entitled “Interspinous spacer” filed on Apr. 16, 2008, which issued as U.S. Pat. No. 8,292,922 on Oct. 23, 2012, which is a non-provisional of U.S. Provisional Patent Application Ser. No. 60/923,971 entitled “Interspinous spacer” filed on Apr. 17, 2007 and U.S. Provisional Patent Application Ser. No. 60/923,841 entitled “Spacer insertion instrument” filed on Apr. 16, 2007, all of which are hereby incorporated by reference in their entireties. This application is also a continuation-in-part of U.S. patent application Ser. No. 11/593,995 entitled “Systems and methods for posterior dynamic stabilization of the spine” filed on Nov. 7, 2006, which issued as U.S. Pat. No. 8,425,559 on Apr. 23, 2013, and a continuation-in-part of U.S. patent application Ser. No. 11/582,874 entitled “Minimally invasive tooling for delivery of interspinous spacer” filed Oct. 18, 2006, which issued as U.S. Pat. No. 8,128,662 on Mar. 6, 2012, and a continuation-in-part of U.S. patent application Ser. No. 11/314,712 entitled “Systems and methods for posterior dynamic stabilization of the spine” filed on Dec. 20, 2005, which issued as U.S. Pat. No. 8,152,837 on Apr. 10, 2012, and a continuation-in-part of U.S. patent application Ser. No. 11/190,496 entitled “Systems and methods for posterior dynamic stabilization of the spine” filed on Jul. 26, 2005, which issued as U.S. Pat. No. 8,409,282 on Apr. 2, 2013, and a continuation-in-part of U.S. patent application Ser. No. 11/079,006 entitled “Systems and methods for posterior dynamic stabilization of the spine” filed on Mar. 10, 2005, which issued as U.S. Pat. No. 8,012,207 on Sep. 6, 2011 and a continuation-in-part of U.S. patent application Ser. No. 11/052,002 entitled “Systems and methods for posterior dynamic stabilization of the spine” filed on Feb. 4, 2005, which issued as U.S. Pat. No. 8,317,864 on Nov. 27, 2012, and a continuation-in-part of U.S. patent application Ser. No. 11/006,502 entitled “Systems and methods for posterior dynamic stabilization of the spine” filed on Dec. 6, 2004, which issued as U.S. Pat. No. 8,123,807 on Feb. 28, 2012, and is a continuation-in-part of U.S. patent application Ser. No. 10/970,843 entitled “Systems and methods for posterior dynamic stabilization of the spine” filed on Oct. 20, 2004, which issued U.S. Pat. No. 8,167,944 on May 1, 2012, and a continuation-in-part of U.S. patent application Ser. No. 11/006,521 entitled “Systems and methods for stabilizing the motion or adjusting the position of the spine” filed on Dec. 6, 2004, and is a continuation-in-part of U.S. patent application Ser. No. 11/305,820 entitled “Systems and methods for posterior dynamic stabilization of the spine” filed on Dec. 15, 2005, which issued as U.S. Pat. No. 7,763,074 on Jul. 27, 2010, all of which are hereby incorporated by reference in their entireties.
BACKGROUND
With spinal stenosis, the spinal canal narrows and pinches the spinal cord and nerves, causing pain in the back and legs. Typically, with age, a person's ligaments may thicken, intervertebral discs may deteriorate and facet joints may break down—all contributing to the condition of the spine characterized by a narrowing of the spinal canal. Injury, heredity, arthritis, changes in blood flow and other causes may also contribute to spinal stenosis.
Doctors have been at the forefront with various treatments of the spine including medications, surgical techniques and implantable devices that alleviate and substantially reduce debilitating pain associated with the back. In one surgical technique, a spacer is implanted between adjacent spinous processes of a patient's spine. The implanted spacer opens the spinal canal, neural foramen, maintains the desired distance between vertebral body segments, and as a result, reduces the impingement of nerves and relieves pain. For suitable candidates, an implantable interspinous spacer may provide significant benefits in terms of pain relief.
Any surgery is an ordeal. However, the type of device and how it is implanted has an impact. For example, one consideration when performing surgery to implant an interspinous spacer is the size of the incision that is required to allow introduction of the device. Small incisions and minimally invasive techniques are generally preferred as they affect less tissue and result in speedier recovery times. As such, there is a need for interspinous spacers and instruments that are used to implant them that work well with surgical techniques that are percutaneous and/or minimally invasive for the patient that can also be used in an open or mini-open procedure. The present invention sets forth such an instrument system.
SUMMARY
According to one aspect of the invention, an instrument system is provided. The system includes an interspinous process spacer, an inserter, a driver and a deployment indicator. The inserter is configured to releasably attach to the spacer at one end for implanting the spacer into a patient's interspinous process space. The driver that is connected to the inserter is configured to arrange the spacer from at least one undeployed configuration to at least one deployed configuration and the deployment indicator provides at least one information to the user pertaining to the degree of deployment of the attached spacer.
According to another aspect of the invention, an instrument for inserting a deployable interspinous process spacer into a patient is provided. The instrument includes a first end connectable to an interspinous process spacer and a second end configured to arrange a connected spacer between at least a first configuration and at least a second configuration. The instrument includes a sensor configured to measure the arrangement of a connected spacer and provide a signal regarding the arrangement of a connected spacer to the user.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1A illustrates a side view of a spacer instrument system connected to a spacer in a closed or an undeployed configuration according to the present invention.
FIG. 1B illustrates a side view of a spacer instrument system connected to a spacer in an open or deployed configuration according to the present invention.
FIG. 2 illustrates a perspective partial end view of an inserter and driver of a spacer instrument system according to the present invention.
FIG. 3A illustrates a perspective view of a driver according to the present invention.
FIG. 3B illustrates a side view of a driver according to the present invention.
FIG. 3C illustrates a cross-sectional view taken along line A-A of FIG. 3B of the driver according to the present invention.
FIG. 3D illustrates a side view of a driver according to the present invention.
FIG. 4A illustrates a perspective view of a spacer in an undeployed or closed configuration according to the present invention.
FIG. 4B illustrates a perspective view of a spacer in a deployed or open configuration according to the present invention.
FIG. 4C illustrates a top view of a spacer in a deployed or open configuration according to the present invention.
DETAILED DESCRIPTION
Referring first to FIGS. 1A and 1B , there is shown a spacer instrument system 10 with a deployment indicator according to the present invention connected to an interspinous process spacer 12 in a closed or undeployed configuration and in an open or deployed configuration, respectively. The spacer instrument system 10 includes an inserter 14 and a driver 16 .
Still referencing FIGS. 1A and 1B and with additional reference to FIG. 2 , the inserter 14 will now be described. The inserter 14 is of the type described in co-pending U.S. patent application Ser. No. 12/338,793 entitled “Spacer insertion instrument” filed on Dec. 18, 2008 which claims the benefit of U.S. Provisional patent application Ser. No. 61/008,418 entitled “Spacer insertion instrument” filed on Dec. 19, 2007 both of which are assigned to VertiFlex, Inc. and hereby incorporated by reference in their entireties. The inserter 14 is configured to releasably clamp to a body of an interspinous process implant or spacer 12 to be delivered into or removed from a patient using the system 10 . The inserter 14 includes an inner shaft 18 , an outer shaft 20 , a control 22 and handle assembly 24 . The inner shaft 18 is connected to the handle assembly 24 of the inserter 14 and the outer shaft 20 is passed over the inner shaft 18 and allowed to translate with respect to the inner shaft 18 by means of a control 22 that is threadingly engaged with the outer shaft 20 . With rotation of the control 22 in one direction, the outer shaft 20 translates distally with respect to the stationary inner shaft 18 . With rotation of the control 22 in the opposite direction, the outer shaft 20 translates proximally with respect to the stationary inner shaft 18 . In another variation of the invention, the outer shaft 20 is connected to handle assembly 24 and the inner shaft is threadingly connected to the control 22 such that rotation of the control 22 moves the inner shaft 18 with respect to the outer shaft 20 proximally or distally. Although rotation of the control 22 is used in one variation, other variations are within the scope of the present invention such as, for example, translation of the control 22 or movement of the outer shaft 20 relative to the inner shaft 18 .
With particular reference to FIG. 2 , the inner shaft 18 of the inserter 14 is substantially cylindrical in shape having a central bore extending from end to end. The distal end of the inner shaft 18 includes a pair of prongs 26 with each prong being substantially oppositely located from each other. The finger-like prongs 26 are flexible and, when in a normal position, splay slightly outwardly from the longitudinal axis. The prongs 26 are configured to connect with the spacer 12 . In particular, the prongs 26 include extensions 28 that extend inwardly toward the longitudinal axis in a hook-like fashion. These extensions 28 are configured to be inserted into prong-receiving portions 30 (see FIGS. 4A , 4 B and 4 C) on the spacer 12 and securely clamp thereto. The prongs 26 also include conforming surfaces configured to conform to the spacer 12 in a manner best suited for secure attachment thereto. The proximal end of the inner shaft 18 is configured for insertion into and connection with a conformingly shaped recess in the handle 24 .
The outer shaft 20 of the inserter 14 will now be described. As seen in FIG. 2 , the outer shaft 22 is substantially cylindrical in shape having a central bore 32 extending from end to end. The outer shaft 20 is sized such that the inner shaft 18 fits inside the outer shaft 20 . The distal end includes a pair of flattened portions 34 located substantially opposite from each other for a narrower profile and in one variation a ramped profile for insertion or placement between adjacent spinous processes of a patient's spine. The ramped profile serves to distract the adjacent spinous processes apart slightly as the inserter is being inserted between the adjacent spinous processes for insertion of the connected spacer 12 wherein the flattened portions 34 are separated by an increasingly wider distance towards the proximal end of the instrument. The outer shaft 20 includes a threaded proximal portion (not shown). The threaded proximal portion is configured for threaded connection with the control 22 such that movement of the control 22 moves the outer shaft 20 .
The control 22 includes a user interface such as a finger portion or grip. In one variation, the user interface is an outer circular or disk-shaped portion for easily effecting rotation of the control 22 with a thumb or index finger. The control 22 is configured to effect relative translation of the inner shaft 18 with respect to the outer shaft 20 .
The spacer instrument system 10 functions to engage with, insert and deploy an interspinous spacer 12 in an interspinous process space between two adjacent vertebrae. Illustrative examples of interspinous spacers that are compatible with the insertion instrument are described in applicant's co-pending U.S. patent application Ser. No. 12/148,104 entitled “Interspinous spacer” filed on Apr. 16, 2008 which claims the benefit of U.S. Provisional Patent Application Ser. No. 60/923,841 entitled “Spacer insertion instrument” filed on Apr. 16, 2007 and U.S. Provisional Patent Application Ser. No. 60/923,971 entitled “Interspinous spacer” filed on Apr. 17, 2007, U.S. patent application Ser. No. 12/217,662 entitled “Interspinous spacer” filed on Jul. 8, 2008 which claims the benefit of U.S. Provisional Patent Application Ser. No. 60/958,876 entitled “Interspinous spacer” filed on Jul. 9, 2007, U.S. patent application Ser. No. 12/220,427 entitled “Interspinous spacer” filed on Jul. 24, 2008 which claims the benefit of U.S. Provisional Patent Application Ser. No. 60/961,741 entitled “Interspinous spacer” filed on Jul. 24, 2007, and U.S. patent application Ser. No. 12/205,511 entitled “Interspinous spacer” filed on Sep. 5, 2008 which claims the benefit of U.S. Provisional Patent Application Ser. No. 60/967,805 entitled “Interspinous spacer” filed on Sep. 7, 2007, and U.S. patent application Ser. No. 12/354,517 entitled “Interspinous spacer” filed on Jan. 15, 2009 which claims the benefit of U.S. Provisional Patent Application Ser. No. 61/011,199 entitled “Interspinous spacer” filed on Jan. 15, 2008 the disclosure of all of which are incorporated herein by reference in their entireties. An example of an interspinous spacer 12 is shown in FIGS. 4A , 4 B and 4 C. In general, each spacer 12 includes a body portion 36 with at least one prong receiving portion 30 for connecting with the instrument 10 , at least one wing 40 rotatably connected to the body 36 and an actuator shaft 38 housed in the body portion 36 and configured to arrange the at least one wing 40 from at least one undeployed configuration (see FIG. 4A ) to at least one deployed configuration (see FIGS. 4B and 4C ) and vice versa. The wings 40 are configured to laterally stabilize the body portion 36 relative to thespinous processes, seat and/or space apart the spinous processes of adjacent vertebrae when in the deployed configuration to relieve pain.
The spacer instrument system 10 utilizes the working channel that is preferably created by the use of one or more tools such as a target needle, K-wire, dilators, mounting bracket, cannula, stabilizing arm, interspinous knife, interspinous reamer, and interspinous gage, all described in applicant's co-pending U.S. patent application Ser. No. 11/582,874 entitled “Minimally invasive tooling for delivery of interspinous spacer” filed on Oct. 18, 2006, incorporated herein by reference in its entirety. The inserter 14 is typically inserted through a cannula with the distal end positioned at the interspinous process space in a minimally invasive, percutaneous, mini-open or open surgical procedure. In some procedures, a cannula is not employed to deliver the spacer instrument system 10 and spacer 12 to the interspinous space.
In use, a spacer 12 is placed in juxtaposition to the distal end of the inserter 14 such that the prongs 26 of the inserter 14 are adjacent to the prong receiving portions 30 on the spacer 12 . The control 22 is then activated to clamp the prongs 26 of the inner shaft 18 onto the spacer 12 . In particular, the control 22 is rotated in one direction which advances the outer shaft 20 over the inner shaft 18 to thereby inwardly deflect the outwardly splayed prongs 26 at the distal end of the inner shaft 18 . This inward deflection allows the prongs 26 to engage the spacer body 36 and, in particular, allows the prong extensions 28 to be inserted into the prong receiving portions 30 and with further rotation of the control 22 to lock the inserter 14 securely onto the spacer 12 . Reverse rotation of the control 22 translates the outer shaft 20 proximally to expose the prongs 26 allowing them to splay outwardly to their pre-stressed normal position and thereby release the spacer 12 from the inserter 14 .
If a cannula is employed in the operative site, the inserter 14 with the attached spacer 12 is sized to fit through a cannula and is passed through the cannula to the interspinous process space. Once in position inside the patient, the driver 16 is inserted into the proximal opening of the central passageway of the inserter 14 and passed until the driver 16 connects with the spacer 12 .
Turning now to FIGS. 3A , 3 B, 3 C and 3 D, the driver 16 will now be described. The driver 16 includes: (1) a handle 42 having a proximal end 44 and a distal end 46 , (2) a inner shaft 48 , (3) outer shaft 50 , (3) a spacer engaging bit 54 connected to the distal end of the outer shaft 50 , and (4) a spring 52 . The outer shaft 50 which is connected to the distal end 46 of the handle 42 includes a lumen in which the inner shaft 48 is disposed. The inner shaft 48 includes a collar 56 (shown in FIG. 3C ) configured to be located inside the handle 42 and biased against the spring 52 and configured such that the spring 52 forces the inner shaft 48 distally in a direction towards the spacer engaging bit 54 . The proximal end 44 of the handle 42 includes a deployment indicator window 58 through which the inner shaft 48 is viewed. FIG. 2 illustrates the distal end of the driver 16 inserted into the inserter 14 .
Depending on the spacer 12 design, the connection of the driver 16 with the spacer 12 , in particular the spacer engaging bit 54 , will be different. In general, however, the driver 16 connects to the spacer 12 such that movement, such as rotation, of the driver 16 effects deployment of a deployable spacer 12 , in particular, the deployment of the at least one wing 40 of the spacer 12 . In particular, and with respect to the spacer embodiment shown in FIGS. 4A-4C , rotation of the driver 16 that is connected to the spacer 12 effects translation of the actuator shaft 38 of the spacer 12 which in turn is connected to the at least one wing 40 causing it to deploy into an expanded configuration or deployed configuration.
The driver 16 that is configured to connect with the spacer 12 of FIGS. 4A-4C will have a spacer engaging bit 54 that includes two projecting features 60 . The two projecting features 60 engage complementary features 62 on the spacer 12 located inside the spacer body portion 36 as shown in FIGS. 4A-4C . Once engaged to the spacer 12 , rotation of the driver 16 rotates the spindle 64 which in turn advances the actuator shaft 38 to deploy the wings 70 into the configuration shown in FIGS. 4B and 4C . Reverse rotation of the driver 16 will turn the spindle 64 in an opposite direction and proximally translate the actuator shaft 38 to undeploy the wings 40 . As can be seen in FIGS. 4B and 4C , when in the deployed configuration, the actuator shaft 38 is distally translated with rotation of the driver 16 relative to when in the undeployed configuration as shown in FIG. 4A wherein the actuator shaft 38 projects proximally from the spacer body 36 . This distance traveled by the actuator shaft 38 provides the information about the degree of deployment of the wings 40 of the spacer 12 that is communicated to the inner shaft 48 of the driver 16 . With the inserter 14 connected to the spacer 12 and the driver 16 inserted into the central passageway of the inserter 14 and connected to the spindle 64 such that the projecting features 60 of the bit 54 engage the features 62 on the spindle 64 , the inner shaft 48 of the driver 16 contacts the proximal end 66 of the actuator shaft 38 and will bias the inner shaft 48 a distance related to the distance with which the actuator shaft 38 projects proximally from the spacer body 36 . Hence, as the driver 16 is rotated to effect translation of the actuator shaft 38 inwardly or outwardly to deploy or undeploy the spacer, the bias force of the spring 52 will keep the distal end of the inner shaft 48 of the driver 16 in contact with the proximal end 66 of the actuator shaft 38 as it translates proximally or distally providing an indication as to the degree of deployment of the spacer 12 . The indication as to the degree of deployment of the spacer 12 is viewed at the proximal end of the system 10 . Because the handle 24 resides outside the patient, the deployment information is readily visible to the surgeon.
Referring back to FIG. 1A , there is shown the system 10 in an undeployed configuration. As can be seen, at the proximal end, the inner shaft 48 projects outwardly from the proximal end 44 of the handle 24 . As the driver 16 is rotated to deploy the spacer 12 , the inner shaft 48 moves distally until the inner shaft 48 does not project outwardly from the proximal end 44 of the handle 24 and/or is co-planar with the proximal end 44 of the handle 24 as shown in FIG. 1B , thereby providing the user with a visual indication of the degree of deployment of the spacer 12 wherein if the inner shaft 48 is not projecting then the spacer 12 is fully deployed and if the inner shaft 48 is projecting from the proximal end 44 of the handle 24 then a state other than full deployment is indicated. The degree of deployment is related to the distance with which the inner shaft 48 is projecting outwardly from the proximal end 44 of the handle 24 . The proximal end of the inner shaft 48 or “button” provides the surgeon not only with visual feedback but also tactile feedback as to the degree of deployment.
Another deployment indicator is provided alternatively or in conjunction with the projection of the inner shaft 48 from the proximal end 44 just described. This other deployment indicator includes an indicator line 68 (shown in FIGS. 1B and 3D ) provided on the inner shaft 48 of the driver 16 , which becomes visible through the indicator window 58 as the inner shaft 48 translates with deployment of the spacer 12 . When in the undeployed configuration as shown in FIG. 1A , the indicator line 68 is proximal of the window 58 and therefore not visible through the indicator window 58 . When the spacer 12 approaches a deployed configuration, the indicator line 68 will enter the indicator window 58 and be visible to the user. An additional alignment line or lines 70 is provided on the proximal end 44 of the handle 24 adjacent to the indicator window 58 as shown in FIGS. 1B and 3D . When the indicator line 68 on the inner shaft 48 is aligned with the alignment line or lines 70 on the handle 24 , a fully deployed configuration of the spacer 12 is indicated providing a visual information of deployment to the surgeon.
The above description is one variation of mechanical sensor connected to the instrument for measuring the arrangement of a connected spacer 10 . One skilled in the art will recognize that the instrument can be configured with any suitable sensor that can be effectively employed to measure the arrangement of the spacer and provide a signal to the user regarding the arrangement of the connected spacer. Examples of suitable sensors include, but are not limited to mechanical, position, optical, electromagnetic, motion, and distance sensors. Of course, suitable signals communicating the measured information include audible, visual, tactile signals and the like. The signal may be transmitted to a receiver located on the instrument itself preferable at a location that is resident outside the patient while in use or at a location remote of the instrument. In one variation, the sensor provides a signal only upon full deployment of the spacer. In another variation, the sensor provides continuous information as to the arrangment of the spacer.
Hence, the present invention advantageously provides information regarding the degree of deployment of the spacer to the surgeon which is particularly advantageous in minimally invasive and percutaneous procedures where the device cannot be viewed without the aid of fluoroscopy because of visual obstruction accompanying very small incisions. As a result of the deployment information provided by the system, this invention advantageously reduces time required to implant the spacer and also advantageously reduces the number of fluoroscopy shots that the clinicians and patients are exposed to during the procedure as the deployment information is readily provided to the surgeon by the spacer instrument system with deployment indicator that is located outside patient incision.
All publications mentioned herein are incorporated herein by reference to disclose and describe the methods and/or materials in connection with which the publications are cited. The preceding illustrates the principles of the invention. It will be appreciated that those skilled in the art will be able to devise various arrangements which, although not explicitly described or shown herein, embody the principles of the invention and are included within its spirit and scope.
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A percutaneous and minimally invasive instrument system for implanting an interspinous process spacer into a patient is disclosed. The insertion instrument system includes an inserter and a driver. The inserter is configured to releasably clamp to an interspinous process spacer for its delivery, implantation and deployment. The driver is configured for removable insertion into a proximal end of a passageway of the inserter. The driver has a distal spacer engaging portion configured to engage that part of the spacer requiring activation for the deployment of the spacer from at least one undeployed configuration to at least one deployed configuration and vice versa. As the spacer goes from the undeployed to the deployed configuration and vice versa, the system advantageously provides a degree of deployment information to the user via at least one deployment indicator.
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SUMMARY
A slider generally comprises a substrate forming at least part of a body of the slider, a heat-assisted media recording (HAMR) read/write transducer proximate the substrate, and an end cap substantially encapsulating the HAMR read/write transducer. The end cap has a first surface proximate the substrate and a second surface as a trailing edge of the slider. The end cap has a first coefficient of thermal expansion (CTE) similar to a corresponding CTE of the substrate. At least a portion of the second surface of the end cap has a second CTE that is lower than the first CTE. A body of the end cap is intermediate to the first and second surfaces of the end cap and has a CTE intermediate of the first and second CTE.
The above summary is not intended to describe each embodiment or every implementation. A more complete understanding will become apparent and appreciated by referring to the following detailed description and claims in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a HAMR a slider of an example embodiment.
FIG. 2 is a sectional view of a trailing edge cap of an example embodiment.
FIG. 3 is a sectional view of a trailing edge cap of an example embodiment.
The figures are not necessarily to scale. Like numbers used in the figures refer to like components. However, it will be understood that the use of a number to refer to a component in a given figure is not intended to limit the component in another figure labeled with the same number.
DETAILED DESCRIPTION
The present disclosure is directed to apparatus, systems and methods to reduce thermal profile changes of head sliders in heat assisted magnetic recording (HAMR) drives through the use of selected materials in the trailing edge cap and/or substrate of the slider body.
HAMR generally refers to the concept of locally heating a recording medium with a laser to reduce the coercivity. This allows the applied magnetic writing fields to more easily direct the magnetization during temporary magnetic softening caused by the heat source. HAMR allows for the use of small grain media, with a larger magnetic anisotropy at room temperature to assure sufficient thermal stability, which is desirable for recording at increased areal densities. HAMR can be applied to any type of magnetic storage media including tilted media, longitudinal media, perpendicular media, and patterned media. By heating the media, the coercivity is reduced such that the magnetic write field is sufficient to write to the media. Once the media cools to ambient temperature, the coercivity has a sufficiently high value to assure thermal stability of the recorded information.
In a HAMR magnetic data storage and retrieval system, a thin film transducing head, which is also known as a slider, may include a transducer, a substrate upon which the transducer is built, and an encapsulating end cap layer at the trailing edge of the transducing head. The transducer may include a writer portion, assisted by a thin beam laser, to record magnetically encoded information on a magnetic media and a reader portion to retrieve magnetically encoded information. During operation, the slider is positioned in close proximity to the magnetic media. The distance between the slider and the media is small enough to allow for writing to and reading from the magnetic media and large enough to prevent contact between the magnetic media and the slider.
During HAMR write operations the laser can be subject to a high power loss which is largely converted to heat. The heat affects the various layers/elements of the slider in different ways as each of the layers/elements are made from different materials having different coefficients of thermal expansion (CTEs). For example, the substrate of the slider is may be comprised of aluminum oxide/titanium carbide (AlTiC), the end cap layer of alumina, and the transducer of many layers including metals. The CTE for TiC is 7.7×10 −6 /° C. linear while the CTE for alumina is 8.1×10 −6 /° C. linear. Metallic layers have a very high CTE. All elements of the slider are subject to expansion and deformation caused by the heat of the laser. The deformed head slider will protrude towards the disk surface causing changes in head-disk clearance, which is controlled at nanometer range, for example, ˜1.5 nm or less, and in air-bearing flyability; these changes may lead to problematic clearance control and head-disk contact. The heat may also cause the elements along the path of the laser to expand in a lateral dimension which can affect servo and read/write performances of the slider head. Thermal-fly-height (TFC) heaters are used to help control thermal expansion to achieve a low flight-height recording; however, more can be done to control thermal expansion through the optimization of materials chosen for the slider body.
FIG. 1 illustrates a perspective view of an example HAMR recording head slider 100 attached to suspension 102 . Slider 100 presents an air bearing surface (ABS) 104 , a leading edge 106 and a trailing edge 108 , and generally comprises a substrate 110 , an optional insulating layer 112 , and an encapsulating trailing edge cap 114 . Trailing edge cap 114 encapsulates a magnetic HAMR transducer 116 , an electromagnetic energy source, e.g., laser, 118 , and other microelectronic and associated photonic elements and circuitry, which can include, for example, shields, TFC heaters, and sensors (not shown). Transducer 116 meets the ABS 104 at media facing surface interface 119 . Trailing edge cap 114 is additionally provided with external electrical contacts 120 .
As explained above, the trailing edge cap alumina and AlTiC substrate of slider bodies may have significant CTEs, which make them protrude/deform heavily under the write duty cycle laser heat in HAMR drives. To improve thermal profile changes, materials of low CTEs are used in slider bodies especially in high-heat areas. In an example embodiment, the sputtered alumina of the trailing edge cap 114 is replaced with a carbide, nitride, or oxide of a very low CTE. Preferred examples of materials for the trailing edge cap 114 and their CTE values are provided in Table 1 below, with the highest CTE value being 6.9×10 −6 /° C. linear.
TABLE 1
Coefficient of Thermal Expansion
of Selected Ceramics
Ceramic
CTE (×10 −6 /° C.)
AlN
4.6
BN
2.2
Si 3 N 4
3.3
GeN
5.6
GaN
4.5
B 4 C
5.5
SiC
2.8
HfC
6.6
ZrC
6.9
WC
4.3
W 2 C
5.8
NbC
6.6
TaC
6.3
HfB 2
5.0
ZrB 2
5.9
TiB 2
5.5
VB 2
5.3
CrB 2
5.7
ZnO
4.0
SiO 2 Al 2 O 3
5.1
SiO 2 ZrO 2
4.5
CaOHfO 2
3.3
Si
2.6
SiO 2
2.6
ZrW 2 O 8
(−6) − (−9)
ZrMo 2 O 8
−11
HfW 2 O 8
−10
ZrV 2 O 7
(−1) − (7.1)
ScW3O12
−2.2
ReO 3
(−0.5) − (−0.7)
LiAlSiO 4
(−1) − (−6)
Mn 3 Cu 0.53 Ge 0.47 N
−16
Mn 3 Zn 0.4 Sn 0.6 N 0.85 C 0.15
−23
Mn 3 Zn 0.5 Sn 0.5 N 0.85 C 0.1 B 0.05
−30
(HfMg)(WO 4 )
−2
Bi 0.95 La 0.05 NiO 3
−82
Note:
CTE in Table 1 may vary with the structure, structure orientation, application temperature, pressure and the preparation conditions, for example, vacuum pressure, gas composition, substrate temperature and deposition technique.
The materials in Table 1 may be used in pure phases or as components in composite materials with tailored thermal expansion coefficients. The atomic ratio in the materials may vary slightly which may correspondingly vary the thermal expansion coefficient of the materials. For example, ZrW 2 O 8 may have varied atomic ratio which in general expressed ZrW x O y , in which the values of X and Y vary within a range.
Compounds belonging to the zirconium vanadate family have a general formula of AM 2 O 7 . When M=V, the A cation can be Zr and Hf. When M=As, the A cation can be Zr or Th. When M=P, the A cation can be Zr, Hf, Ti, U, Th, Pu, Ce, Mo, W, Re, Pb, Sn, Ge, or Si. The vanadate and phosphate compounds exist in a cubic structure in space group of Pa3 − . These compounds adopt a NaCl structure made up of AO 6 octahedra and M 2 O 7 units.
The materials of Table 1 may be prepared by vacuum deposition techniques such as chemical vapor deposition, sputtering, cathodic arc deposition, laser beam ablation, etc. While the materials of Table 1 present CTEs significantly lower than the CTE of sputtered alumina, these materials also have acceptable hardness and large optical band gaps from 3 to 6 eV, which make them wear-resistant and electrically insulating and, therefore, desirable selections for the trailing edge cap 114 to resist profile changes under the write cycle laser heat in HAMR drives. The materials for the trailing edge cap 114 are most appropriate when they also have a low intrinsic stress (compressive and tensile) relative to the transducer electronics so as to protect the electronics. Low intrinsic stress for the trailing edge cap materials of Table 1 can be obtained by regulating the substrate bias/temperature, deposition rate and gas pressure during vacuum deposition.
In another example embodiment, see FIG. 2 , the trailing edge cap 114 , adjacent substrate 110 , is designed to incorporate multiple materials, such as those from Table 1. In this embodiment, the trailing edge cap is presented in a configuration where a first material 130 surrounds or encapsulates the area of highest heat, for example, around the read/write transducers (not shown) and the laser near-field transducer (not shown), is of the lowest CTE. A second material 132 surrounding or encapsulating the first material 130 may be of a slightly higher CTE, a third material 134 surrounding or encapsulating the second material may be of a still slightly higher CTS than material 132 , and so on. Any number of layers of materials may be used with the low CTE material increasing in CTE value from the area of highest heat within the slider out to the substrate 110 . The materials with a CTE approximating or greater than 7×10 −6 /° C. linear are nearest the substrate 110 while the materials of Table 1 with a CTE at or less than 5×10 −6 /° C. linear, (e.g., at or less than 3×10 −6 /° C. linear), are nearest the trailing edge 108 .
In another example embodiment, the material chosen for the trailing edge end cap 114 has a CTE comparable to that of the AlTiC slider body 110 , see FIG. 3 . In this embodiment, the trailing edge end cap 114 is in a laminated configuration presenting layers, e.g., 141 - 149 , whose CTE gradually decreases towards the extreme edge (layer 149 ). As carbides and nitrides possess good adhesion to one another, the material of the cap end layer (layer 141 ) can either be a carbide or nitride so as to bind well with the AlTiC substrate 110 of the slider body 100 ; the AlTiC substrate has ˜30 wt. % of carbide as TiC. Once again, the materials with a CTE approximating or greater than 7×10 −6 /° C. linear are nearest the substrate 110 while the materials of Table 1 with a CTE at or less than 5×10 −6 /° C. linear, e.g., at or less than 3×10 −6 /° C. linear, are nearest the trailing edge 108 .
In another example embodiment, represented again by FIG. 1 , a configuration of the low CTE trailing edge cap 114 , such as those described above, is combined with a slider body substrate 110 of a low CTE. In this embodiment, the slider body substrate 110 , may include AlTiC or similar material having a significant thermal expansion tendency, is instead made of a material or materials having low CTEs so as to reach an optimal thermal compatibility with the trailing edge cap 114 . A low CTE edge cap 114 in combination with a low CTE slider body substrate 110 can altogether reduce the thermal profile changes for the whole head slider 100 under the write duty cycle laser heat in HAMR drives. Example slider body substrate 110 materials include SiC, ZrC, Si, metal oxide and carbide composites and have a CTE of 3×10 −6 /° C. linear or less. These materials also have high hardness and acceptable electrical conductivity.
Systems, devices or methods disclosed herein may include one or more of the features structures, methods, or combination thereof described herein. For example, a device or method may be implemented to include one or more of the features and/or processes above. It is intended that such device or method need not include all of the features and/or processes described herein, but may be implemented to include selected features and/or processes that provide useful structures and/or functionality.
Unless otherwise indicated, all numbers expressing feature sizes, amounts, and physical properties used in the specification and claims are to be understood as being modified in all instances by the term “about.” Accordingly, unless indicated to the contrary, the numerical parameters set forth in the foregoing specification and attached claims are approximations that can vary depending upon the desired properties sought to be obtained by those skilled in the art utilizing the teachings disclosed herein. The use of numerical ranges by endpoints includes all numbers within that range (e.g. 1 to 5 includes 1, 1.5, 2, 2.75, 3, 3.80, 4, and 5) and any range within that range.
Various modifications and additions can be made to the disclosed embodiments discussed above. Accordingly, the scope of the present disclosure should not be limited by the particular embodiments described above, but should be defined only by the claims set forth below and equivalents thereof.
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A slider generally comprises a substrate forming at least part of a body of the slider, a heat-assisted media recording (HAMR) read/write transducer proximate the substrate, and an end cap substantially encapsulating the HAMR read/write transducer. The end cap has a first surface proximate the substrate and a second surface as a trailing edge of the slider. The end cap has a first coefficient of thermal expansion (CTE) similar to a corresponding CTE of the substrate. At least a portion of the second surface of the end cap has a second CTE that is lower than the first CTE. A body of the end cap is intermediate to the first and second surfaces of the end cap and has a CTE intermediate of the first and second CTE.
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RELATED APPLICATION
[0001] The present application claims the benefit of U.S. Provisional Application No. 61/613,770 filed Mar. 21, 2012, and entitled “AUTOMATED IMPLANTABLE PENILE PROSTHESIS PUMP SYSTEM”, which is incorporated herein in its entirety by reference.
FIELD OF THE INVENTION
[0002] The present invention is generally directed to a pump system for an implantable penile prosthesis. Specifically, the present invention is directed to a suction poppet assembly for an implantable penile prosthesis pump system.
BACKGROUND OF THE INVENTION
[0003] Implantation of an implantable penile prosthesis (IPP) is a common surgical procedure for treating erectile dysfunction and other penile ailments. An IPP comprises an inflatable cylinder connected by a pump to a separate reservoir for holding the quantity of fill liquid via kink resistant tubing. This version of the IPP is available under the trade name AMBICOR from American Medical Systems of Minnetonka, Minn. Typically, the entire IPP is implanted into the patient's body with the inflatable cylinder being placed in the corpus cavernosum and the pump being placed within the scrotum. The reservoir can also be placed within the scrotum or placed elsewhere within the pelvic region. To operate the IPP, the pump is manually actuated to transfer fill liquid from the integrated or implanted reservoir into the inflatable cylinder to fill and pressurize the inflatable cylinder.
[0004] A typical pump system for an IPP comprises a pump bulb that can be compressed to draw fluid from a reservoir and push the inflation fluid into the inflatable cylinder. Generally, the pump is compressed and released to draw fluid from the reservoir into the pump. The pump is compressed again to force fluid from the pump into the inflatable cylinder. Two selective poppet valves are positioned along the flow path between reservoir and inflatable cylinder to control the direction of the fluid flow through the pump system.
[0005] Typically, the IPP and the pump system are provided to the medical personnel without any working fluid within the system. Prior to implantation, each component of the IPP is filled or nearly filed with the working fluid by the medical personnel. The medical personnel also often test the operation of the IPP to insure that the all the components of the IPP are functioning properly prior to implantation. However, if too much air remains in the IPP when the pump system is operated by the medical personnel or the patient, the air within the system can cause pump to lock up. Specifically, the pump bulb can remain compressed after being actuated rather than re-expanding to draw additional fluid into the pump bulb.
[0006] Another drawback of the pump system is that the poppet valves can become misaligned during filling and operation of the IPP and pump system. If the poppet becomes misaligned, uncontrolled leakage can occur allowing fluid to travel through the fluid pathway. Similarly, the misaligned poppet can become stuck preventing any operation of the poppet.
[0007] As such, there is a need for a pump system for an IPP that can be operated by medical personnel with a reduced risk of damage or malfunction during test operation.
SUMMARY OF THE INVENTION
[0008] The present invention is directed to an IPP having a valve assembly comprising a dual poppet design. The valve assembly is integrated into a pump assembly comprising a pump bulb that can be actuated to transfer working fluid from a reservoir to at least one inflatable cylinder. The valve assembly defines a valve flow path, for example, a generally linear flow path, between the reservoir and the inflatable cylinder. The valve flow path intersects the opening to the pump bulb such that actuating the pump bulb moves fluid along the flow path. In one aspect, the valve flow path also defines a suction annulus positioned in the valve flow path between the reservoir and the pump bulb. Similarly, the valve flow path can also define a cylinder annulus positioned between the pump bulb and the cylinder.
[0009] In one aspect, the valve assembly comprises a suction poppet engagable to the suction annulus and a cylinder poppet engagable to the cylinder annulus. Each poppet is movable along a central axis defined by the flow path between an engaged position in which the poppet is engaged to its corresponding annulus to prevent the flow of working fluid through the annulus and a disengaged positioned wherein the poppet is positioned to allow working fluid to pass through the corresponding annulus. In one aspect, the poppets are both biased to the engaged position to prevent flow of working fluid until the pump bulb is actuated. The suction poppet is positioned on the pump bulb side of the suction annulus such that releasing the compressed pump bulb creates a suction that pulls the suction poppet into the disengaged position and draws a quantity of working fluid through the suction annulus into the pump bulb. In contrast, the cylinder poppet is positioned on the opposite side of the cylinder annulus from the pump bulb, wherein compressing the pump bulb creates a positive pressure pushing the cylinder poppet into the disengaged position and a forcing a quantity of working fluid through the cylinder annulus into the inflatable cylinder.
[0010] In one aspect, the flow path further defines an annular ring positioned between the suction annulus and the pump bulb opening. If the pump bulb is actuated too quickly and/or air is present within the pump bulb opening such as, for example, during the initial installation, the suction poppet can become wedged against the annular ring blocking all flow and creating a vacuum condition essentially locking the pump bulb in the compressed state. In one aspect, the suction poppet can further comprise a head extending through the suction annulus. The head can define a lip engagable by a plurality of fingers extending from the suction annulus. The fingers engage the lip when the suction poppet is slid into the disengaged position to prevent the suction poppet from engaging the annular ring and creating vacuum lock up. The fingers allow for a controlled travel distance of the suction poppet preventing vacuum lock up of the pump bulb.
[0011] In one aspect, the suction puppet can further comprise an elongated suction poppet shaft extending through the cylinder annulus. In this configuration, a cylinder poppet can define defines a cylinder poppet bore for slidably receiving the elongated suction poppet shaft. If the suction poppet becomes misaligned, the suction poppet may not properly engage the suction annulus allowing working fluid to leak through the suction annulus. The cylinder poppet bore guides the suction poppet to maintain an axial alignment of the suction poppet along a valve chamber axis as the suction poppet moves between the engaged position and the disengaged position relative to suction annulus.
[0012] In one aspect, the valve assembly can further comprise a release button that can be pressed against an elongated head of the suction poppet to push the suction poppet to the disengaged position along the valve chamber axis without operating the pump bulb. The elongated suction poppet shaft can be used to push against an end of the cylinder poppet bore such that both the suction poppet and the cylinder poppet are positioned in the disengaged position allowing free flow through the valve flow path. The release button can be used to return the working fluid to the reservoir from the inflatable cylinder. The release button can also be used to reset the operation of the valve assembly.
[0013] A method of preventing vacuum lock up of the pump bulb, according to an aspect of the present invention, can comprise providing a suction poppet positioned between the suction annulus leading to the reservoir and the pump bulb, wherein the suction poppet further comprises an elongated head extending through the suction annulus. The method can further comprise defining a plurality of fingers extending from the suction annulus to limit the travel distance of the suction poppet and prevent uncontrolled engagement of the suction poppet to other features within the valve assembly.
[0014] The above summary of the various representative embodiments of the invention is not intended to describe each illustrated embodiment or every implementation of the invention. Rather, the embodiments are chosen and described so that others skilled in the art can appreciate and understand the principles and practices of the invention. The figures in the detailed description that follow more particularly exemplify these embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] The invention can be completely understood in consideration of the following detailed description of various embodiments of the invention in connection with the accompanying drawings, in which:
[0016] FIG. 1 is a top view of a implantable penile prosthesis according to an embodiment of the present invention.
[0017] FIG. 2 is a partial cross-sectional view of a valve assembly according to an embodiment of the present invention.
[0018] FIG. 3 is a side view of a suction poppet according to an embodiment of the present invention.
[0019] FIG. 4 is a perspective view of a suction annulus with a head of the suction poppet extending through annulus according to an embodiment of the present invention.
[0020] While the invention is amenable to various modifications and alternative forms, specifics thereof have been shown by way of example in the drawings and will be described in detail. It should be understood, however, that the intention is not to limit the invention to the particular embodiments described. On the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
DETAILED DESCRIPTION
[0021] As shown in FIG. 1 , an implantable penile prosthesis (IPP) 2 , according to an embodiment of the present invention, comprises at least one inflatable cylinder 4 , a reservoir 6 , a pump 8 and a valve assembly 10 . The pump 8 can further comprise a pump bulb 12 that can be compressed and released to draw and pump working fluid. The IPP 2 generally operates by actuating the pump bulb 12 to draw a quantity of working fluid from the reservoir 6 and pumping the working fluid into the inflatable cylinder 4 . The valve assembly 10 is generally adapted to prevent back flow of the working fluid during operation of the pump 8 to inflate inflatable cylinder 4 .
[0022] As shown in FIGS. 1-2 , the valve assembly 10 defines a valve flow path 14 and comprises a suction poppet 16 and a cylinder poppet 18 . The valve flow path 14 is defined between a reservoir inlet 20 from the reservoir 6 and a cylinder outlet 22 leading to the cylinder 4 . The valve flow path 14 also further comprises a linear valve chamber 24 extending along a central valve chamber axis a-a. The linear valve chamber 24 defines a pump bulb opening 26 providing fluid communication between the pump bulb 12 and the linear valve chamber 24 . The linear valve chamber 24 also defines a suction annulus 28 and an annular ring 30 positioned between the reservoir inlet 20 and the pump bulb opening 26 . Similarly, the linear valve chamber 24 also defines a cylinder annulus 32 positioned between the pump bulb opening 26 and the cylinder outlet 32 . In one aspect, the suction annulus 28 further comprises a plurality of fingers 34 as shown in FIG. 4 that extend radially toward the central valve chamber axis a-a.
[0023] As shown in FIGS. 2-3 , the suction poppet 16 defines a sealing surface 36 and is linearly movable along the central valve chamber axis a-a between an engaged position and a disengaged positioned. In the engaged position, the sealing surface 36 is engaged to the suction annulus 28 preventing flow of working fluid through the suction annulus 28 . In the disengaged positioned, the sealing surface 36 is disengaged from the suction annulus 28 allowing working fluid to pass through the suction annulus 28 . As shown in FIGS. 2-3 , the suction poppet 16 is positioned on the pump bulb opening 26 side of the suction annulus 28 such that the suction poppet 16 is biased to maintain flow in a single direction during inflation of the cylinders 4 . In one aspect, the suction poppet 16 further comprises a suction poppet spring 38 maintaining the suction poppet 16 in the engaged position to prevent flow through the valve flow path 14 without operation of the pump bulb 12 .
[0024] In one aspect, the suction poppet 16 further comprises an elongated head 40 extending through the suction annulus 28 and defining a lip 42 engagable by the plurality of fingers 34 when the suction poppet 16 moves toward the disengaged position limiting the travel distance of the suction poppet 16 and preventing the suction poppet 16 from engaging the annular ring 30 .
[0025] As shown in FIG. 2 , the cylinder poppet 18 also defines a sealing surface 44 engagable to the cylinder annulus 32 . The cylinder poppet 18 is also movable along the central valve chamber axis a-a between an engaged position in which the sealing surface 44 is engaged to the cylinder annulus 32 preventing flow of working fluid through the cylinder annulus 32 and a disengaged positioned allowing working fluid to pass through the annulus 32 . As shown in FIG. 2 , the cylinder poppet 18 is positioned on the cylinder outlet 22 side of the cylinder annulus 32 such that the cylinder poppet 18 is biased to maintain a flow direction from the reservoir 6 to the cylinder 4 during normal operation. In one aspect, the cylinder poppet 18 further comprises a cylinder poppet spring 45 to maintain the suction poppet 16 in the engaged position to prevent flow through the valve flow path 14 without operation of the pump bulb 12 .
[0026] In one aspect, the cylinder poppet 18 further comprises an elongated cylinder poppet shaft 46 and defines a lip 48 . In this configuration, the valve flow path 14 further defines a cylinder journal 50 defining a journal bore 52 for receiving the elongated cylinder poppet shaft 46 . The journal bore 52 guides the cylinder poppet 18 along the central valve chamber axis a-a during movement of the cylinder poppet 18 between the engaged and disengaged position such that the cylinder poppet 18 is prevented from moving along an axis transverse to the central valve chamber axis a-a. The cylinder journal 50 also engages the lip 48 of the cylinder poppet 18 when the poppet 18 moves to the disengaged position to limit the travel of the cylinder poppet 18 .
[0027] In one aspect, the suction poppet 16 can further comprise an elongated suction poppet shaft 54 extending through the cylinder annulus 32 . In this configuration the cylinder poppet 18 further defines a cylinder poppet bore 56 for receiving the elongated suction poppet shaft 54 . The cylinder poppet bore 56 guides the elongated suction poppet shaft 54 along the central valve chamber axis a-a during movement of the suction poppet 16 between the engaged and disengaged position such that the suction poppet 16 is prevented from moving along an axis transverse to the central valve chamber axis a-a. The elongated suction poppet shaft 54 can also be used to engage the end of the cylinder poppet bore 56 to push the cylinder poppet 18 into the disengaged position.
[0028] In operation, compressing the pump bulb 12 creates a positive pressure pushing working fluid and/or air within the pump bulb 12 out of the pump bulb opening 26 into the valve flow path 14 . The positive pressure also pushes against the cylinder poppet 18 moving the cylinder poppet 18 into the disengaged position forcing the fluid and/or air into the inflatable cylinder 4 . Releasing the compressed pump bulb 12 allows the pump bulb 12 to expand and creates a vacuum pulling the cylinder poppet 18 into the engaged position and the suction poppet 16 into the disengaged position allowing working fluid to be drawn from the reservoir 6 into the pump bulb 12 . The process can be repeated to continuously draw working fluid from the reservoir 6 to inflate the inflatable cylinder 4 .
[0029] In one aspect, the valve assembly 10 can further comprise a release button 58 for allowing fluid to flow in reverse through the valve flow path 14 . The release button 58 can be actuated to push against the elongated head 40 to push the suction poppet 16 into the disengaged position. In this configuration, the elongated suction poppet shaft 54 is adapted to engage the end of the cylinder poppet bore 56 to push the cylinder poppet 18 into the disengaged position. With both the suction poppet 16 and the cylinder poppet 18 are in the disengaged position with respect to the their corresponding annulus, the pressure of the working fluid within the inflatable cylinder 4 pushes working fluid through the valve flow path 14 back to the reservoir 6 .
[0030] As shown in FIG. 2 , a method of preventing vacuum lock up of the pump bulb 12 comprises positioning the suction poppet 16 positioned between the suction annulus 28 and the pump bulb 12 , wherein the suction poppet 16 further comprises an elongated head 40 extending through the suction annulus 28 . The method further comprises defining a plurality of fingers 34 extending from the suction annulus 28 to limit the travel distance of the suction poppet 16 to prevent uncontrolled engagement of the suction poppet 16 to other features within the valve assembly 10 .
[0031] While the invention is amenable to various modifications and alternative forms, specifics thereof have been shown by way of example in the drawings and described in detail. It is understood, however, that the intention is not to limit the invention to the particular embodiments described. On the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
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A dual poppet valve assembly for a pump assembly of an implantable penile prosthesis having a suction poppet engagable by a plurality of fingers allowing free travel of the poppet and to prevent vacuum lockup of the pump assembly. The suction poppet can also include an elongated shaft receivable within a corresponding bore of a cylinder poppet to prevent the suction poppet from becoming misaligned during the operation of the pump assembly.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application claims benefit under 35 U.S.C. 119(a) of Canadian Patent Application No. 2,907,245, filed Oct. 5, 2015, the entirety of which is incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates generally to building construction, and more particularly to the use of corrugated furring strips that are particularly useful in steel-framed cladded wall construction with a rainscreen, where potential benefits include reduced thermal bridging and improved ease of installation.
BACKGROUND
In commercial grade building construction, it is common to employ a multi-layered wall construction in which vertical steel studs are covered with an external sheathing layer, over which a series of metal Z-channels are installed with rigid insulation panels between them to define an external insulation layer, over which another series of metal channels (e.g. hat-channels) are then installed as furring to support the final exterior cladding layer at a spaced distance from the underlying insulation layer in order to create a rainscreen, whereby the resulting air space between the cladding and the insulation space allows drainage and evaporation to occur. This construction method is material and time intensive, requiring installation of the sheathing, addition of the Z-channels thereto, insertion of the insulation between the Z-channels, subsequent mounting of the hat-channels, and finally installation of the exterior cladding. In addition, each Z-channel creates a thermal bridge across the insulation layer over the full length of the channel, thereby reducing the effectiveness of the insulation layer.
Applicant has developed a new furring product and new resulting steel wall construction that addresses the forgoing shortcomings of the forgoing conventional steel wall construction technique.
SUMMARY OF THE INVENTION
According to a first aspect of the invention, there is provided, in combination, an upright wall structure, an exterior cladding for said upright wall structure, and a furring strip comprising an elongated strip of material that is corrugated with alternating lands and grooves in a longitudinal direction of said elongated strip, wherein the elongated strip is mounted to an exterior side of the upright wall structure in abutment therewith at the grooves of the elongated strip, and an interior side of the exterior cladding is mounted to the elongated strip at the lands thereof on an opposite side of an air space that is maintained between said exterior cladding and said upright wall structure by the elongated strip, whereby the elongated strip situates the exterior cladding across the air space from the upright wall structure to create a rainscreen that enables drainage and evaporation from behind the exterior cladding.
According to a second aspect of the invention, there is provided a finished exterior wall comprising:
a wall structure comprising:
a plurality of framing members; sheathing supported on the plurality of framing members; an insulation layer situated on an exterior side of the sheathing opposite to the framing members;
furring strips disposed externally of the insulation layer on an outer side thereof opposite the sheathing; each furring strip being corrugated with alternating lands and grooves in a longitudinal direction of said furring strip, the furring strips being oriented with the lands held outwardly away from the insulation layer and the grooves being recessed toward the insulation layer from said lands, and the furring strips being fastened to the framing members at the grooves in said corrugated furring strips; and
exterior cladding placed over, and fastened to, the lands of the corrugated furring strips, whereby the corrugated furring strips space the exterior cladding outwardly away from the insulation layer to create a rainscreen;
wherein the corrugated furring strips are abutted directly against the insulation layer with no intermediate disposed therebetween.
According to a third aspect of the invention, there is provided a method of assembling a finished exterior wall, the method comprising:
on a wall structure having a plurality of framing members, sheathing supported on the plurality of framing members, and an insulation space situated on an exterior side of the sheathing opposite to the framing members:
(a) installing corrugated furring strips externally of the insulation space on an outer side thereof opposite the sheathing with lands of the corrugated furring strips held outwardly away from the insulation space and grooves of the corrugated furring strips recessed toward the insulation space from said lands, including fastening the furring strips to the framing members at the grooves in said corrugated furring strips; and
(b) installing exterior cladding over the lands of the corrugated furring strips, whereby the corrugated furring strips space the exterior cladding outwardly away from the insulation space;
wherein step (a) comprises starting at one end of the wall structure, and in a single pass moving toward an opposing second end of the wall structure, inserting insulation material into the insulation space and periodically fastening the corrugated furring strips in place through inserted pieces of said insulation material prior to insertion of subsequent pieces of said insulation material into the insulation space.
According to a fourth aspect of the invention, there is provided a furring strip comprising an elongated strip of material that is corrugated with alternating lands and grooves in a longitudinal direction of said elongated strip, and has at least one longitudinal rib formed in said elongated strip.
According to a fifth aspect of the invention, there is provided a furring strip in combination with an upright wall structure, a plurality of fasteners by which the furring strip is mounted to said upright wall structure, and a plurality of washers respectively installed between the elongated strip and heads of said plurality of fasteners, wherein the furring strip comprises an elongated strip of material that is corrugated with alternating lands and grooves in a longitudinal direction of said elongated strip and the washers are less thermally conductive than the fasteners.
According to a sixth aspect of the invention, there is provided a furring strip in combination with a land-covering bridging member, the furring strip comprising an elongated strip of material that is corrugated with alternating lands and grooves in a longitudinal direction of said elongated strip, and the land-covering bridging member being arranged for mating with the furring strip in a position lying perpendicularly thereto with a cross-sectional profile of the land-covering bridging member conformingly overlying a respective land of the elongated strip and reaching downwardly into adjacent grooves on opposite sides of said respective land.
According to a seventh aspect of the invention, there is provided a furring strip in combination with a groove-occupying bridging member, the furring strip comprising an elongated strip of material that is corrugated with alternating lands and grooves in a longitudinal direction of said elongated strip, and the groove-occupying bridging member being arranged for mating with the furring strip in a position lying perpendicularly thereto with a cross-sectional profile of the groove-occupying bridging member received in a respective groove of the elongated strip.
BRIEF DESCRIPTION OF THE DRAWINGS
One embodiment of the invention will now be described in conjunction with the accompanying drawings in which:
FIG. 1 is an elevational view illustrating horizontal installation of corrugated metal furring strips to exterior sheathing during erection of a steel construction exterior wall.
FIG. 2 is an elevational view illustrating vertical installation of corrugated metal furring strips to exterior sheathing during erection of a steel construction exterior wall.
FIG. 3A is a plan view of an outside corner of the steel construction exterior wall of FIG. 1 .
FIG. 3B is a plan view of an inside corner of the steel construction exterior wall of FIG. 1 .
FIG. 4A is a plan view of an outside corner of the steel construction exterior wall of FIG. 2 .
FIG. 4B is a plan view of an insider corner of the steel construction exterior wall of FIG. 2 .
FIG. 5A is an isolated view of a bridging member that spans between the corrugated furring strips of FIGS. 1 and 2 in a position overlying matching lands of the two corrugated furring strips.
FIG. 5B is a cross-sectional view of the bridging member of FIG. 5A as taken along line B-B thereof.
FIG. 5C is a cross-sectional view of the bridging member of FIG. 5A as taken along line C-C thereof.
FIG. 6A is an isolated view of a support brace for providing auxiliary support to the bridging member of FIG. 5A at an intermediate location between the corrugated furring strips.
FIG. 6B is a cross-sectional view of the support brace of FIG. 6A as viewed along line B-B thereof.
FIG. 6C is a cross-sectional view illustrating the bridging member and support brace of FIGS. 5C and 6B in cooperative assembly with one another.
FIG. 7A is an isolated view of another bridging member that spans between the corrugated furring strips of FIGS. 1 and 2 in a position occupying matching grooves of the two furring strips.
FIG. 7B is a side view of the bridging member of FIG. 7A .
FIG. 7C is a cross-sectional view of the bridging member of FIG. 7A , as viewed along line C-C thereof, in combination with fasteners for attaching the bridging member to the corrugated furring strips.
FIG. 7D is a cross-sectional view similar to FIG. 7C , but showing the bridging member thereof in cooperative assembly with one of the corrugated furring strips.
In the drawings like characters of reference indicate corresponding parts in the different figures.
DETAILED DESCRIPTION
FIGS. 3A and 3B illustrate a construction of a steel framed externally insulated exterior wall using corrugated metal furring strips 10 to support the final exterior cladding layer 18 of the finished wall. The wall features a series of vertically upright steel studs 12 horizontally spaced apart from one another at regular intervals to form a structural framework of the wall, and a layer of exterior sheathing 14 fastened to the studs 12 at outwardly facing edges thereof. A layer of insulation 16 resides opposite the studs on the external side of the sheathing 14 , and may feature semi-rigid mineral wool, rigid insulation, insulation panels, structural insulated panels (SIP), or other thermal insulation. Each furring strip 10 is mounted opposite the sheathing 14 on the outer side of the insulation layer 16 , and is fastened to the studs 12 through the insulation layer 16 and underlying sheathing 14 . The finished wall is completed by the installation of cladding 18 over the furring strips 10 , which act to space the cladding 18 outwardly away from the underlying insulation layer 16 in order to create a rainscreen having an open airspace behind the cladding 18 for drainage and evaporation purposes.
Each corrugated furring strip 10 has a longitudinal direction in which its corrugated shape alternates between lands 20 and grooves 22 . In longitudinal planes parallel to the longitudinal direction of the furring strip 10 , the lands 20 are flat or linear in shape, and the grooves are trapezoidal. A floor or bottom 22 a of each groove 22 lies coplanar with the floors or bottoms of the other grooves, and parallel to the lands 20 , which are likewise coplanar with one another. The floor or bottom 22 a of each groove is obliquely joined to the two neighbouring lands 20 by angled side walls 22 b of the groove's trapezoidal shape. The furring strips 10 are installed in an orientation placing the floor or bottom 22 a of each groove against the outer side of the insulation layer 16 (i.e. the side thereof facing outwardly away from the interior space of the building). The lands 20 are thus held outwardly away from the insulation layer 16 by the angled side walls 22 b of the grooves, while the bottom 22 a of each groove is recessed toward the insulation layer from the lands 20 . To support the furring strips 10 , threaded fasteners 24 are driven through the furring strips 10 at select grooves 22 that align with the studs 12 of the wall's structural framework.
FIGS. 1 and 3 illustrate horizontal installation of the furring strips, in which case the longitudinal direction of each corrugated furring strips spans horizontally across multiple studs 12 and is accordingly fastened to more than one such stud. While the bottoms of the fastened grooves are held against the insulation by the fasteners, drainage and airflow vertically across the horizontal furring strip is allowed by the open space between the insulation and the lands 20 on both sides of each fastened groove.
FIGS. 2 and 4A -B illustrate vertical installation of the furring strips, in which case the longitudinal direction of each corrugated furring strip spans vertically along a singular studs 12 at a position aligned therewith across the insulation and sheathing layers, and so each furring strip is fastened only to a respective single stud at vertically spaced positions therealong. If the framework of the wall features bridges or blocks spanning horizontally between adjacent studs, furring strips may additionally be fastened to such components of the framework at grooves of the furring strips that align therewith. The open space between the insulation layer and each land enables airflow across the vertical furring strip to communicate the airspaces or cavities on opposite sides of each furring strip with one another.
To minimize thermal bridging between the interior and exterior of the finished wall, each threaded fastener 24 is fitted with a washer ( 26 ) of thermally insulative material that has lower thermal conductivity than the threaded fastener 24 and the corrugated furring strip, whereby the head of the fastener 24 is separated from the floor or bottom 22 a of the groove 22 by the washer 26 in order to thermally isolate the furring strip 10 from the fastener 24 . The fasteners 24 are the only members traversing the insulation layer 16 , thus reducing the amount of thermal bridging compared to conventional steel wall construction techniques in which Z-channels traverse the external insulation layer. Together with the insulative washers 26 that reduce conductive heat transfer from the fasteners 24 to the corrugated metal furring strips 10 , the insulation layer of the finished wall structure is particularly effective.
As shown in FIGS. 1 and 2 , the floor or bottom 22 a of each groove 22 in each furring strip 10 features a predefined fastener opening 28 having an oblong shape that is elongated in the longitudinal direction of the furring strip 10 . The width of the oblong shape (measured perpendicularly of the longitudinal direction along the minor axis of the oblong shape) slightly exceeds to the diameter of the threaded fasteners 24 to accommodate passage of the respective fastener 24 through the fastener opening without requiring drilling of the metal furring strip during installation. The length dimension of the fattener opening 28 measured in the longitudinal direction on the major axis of the oblong shape exceeds the width of the fastener opening in order to accommodate a degree of longitudinal adjustment of the fastener position along the floor or bottom of the groove to enable proper alignment of the fastener with a respective stud 12 of the wall framework in the case of horizontal installation of the furring strip 10 .
Each furring strip 10 features a pair of longitudinal ribs 30 at each land 20 , and a matching pair of longitudinal ribs at the floor or bottom 22 a of each groove 22 . The two ribs of each pair lie parallel to the central longitudinal axis of the furring strip 10 at symmetric positions on opposite sides thereof, and so each rib thus resides adjacent a respective side edge of the furring strip. The longitudinal ribs 30 are of radiused curvature in cross-sectional planes lying normal to the longitudinal direction, and serve to reinforce the strength of the corrugated strip. During manufacture, each strip may be pressed into its corrugated form from an initially flat strip-shaped blank, which for example may have been punched or cut from a larger metal sheet, and then punched in one or more operations to create the oblong fastener openings 28 and the longitudinal reinforcement ribs 30 . While the drawings show separation of the ribs on the floor of each groove from the ribs on the adjacent lands, i.e. a lack of illustrated connecting ribs on the side walls of the groove that join up with the ribs on the lands and the groove floors, the furring strip may alternatively feature full-length ribs continuously spanning the entirety of the strip from one end to the other. In such instance, the continuous full-length ribs may be pressed into the sheet or blank prior to forming thereof into the final corrugated shape.
FIG. 1 illustrates horizontal installation of the corrugated furring strips 10 during erection of a steel-framed, externally insulated wall. Here, the insulation layer 16 is formed by elongated rectangular insulation panels 32 that are mated together side-by-side in upright orientations over the underlying stud framework of the wall. Each furring strip 10 spans across a plurality of the insulation panels 32 and is fastened to the regularly spaced framework studs 12 through the insulation panels. To accomplish this, the insulation panels and furring strips 10 may be installed together during a single pass along the sheathed wall framework from one end to the other. Starting at one end, a first insulating panel, or first set of two or more insulating panels, are placed up over the sheathing, and then one of the furring strips is held up at a selected height and a first threaded fastener 24 is driven into a stud at this starting end of the sheathed wall structure through the underlying first insulation panel. At any subsequent studs likewise already covered by the initially placed insulation panel(s), a respective fastener 24 (accompanied by a thermally insulative washer 26 ) is driven into the stud 12 through insulation layer 16 at the respective groove 22 of the corrugated furring strip 10 . This placement and fastening of a corrugated furring strip is repeated at another height on the same wall at a positioned spaced from and parallel to the first strip, for example to accomplish the illustrated two-strip furring configuration of FIG. 1 . The next insulation panel (or next group of panels) is then inserted behind the furring strips and shifted back toward the first end of the wall framework in order to mate with the last inserted insulation panel at the upright side edge thereof, at which point the furring strips can be fastened into the next stud 12 through this latest insulation panel. These steps are repeated until the installer reaches the second end of the wall framework, where this same process can be repeated along the next side of the building until the full perimeter of the building has been furred.
FIG. 2 illustrates vertical installation of corrugated furring strips 10 . Here, the insulation layer 16 is again formed by elongated rectangular insulation panels 32 , but this time mated together in horizontal orientations stacked one atop the other over the underlying stud framework of the wall. Each furring strip 10 spans vertically across a plurality of the insulation panels 32 and is fastened to a respective singular stud 12 of the wall framework. Again, the insulation panels and furring strips 10 may be installed together during a single pass along the sheathed wall framework from one end to the other. Starting at one end, a first set of two or more insulating panels are stacked atop one another over the sheathing, and then one of the furring strips is aligned over the first stud at this first end of the sheathed wall framework and fastened into place using a series of threaded fasteners 24 driven into the first stud through the insulation panels at grooves of this first furring strip, again using the insulative washers 26 . At any subsequent studs likewise already covered by the first stack of insulation panel(s), an additional respective furring strip is likewise fastened in place in alignment with the respective wall stud 12 . The next set of insulation panels are then stacked up and mated side-to-side with the previous stack, with corresponding furring strips then respectively fastened to the studs residing behind this latest stack of insulation panels. These steps are repeated until the installer reaches the second end of the wall framework, where this same process can be repeated along the next side of the building until the full perimeter of the building has been furred.
In the forgoing installation processes, the insulation and furring strip are installed in conjunction and do not require two separate steps, substantial additional fasteners, adhesives or supplementary layers of additional metal framing or furring, as is traditionally required. Cladding is subsequently installed over the lands of the furring strips, whereupon the corrugated strips provide for a complete separation of cladding and substrate, and a full thermally-broken rain screen system is achieved.
As different types of cladding will vary in weight and required structural support, the fastening of the furring strips to the studs may alone be sufficient for some types of cladding, but not others. Accordingly, bridging members 40 , 42 may be used to perpendicularly interconnect two or more corrugated furring strips 10 as shown in FIGS. 1 and 2 to form a more rigid support grid for carrying the final cladding layer of the finished wall assembly. Use of the bridging members can also serve other purposes, for example to provide for additional fastening locations at areas other than the furring strips themselves, for example at panel joints or at locations of wall penetrations where mechanical, electrical or other protuberances are present or required.
FIG. 5 shows a first type of bridging member 40 configured to mate with the corrugated furring strips in positions overlying the lands 20 thereof, and is therefore referred to herein as a land-covering bridging member 40 . The land-covering bridging member 40 is an elongated metal channel of trapezoidal cross-sectional profile, which has a central span 44 and two side walls 46 extending obliquely downward from opposing sides of the central span. As best shown in FIGS. 5B and 5C , the thickness of each side wall 46 may be doubled up by bending of the channel back over itself at the lower end of the side wall 46 to increase the strength of the channel profile. The angle of divergence between the side walls 46 of the land-covering bridging member 40 matches the angle of divergence between the angled sides 22 b of the trapezoidal grooves 22 in the furring strips 10 , and the width of the central span 44 between the two side walls 46 of the land-covering bridging member 40 matches or slightly exceeds the width of each land 20 of the corrugated furring strips 10 . As a result, each land-covering bridging member 40 is matable with each furring strip 10 in a position embracing over a respective one of the lands and reaching downwardly into the two adjacent grooves 22 . In width, the side walls 46 of the land-covering bridging member 40 are equal to or slightly shorter than the side walls of the grooves 22 so that the land-covering bridging member 40 conforms to the underlying furring strip 10 , with the central span 44 of the land-covering bridging member 40 sitting flush atop the respective land 20 of the furring strip and the side walls 46 of the land-covering bridging member 40 likewise sitting generally flush atop the adjacent sides 22 b of the two neighbouring grooves 22 .
Placement of the land-covering bridging member 40 over a set of matching lands on the installed furring strips 10 places the land-covering bridging member 40 in a position spanning perpendicularly across the furring strips 10 . Each side wall 46 of the land-covering bridging member 40 features a series of vent holes 48 therein that are uniformly spaced apart in relatively close proximity over the full length of the land-covering bridging member 40 . Where these vented side walls of the land-covering bridging member 40 overlie the corrugated furring strips, the land-covering bridging member 40 can be attached to each of the furring strips by driving a respective self-tapping screw fastener 50 through the vent hole 48 in one or both of the bridging member's side walls into the angled side wall 22 b of the respective groove 22 of the furring strip 10 . Accordingly, the head of the screw fastener 50 resides within the groove 22 , and therefore does not project beyond the plane of the lands 20 and interfere with flush mounting of the cladding 18 against the gridwork of furring strips and bridging members. Other means of securing the land-covering bridging member 40 to the furring strips may be employed, for example using mating features built-into these components to provide a snap-lock fit or other self-locking attachment therebetween, for example similar that mentioned below for the groove-occupying bridging member.
While the described flush-mounted conformance of the land-covering bridging member 40 to the furring strips means that the land-covering bridging member 40 will be spaced from the underlying insulation layer 16 by at least the thickness of the furring strips 10 at the bottom of floor of the grooves, thereby allowing airflow across land-covering bridging member 40 from one side thereof to the other in the finished wall structure, the vent holes 48 in the side walls 46 improve this allowable airflow, while also allowing drainage. For strengthening purposes, the central span 44 of the land-covering bridging member 40 features a pair of symmetrically disposed longitudinal ribs 30 on opposite sides of the central longitudinal axis of the bridging member 40 , for example, just like those of the corrugated furring strips 10 .
The attachment of each land-covering bridging member 40 to the furring strips reinforces the mounting of the furring strips to the studs 12 in order to provide a substantially rigid support grid on which to the carry the cladding. Further reinforcement of the support grid can be provided by installation of the support brace 52 shown in FIG. 6 , which cooperates with the bridging member 40 at an intermediate position therealong between the furring strips 10 . The support brace 52 is similar to a short length of hat-shaped channel with short upturned retention tabs 54 on opposite sides of the channel-profile. The support brace 52 thus has a three-sided central rectangular channel 56 that opens downwardly, a pair of legs 58 that extend laterally outward from opposite sides of the open side of the channel 56 , and a respective upturned retention tab 54 at the distal end of each leg 58 . The coplanar legs 58 lying perpendicular the side walls of the central channel 56 define a base plane of the support brace 52 . In the installed position of the brace 52 , this base resides against a support surface defined by the outer side of the insulation layer 16 . The three-sided central channel 56 of the support brace 52 stands off from the base plane to one side thereof in order to abut against an underside of the central span 44 of the land-covering bridging member 40 , and thereby provide support to same.
The central span 44 of the land-covering bridging member 40 has recessed areas 60 therein at spaced apart positions along the member's longitudinal direction. These recessed areas 60 reside between the furring strips 10 in the final assembled state of the support grid. Each support brace 52 is placed beneath a respective one of these recessed areas 60 , and the height of the support brace 52 measured from the underside of the base legs 58 to the topside of the central rectangular channel 56 is generally equal to the distance from the plane of the outside surface of the insulation layer to the underside of the recessed area 60 of the land-covering bridging member 40 . Accordingly, the topside of the support brace's central channel 56 abuts against the recessed area 60 of the land-covering bridging member 40 . Each recessed area 60 features a predefined fastener hole 62 at a central location of the recess to enable driving of threaded fastener 64 through a corresponding aperture 63 in the central channel 56 of the support brace 52 and onward through the insulation layer 16 to a suitable anchor point in the wall framework (e.g. in a stud, or bridge/block thereof). The fastener 64 , shown in FIG. 6C , thereby couples the support brace 52 and overlying bridging member 40 together, and secures the same to the rigid wall framework. A thermally insulative washer 65 is again used with this insulation-piercing fastener 64 to minimize thermal bridging by thermally isolating the fastener 64 from the underlying bridging member 40 .
The upturned tabs 54 at opposing sides of the support brace 52 angle inwardly toward one another at an angle of convergence generally matching the angle at which the two side walls 46 of the land-covering bridging member 40 converge toward the central span 44 thereof, and the width of the support brace's base between the two tabs 54 generally matches the width of the open side of the land-covering bridging member 40 , as measured across the distal ends of the angled side walls 46 thereof. As shown in FIG. 6C , the land-covering bridging member 40 is placed over the support brace 52 into a position in which the recessed area 60 of the bridge member's central span 44 abuts flush against the topside of the support brace's central channel 56 , and the tabs 54 of the support brace clip externally over the bottom ends of the side walls 46 of the land-covering bridging member 40 below the vent holes 48 therein. Accordingly, the support brace engages to the underside of the land-covering bridging member in a snap-fit therewith that maintains the support brace in proper alignment beneath the recessed area 60 of the land-covering bridging member until the fastener 64 is driven through the aligned fastener hole 62 and aperture 63 in the two snapped-together components 40 , 52 .
FIG. 7 shows the other type of bridging member 42 which is also used to perpendicularly join two or more corrugated furring strips 10 together, as shown in FIGS. 1 and 2 , but does so at matching grooves 22 of the furring strips 10 , rather than at matching lands 20 thereof. This second bridging member 42 , therefore referred to as a groove-occupying bridging member 42 , is an elongated metal channel having a somewhat W-shaped cross-sectional profile. The cross-sectional shape features a downwardly opening three-sided rectangular channel 66 at its center, much like the support brace 52 of FIG. 6 , but instead of two flat legs extending perpendicularly outward from the sides of the central three-sided rectangular channel 66 , the groove-occupying bridging member 42 features two angled wings 68 extending obliquely upwardly and outwardly from the open lower side of the central three-sided rectangular channel 66 at acute angles from the two opposing side walls thereof. The angle at which the wings 68 diverge from one another is generally equal to the angle at which the two side walls 22 b of each groove 22 in the corrugated furring strips diverge from one another, and the width of the central three-sided rectangular channel 66 measured between the two angled wings 68 is generally equal to the floor-width of each such groove 22 .
Accordingly, as shown in FIG. 7D , insertion of the groove-occupying bridging member 42 into one of the grooves 22 with the central three-sided rectangular channel 66 opening downwardly acts to seat the groove-occupying bridging member 42 within the groove in a conforming manner, in which the two angled wings 68 of the groove-occupying bridging member 42 reside flush against the two side walls 22 b of the respective groove 22 . Each angled wing 68 features a respective set of apertures 70 therein near each end of the groove-occupying bridging member 42 . The distance between the two sets of apertures 70 in each angled wing 68 matches the distance by which two corrugated furring strips 10 are spaced apart from one another in the assembled support grid. Accordingly, a respective self-tapping fastener 72 can be driven through one or more of the apertures 70 in each set in order to fasten the groove-occupying bridging member 42 to the side walls 22 b of the grooves 22 in the furring strips. In addition to anchoring of each groove-occupying bridging member 42 to the respective corrugated furring strips with threaded fasteners, the bridging member 44 and furring strips may be arranged to self-couple to one another by way of a clip-like connection, for example through use of small tabs pressed into the bridging during manufacture, which can then be snapped into receiving openings on the furring members. This clipped snap fit connection would temporarily secure the two components together while the fasteners 72 are installed to form a more robust attachment between them.
Fastening of both types of bridging members 40 , 42 to the side walls of the grooves places all the fastener heads inside the grooves 22 , where they won't project beyond the plane of the lands 20 of the furring strip in the finished support grid. This prevents the fasteners from interfering with flush mounting of the cladding layer 18 atop the support grid in the final step of the wall construction. To enable driving of the self-tapping fasteners 72 perpendicularly through the angled wings 68 of the groove-occupying bridging member 42 and underlying angled side of the furring strip groove 22 without interference from the central rectangular channel 66 of the bridging member 42 , a respective fastener depression 73 is provided at the topside of the channel 66 at a position aligned with each fastener hole 70 in the wing 68 . The depression 73 slopes downwardly and outwardly away from the center of the rectangular channel's topside 66 a to the respective side wall 66 b of the rectangular channel, thus defining a recessed area at the corner of the three-sided central channel 66 . The depression or recess is sloped at an angle of ninety degrees to the plane of the respective wing 68 . Accordingly, each depression 73 defines a sloped pathway along which the respective fastener 72 can be driven through the wing 68 of the groove-occupying bridging member 42 at a proper ninety degree angle thereto. Each predefined fastener aperture 70 and its respective fastener depression 73 thus collectively define a fastening guide for driving the respective fastener 72 into the side of the furring strip groove 22 at the appropriate angle.
With reference to FIG. 7B , a series of notches or cut-outs 74 are provided at regularly spaced intervals over the length of the groove-occupying bridging member 42 at the bent corner between each angled wing 68 and the respective side wall of the central three-sided rectangular channel 66 . These act similar to the vent holes 48 of the land-covering bridging members 40 to improve the allowed airflow across the groove-occupying bridging member 42 within the assembled support grid. These notches or cut-outs 74 may be formed by punching holes into a flat metal blank along the intended bend lines on which the blank is subsequently folded during a pressing operation to create the cross-sectional profile of the groove-occupying bridging member 42 . This way, a single linear array of holes produces openings in both the angled wing 68 and the adjacent side wall of the central three-sided rectangular channel 66 .
A height of the central channel 66 of the groove-occupying bridging member 42 is equal to a height of depth of each groove 22 in the corrugated furring strips 10 such that the topside of the channel 66 resides flush with the coplanar lands 20 of the corrugated furring strip 10 in the installed position of the groove-occupying bridging member 42 , in which the open bottom side of the central channel 66 is seated against the bottom or floor 22 a of the respective groove 22 . This way, placement of a cladding layer 18 in abutment against the lands 20 of the furring strips 10 will likewise place the cladding layer 18 in abutment against the central channel 66 of the groove-occupying bridging member 42 for robust support of the cladding layer.
When reinforcement of the furring strips by bridging members is required, for example to ensure adequate support for the cladding layer that is to be installed over the corrugated furring strips, either the land-covering bridging members or the groove-occupying bridging members 42 , or a combination thereof, may be used to cooperatively form a more rigid support grid with the corrugated furring strips. FIGS. 1 and 2 illustrate use of both types of bridging members to span between parallel corrugated furring strips. FIG. 2 additionally shows the use of support braces 52 to further reinforce the land-covering bridging members 40 at intermediate points thereon between each parallel pair of corrugated furring strips 10 . Once the furring strips, and any optional bridging members, are installed over the insulation layer 16 , the cladding 18 can be placed up over the furring strips or support grid, and fastened thereto through the lands 20 of the corrugated furring strips 10 . Some of these lands 20 may be overlaid with the optional land-covering bridging members 40 , in which case a threaded fastener driven through the cladding 18 and into the corrugated furring strips is driven through the overlying bridging member 40 in the process, thereby further strengthening the fastened connection between the bridging member and the furring strip, and giving the cladding fastener more material to bite into to better support the cladding layer 18 .
In one example, the furring strips may be pre-formed light gauge, galvanized metal strip, 50 mm wide, 25 mm in height, and of any length limited only by ease of use and fabrication. The fasteners 24 by which the furring strips are mounted to the wall framework through the simulation may, for example, be full depth screws, c/w, 30 mm diameter phenolic washers to provide the described thermal break. Use of stainless or non-conductive fasteners will significantly reduce or eliminate thermal bridging at the exterior wall.
The land-covering bridging members 40 may be pre-formed 18-gauge galvanized metal strip, reinforced with rolled edges and the aforementioned radiused channels or ribs along its length. The recessed areas or localized depressions 60 may be spaced apart from one another at 406 mm or 610 mm intervals to match typical wall framing intervals at which the studs are spaced apart from one another, and the furring strips are preferably spaced apart by the same interval during installation so that each support braces reside centrally between two furring strips. The braces allow optional standalone installation of the land-covering bridging members in matching orientation to wall framing members (e.g. studs) behind the insulation layer. The land-covering bridging members may also be used to provide closures at corners of the building where different walls meet, for example by folding a land-covering bridging member around an outside corner of the building. This is shown in FIG. 1 , where broken line 100 denotes the interior side of the insulation layer of an “out-of-plane wall” that lies perpendicularly from the “in-plane” wall (i.e. the wall that features the solid-line insulation layer 16 residing “in the plane” of the drawing sheet). A folded land-covering bridging member 44 ′ overlies a half-land on each of the two illustrated corrugated furring strips 10 on the “in-plane” side of the building, and folds around a corner of the building to the “out-of-plane” side of the building, where the remainder of the folded bridging member 44 ′ overlies a half-land on each of another two corrugated furring strips. The half lands of the furring strips on the two sides of the building meet up with one another at the corner, and each side wall 46 of the folded bridging member 44 ′ resides on a side wall 22 b of the furring strip groove 22 that is nearest the building corner on each of the two furring strips on a respective one of the two adjacent sides of the building.
The groove-occupying bridging members may be pre-formed 18-gauge galvanized metal strip, with folds arranged to reinforce its cross-sectional profile, and may be configured to clip into the grooves of the corrugated furring members, and optionally further fastened with self-tapping fasteners. Even if the cut-outs or notches 74 were omitted from the groove-occupying bridging member, a drainage space is provided therebeneath by the thickness of the main furring strips in order to provide a complete rain screen regardless of the horizontal or vertical installation direction. Both types of bridging members are used for bridging or blocking of the furring strips to create an overall support grid, which provides additional strength, backing and/or blocking for variations in cladding orientation and sizes.
The support brace 52 may be pre-formed 18-gauge galvanized metal piece, 50 mm wide, with a folded profile to clip into the land-covering bridging members. The brace's profile allows for solid bearing of the base of the brace against the insulation/sheathing, and provides support directly under the top of the bridging member's central channel for fastening into the wall framing, similar to fastening of conventional strapping installations.
Although not detailed in the drawings, stretcher clamps may be provided, for example in the form of pre-formed light-gauge galvanized metal strip, 38 mm wide and 203 mm in length, and reinforced with radiused ribs or channels along its length. Three fastener locations are punched to allow for use in localized reinforcement of the corrugated metal furring strips 10 . These can be used in vertical orientations to match wall framing, or in horizontal applications, but only where blocking has been installed in wall framing to suit. Although not shown, adjustable clips may be provided for hidden fastener cladding installation. Such clips may be supported off of the lands of the primary furring strips, and off of one or both types of bridging members 40 , 42 in the horizontal furring installation format.
It will be appreciated that the specific material and dimensional details presented above are for exemplary purposes only, and may be varied without effect on the functionality of the present invention.
Since various modifications can be made in my invention as herein above described, and many apparently widely different embodiments of same made within the scope of the claims without departure from such scope, it is intended that all matter contained in the accompanying specification shall be interpreted as illustrative only and not in a limiting sense.
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Corrugated furring strips are used on the outer side of an exterior insulation layer in an exterior wall construction. The corrugated furring strips support a final cladding layer at an offstanding position from the insulation, thereby providing a rainscreen. The corrugated furring strips are fastened to the framework of the wall through the exterior insulation layer. Optional bridging members shaped to conformingly mate with lands and grooves of the corrugated furring straps cooperate therewith to define a support grid with improved load capacity for heavier cladding materials and more fastening location options. The insulation layer is free of any thermal bridges other than the insulation-penetrating fasteners used to support the furring and optional bridges. Thermally insulative washers isolate the furring and optional bridges from the fasteners to further improve the insulating effect of the wall.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to a method for making multi-layered shingles, and to roofing shingles made thereby. The shingles are uniquely thickened to enhance the appearance of a roof.
[0003] 2. Description of the Prior Art
[0004] There have been many approaches by the roofing industry to the task of covering a roof deck with shingles which are both protective and aesthetically pleasing. Whatever their appearance, suitable shingles have been made sufficiently durable and weatherproof for prolonged protection of the roof. The shingles' visual appeal has been attained in various ways, such as by providing particular butt edge contours and surface treatments which function to simulate more traditional, and in most cases more expensive, forms of roof coverings, including thatch, wooden shakes, slates, and even tiles of various forms.
[0005] Simulation of such more traditional roof coverings is afforded by asphalt shingles of the laminated type. These shingles provide depth or its appearance on the roof, thus more or less giving the look of the wood or other natural appearing shingles. U.S. Pat. No. 3,921,358 provides an example of such composite shingles. After describing the futile attempts in the past to achieve the irregular, bulky, butt edge profile and surface contour characteristic of wood roofing shingles, this patent presents an improved composite shingle comprising a rectangular sheet having a headlap portion and a butt portion. The butt portion is divided into a series of spaced apart tabs and a strip is secured to the sheet in a position underlying the tabs and filling the spaces therebetween. While the resultant bilaminate structure suggests somewhat the substantial and imposing architectural appearance of the more expensive roofing materials, such as wood shingles, the structure still diverges considerably in appearance from them.
[0006] For many years roofing manufacturers have offered a variety of two-layered shingles of the type disclosed in U.S. Pat. No. 3,921,358 in the attempt to present a thicker and more attractive appearance. A structure markedly different from these prior art bilaminate shingles is shown in U.S. Pat. No. 4,869,942. This structure, which has an exposed butt portion three layers in depth, with tabs two layers in depth, and an additional strip under the cut-outs, gives the shingle an appearance that goes well beyond the bilaminates in simulating wood and tile shingles.
[0007] Although the asphalt composite shingles have significant cost, service life and non-flammability advantages over wood shingles, the latter type are still seen by many to be a much more desirable roofing material for aesthetic purposes. A key reason for wood shingles' continuing aesthetic appeal stems from their greater thickness relative to the composite shingles, in spite of the many efforts in the past to simulate this thickness. Accordingly, it would be most beneficial to find ways to enhance the appearance of depth in the composite shingles without sacrificing these shingles' advantageous features.
OBJECT OF THE INVENTION
[0008] It is therefore an object of the invention to provide an asphalt shingle that simulates very closely the thickness of wood or other traditional roof coverings, and also possesses those attributes desired in roof coverings, including waterproofness, durability and fire-resistance.
[0009] It is a further object of the invention to enhance the appearance of a laminated shingle through the use of multiple layers of the butt portion of the shingle.
[0010] It is yet another object of the invention to provide a simple, efficient and economical manufacturing process for the continuous production of a laminated shingle from a single indefinitely long roofing sheet.
SUMMARY OF THE INVENTION
[0011] The foregoing and other objects of the invention have been achieved by a roof shingle which is multi-layered for enhancement of the shingle's visual appeal and thickness. The composite shingle comprises a headlap portion and a butt portion having three or more layers. The headlap portion may also be multi-layered, comprising two or more layers. The butt portion is divided into a series of spaced apart tabs. The spacing between the tabs significantly exceeds that of the slots which have been formed over the years in the manufacture of multi-layered shingles, such as those disclosed in U.S. Pat. Nos. 5,209,802 and 5,426,902. Such narrow openings, which are typically less than one inch, e.g., about ¼ to ⅝ inch, do not provide the openly spaced and particularly deep wells of a roof surfaced by the shingles of the present invention. The spacing between the tabs of the inventive shingles is greater than 1 inch, preferably greater than 2 inches.
[0012] The multi-layered shingle is of the laminated type. The butt portion of this shingle composite is made of at least three laminae, and may have four, five or more laminae. The laminae are preferably constructed of felted material comprising organic or inorganic fibers or a mixture of both. The fibers are usually held together with a binder and are coated, saturated, or otherwise impregnated with an asphaltic bituminous material. The laminae lie one above another in the composite, and are exposed to view as a bulky composite when the shingle is installed on a roof. Inherent in this laminated construction is an appreciable difference in surface elevation between the top surface of the tabs of one shingle and the top surface of the tabs of the underlying shingle(s). The perception of depth is greatly magnified when the array of shingles on the roof is viewed. The viewer's eye will naturally go from the deep wells formed by the adjoining tabs of one shingle to those of the next upper or lower shingle(s) and so forth over the roof.
[0013] A preferred laminate manifesting the inventive shingle's unique structure, incomparable to any of the prior art, comprises an asphalt shingle having a headlap portion and a butt portion which extends from the lower boundary of the headlap portion to the butt edge of the shingle and comprises a series of composite tabs which are separated by spaces, each extending from the side edge of one composite tab to that of the next adjacent composite tab, and each of which comprises at least three layers. The type of laminated shingle consisting of a single overlay member and a single underlay tab is well-known and illustrated, for example, in U.S. Pat. Nos. 3,998,685 and 5,052,162.
[0014] In accordance with the process of the invention, one or more fibrous sheets, which are to be made into the shingles, are treated with a cementitious waterproofing composition, such as asphalt or other bituminous material. The treatment includes surfacing the sheet or sheets with sufficient waterproofing material to which is adhered granules such as crushed rock, slate or other surfacing material. While the entire outer face of the shingle, i.e. the face which is uppermost when the shingle lies on a roof, is desirably covered over its full extent with granular matter, the portion of the outer face which is important for colorful effects is that portion which is exposed to view when the shingles are laid together in overlapping courses on a roof. Accordingly, the sheet portions which ultimately become these exposed portions are profitably surfaced with colorful granules so as to provide areas of distinctive coloration, and lower cost, less decorative granular material is employed to surface the sheet portions which are to become the covered or hidden areas of the final assemblage.
[0015] The process is advantageously carried out continuously with the sheet(s) being transported along a production line for sequential processing. The continuous process is especially useful in the production of laminated shingles from a single elongate sheet. In the process, the top surface of the sheet is coated with asphalt and a coating of granules is applied to this surface. At least two narrow elongate sheets or strips are cut from the total elongate sheet to yield a main sheet and the narrow portions cut therefrom. The narrow elongate sheets are desirably cut from the main sheet in one step, although the cuts may be made in more than one step. The narrow sheets are positioned one above another and below the main sheet. A laminate of the main and narrow sheets is formed.
[0016] Desirably, each narrow sheet is coextensive with the other or others, and the narrow sheets are positioned so that the side edges of each one are in the same vertical plane as the respective side edges of the other(s) lying above and/or below. The first narrow sheet moved directly below the main sheet is centered on the longitudinal line which will become the central line of the multi-layered portion of the total composite sheet before cutting of this total sheet. Each succeeding narrow sheet is centered on the narrow one above it. After centering, each cut-off sheet is adhered to the sheet above it to form a composite. Each cutoff sheet may or may not be inverted before adhesion. In the formation of an advantageous embodiment, the last adhered sheet is inverted. When the bottom sheet is thus inverted, the final multi-layered tab portion of the resultant roofing shingle has exposed granules on both its top and bottom. The eventual shingle's butt edge is thickened by the multiple layers and their protruding granules, leading to an assembly of the shingles on a roof which has the aesthetically attractive, bulky look of a roof of wood or tile shingles.
[0017] A longitudinal cut is made along the centerline of and within the side boundaries of the multi-layered portion of the totally laminated composite sheet advancing along the production line so as to form two complementary sheets, each individually having multi-layered tabs separated by cut-out portions along the thus cut longitudinal edge. The cut defines a substantially zigzag or “dragons' teeth” configuration comprising a series of interdigitated tabs on each complementary sheet. This side-edge arrangement is of the type described in U.S. Pat. No. 5,052,162. Each resulting composite sheet is cut transversely into shingles of preselected lengths. The zigzag cut desirably forms a series of tabs which differ from one another in each individual shingle so as to create a wooden shake simulation. The final shingle may thus be made from a single sheet, e.g., glass mat, by a process which converts this sheet into a plurality of shingles having multi-layered tabs, each layer being made of a portion of the original sheet. This multi-level roofing shingle is more visually appealing than previous bi-level shingles because of its thicker butt edge. This look of thickness is especially manifest when the shingles are arrayed in rows on a roof and the shingles of each row act like levers lifting the butt edges of the row above and so forth over the entire roof.
[0018] An important aspect of the present invention is that it permits laminated shingles having multi-layered tabs, such as those of three layers, to be manufactured continuously and expeditiously from a single sheet(s) of an indefinite length. Each of the steps involved in the formation of the final roofing shingles can be carried out on the base roofing material (e.g., glass fiber mat) as the material advances continuously along the production line in the form of an elongate sheet and strips cut therefrom. The continuously performed steps comprise waterproofing the sheet, coating it with mineral granules, cutting it along its length into elongate strips, laminating these strips together to form a composite multi-level strip, and finally cutting the composite laminated strip into the individual roofing shingles. The granules may be applied before or after the sheet is cut into elongate strips, as described, for example, in U.S. Pat. No. 4,869,942, and may be applied to only a portion of the main sheet or narrow strips. A different coloration may be applied to the main sheet and strips.
[0019] In a preferred embodiment of the invention, trilaminated shingles are continuously produced from a single elongate sheet which is waterproofed and coated over its top surface with mineral granules before being cut into elongate strips. Two first straight cuts divide the sheet into three elongate rectangular strips, one much wider than the other two. Advantageously, one of the straight cuts is made near one of the side edges of the original elongate sheet, and the other straight cut is made near the original sheet's opposite side edge. One of the two narrow strips is shifted, without being inverted, to a position underneath the wide strip and the two strips are laminated together. Prior to lamination, the upper strip's undersurface which is to be bonded is advantageously coated with an adhesive material. Additionally, in another embodiment, the lower strip is turned upside down before lamination so that the laminate of the two strips has the granules of the top strip facing upwardly and the granules of the bottom strip facing downwardly. The second narrow strip is shifted underneath and laminated to the bi-level portion formed in the first lamination. Preferably, the undersurface of the bi-level portion is coated with an adhesive and the second narrow strip is turned upside down before lamination so that the total composite will have granules on both the top and bottom of the three-layered, laminated section.
[0020] A third cut is made (i) alternately across and generally along the centerline of the tri-level section (i.e., multi-layered portion) formed by the two previous laminations and (ii) within the longitudinal side boundaries of this section. This central cut, which divides the sheet into two elongate parts, is made to form a repeating pattern of interdigitating triply thick tabs so that upon separation each part has a long straight edge along one side which is one layer in thickness and alternating triply layered tabs and cut-out portions along the other side. Each of the narrow strips, which were positioned to underlie the uppermost wider strip, is desirably cut to be wide enough to completely cover the underside of the wider strip's tabs, but not so wide as to extend much toward the long straight edge of the wider strip. The width is desirably sufficient to adequately support the overlying shingle portion and to contribute to ease of production in the continuous manufacturing process. The two elongate laminated sheets are finally cut into suitable lengths for shingles and packaged. This final cutting may be accomplished conveniently just about when the third longitudinal cut is made or thereafter.
[0021] The continuous process thus provides a unique shingle structure having alternating tabs, three layers in depth and cut-outs therebetween. Like conventional bilaminates, this structure comprises a rectangular sheet having headlaps and butt portions. When these prior art and inventive laminated shingles are installed in successive offset courses in separate arrangements on a roof, their butt edge portions are exposed to view. Because the inventive trilaminated shingle's butt portion is three layers in depth, with the tabs and cut-outs three layers deep, the shingle presents, through this unusual enlargement of the butt portion, a bulky appearance that very closely approaches that presented by wood and tile shingles.
DESCRIPTION OF THE DRAWINGS
[0022] The invention will now be described with reference to the accompanying drawings in which:
[0023] [0023]FIGS. 1 and 3 are schematic elevational views of one form of apparatus whereby laminated shingles may be manufactured according to this invention;
[0024] [0024]FIG. 2 is a top plan view of a sheet of fibrous material partially coated with granules in accordance with the invention;
[0025] [0025]FIG. 4 is a perspective view of the top and two bottom sheets laminated together;
[0026] [0026]FIG. 5 is a perspective view of the novel roofing shingle of the invention; and
[0027] [0027]FIG. 6 is a perspective view of an assembly of the shingles of the invention as applied on a roof.
DETAILED DESCRIPTION OF THE INVENTION
[0028] Referring now to the drawings and more specifically to FIGS. 1 and 3 thereof, there is shown diagrammatically an overall process for forming multi-layered roofing shingles according to the instant invention. A rectangular sheet or web 10 of an indefinite length is unwound from a roll (not shown) and fed along the production line. Sheet 10 is preferably a mat of glass fibers but may also be fabricated from organic felt or other types of base material. The glass mat is generally about 38 to 48 inches in width, although other widths can be chosen without departing from the scope of the invention. The sheet generally weighs from about 1.35 to 3.00 lbs/100 ft. 2
[0029] After sheet 10 is fed over a series of loopers 11 - 14 and between a pair of tension rollers 15 and 16 for uniform tensioning, it is then passed to a station for the application of filled asphalt coating. Discharge pipe 17 supplies a layer of the asphalt coating 18 to the upper surface of sheet 10 just before the nip of rotating rolls 19 and 20 . Reservoir 21 is placed below the coating area to capture runover asphalt from the operation for application to the sheet by back coating roll 20 immersed in the asphalt of reservoir 21 . Nip rolls 19 and 20 coact to apply the appropriate weight of asphalt coating to the sheet, with the nip of the rolls providing pressure to ensure that the asphalt has impregnated the sheet properly. Heating units 22 keep the coating asphalt at the proper temperature for application.
[0030] Downstream of roll 20 is another back coating roll 23 , which is also immersed in reservoir 21 for pickup of liquid asphalt and deposition on the back surface of sheet 10 . Sheet 10 may be coated by both rolls, as shown in FIG. 1, or it may be subjected to a single treatment by one or the other of the rolls. Excess asphalt is advantageously wiped from the surface of the back coating roll(s) by a doctor knife(s) 24 or the like, installed on either or both sides of the back coating roll(s) to ensure uniform application and avoid excesses of the asphalt. Downstream of the back coating application there is a doctor blade or knife 25 or the like which removes excess coating from the back or under surface of sheet 10 . Sheet 10 is further acted upon by a smoothing roll 26 and a carrier roll 27 , which rolls are generally heated.
[0031] Stabilized asphalt coating 18 suitably has a softening point as measured by ASTM D 36 of from about 195° to 260° F., more preferably from about 215° to 235° F., and is usually applied in an amount from about 50 to 70 pounds, more preferably from about 55 to 65 pounds, per 100 square feet of sheet 10 . The coating is advantageously maintained at about 380° to 450° F. before application to the sheet.
[0032] After the coating step and while the coating material is still hot, soft and tacky, coated sheet 10 passes beneath surfacing apparatus 28 from which decorative granules are deposited on the upper surface of the sheet. Apparatus 28 includes a series of bins filled with mineral granules and positioned above the longitudinally moving sheet. This known type of roofing machinery is equipped for selectively depositing the mineral granules contained in the bins onto the adhesive upper surface of sheet 10 . Apparatus 28 is outfitted with enough bins to hold each collection of granules to be applied to the sheet in the formation of the overall color pattern being developed on the sheet.
[0033] In the mineral granule treatment schematically shown in FIG. 2, sheet 10 is moving longitudinally under apparatus 28 in the direction of the arrow. The granule deposition can be understood with reference to the lines extending longitudinally and transversely over the surface of sheet section 29 , as shown in FIG. 2. The three solid lines running longitudinally between the two side edges of the sheet correspond to the cuts to be subsequently made in the formation of the component laminae of the shingle, as set forth below. It is seen that there will be two straight cuts and one zigzagged cut. The cutting pattern of FIG. 2 is merely one of many such patterns which could be used to produce the component laminae. The two dashed lines extending lengthwise to either side of the zigzagged line do not correspond to eventual cuts but, in conjunction with the other four straight and parallel lines extending lengthwise, including the side edges, demarcate five zones which are designated zones A-E. As indicated in FIG. 2, the widths of the zones across sheet 10 are as follows: zones A and E- 7 ″; zones B and D- 5 ″; and zone C- 14 ″. These five zones extend over the entire length of sheet 10 . The overall width of sheet 10 as well as the number and widths of the zones can vary depending on factors such as the capacity of the apparatus and the number and size of the shingles being produced per unit length of the sheet.
[0034] The granule discharges which are applied onto the five zones of section 29 are made from the above-mentioned bins of apparatus 28 . The bins are contained in two applicator compartments, a so-called blend box 30 and spill box 31 . In progressing along the production line, sheet 10 first passes under applicator box 30 which deposits granules onto zone C, and then under applicator 31 , which deposits granules onto all of the zones. As shown in FIG. 2, the far right side of section 29 of sheet 10 has passed under both applicator boxes 30 and 31 and thus has granules covering all of the zones, while the left-hand side, having passed under only applicator box 30 , has the granules covering only zone C. As sheet 10 progresses further along the production line, the uncovered zones of section 29 will, of course, become covered by granules discharged from applicator box 31 .
[0035] In a preferred embodiment of the invention, the roof's exposed layers from zone C are in the form of an effectively random series of differently colored portions. To form this random pattern in zone C, applicator (blend) box 30 is equipped with a group of bins, each of which contains variously colored granules for application to zone C. The contents of each bin advantageously consist of blends of the colored granules. The deposition of blends is found to protect against the surface flaws encounterable with the use of singly colored granules. There must be a sufficient number of these bins to produce a random look on the covered roof surface. Suitably, there are at least four such bins each holding different color blends of mineral granules. Applicator box 30 of FIG. 1 has four such bins from which the blends of the contained mineral granules are selectively dropped onto the upper surface of sheet 10 as it passes beneath these bins. The average of the colored granules found in these four bins is contained in a bin of applicator box 31 for the follow-up treatment of zone C described below. This average or composite of all the colored granules not only adds an aesthetically pleasing color variation but also permits the utilization of the inevitable accumulation of the spilled granules from the other bins.
[0036] The selective dropping of mineral granules from the bins of applicator box 30 results in deposited bands of mineral granules (so-called “color drops”) on zone C. The first four such bands of FIG. 2, which are designated C 1 through C 4 , are bordered by dotted lines L extending across zone C. The deposition from applicator box 30 is interrupted at various randomly located places along zone C, yielding spaces designated S, which are uncovered by granules.
[0037] After its passage under applicator box 30 , sheet 10 next passes under applicator (spill) box 31 , which is divided into a number of bins supplied with granular material and equipped for the simultaneous application of the granules across sheet 10 to complete the coverage of zones A to E. One of these bins continuously delivers to zone C a blend of colored granules which represent the average of the granules deposited from the four bins of applicator box 30 . The spaces designated S of zone C become covered with this average blend. Additionally, granules of this blend fill in any spots left uncovered in bands C 1 to C 4 after the surfacing by applicator box 30 .
[0038] Applicator boxes 30 and 31 thus together provide on zone C a series of color drops or bands C 1 through C 4 and S, each band having a variable length and a color which contrasts with the color of the mineral granules in the bands adjacent thereto in the completely granule-covered sheet. In the embodiment illustrated in FIG. 2, each of the color drops onto each of zones C 1 , C 2 , C 3 and C 4 (bounded by a pair of dotted lines) is about 11 inches lengthwise along sheet 10 . Applicator boxes 30 and 31 are operated to alternate the color drops from the five mineral granule bins in an effectively random fashion. The term “effectively random fashion” is used since the machinery is constructed to set up a pattern of alternating color drops which for the FIG. 2 embodiment is repeated only after 36 such color drops. This 36 drop cycle results in a pattern of such color drops which, for practical purposes in the final roof covering of the invention, is undetectable visually from an entirely random, nonrepeating pattern.
[0039] As shown in FIG. 2, the first six designated color blends or bands from the five granule-containing bins of applicator boxes 30 and 31 discharging onto sheet 10 are C 1 , S, C 2 , S, C 3 and C 4 in order from right to left. Color drop S, which constitutes the average color blend which would result from a combination of the colored granules of drops C 1 , C 2 , C 3 and C 4 , is applied twice from its bin in this group of six drops. As sheet 10 advances, applicator boxes 30 and 31 apply this same group of six color blends, viz. C 1 to C 4 and S (deposited twice), as a set over and over to zone C but with the sequence of the six drops changed from each set to the next. After the application of six differently ordered sets or a total of thirty-six color drops, the cycle of these six sets is repeated on and on over the entire length of sheet 10 . The result of this coloring process is an effectively random, nonrepeating color pattern on the shingles' overlying laminae derived from zone C.
[0040] Applicator box 31 is further equipped with one or more bins for application, simultaneously with the application of the continuous layers of granules to zone C of continuous layers of granules to zones A, B, D and E. As will hereinafter be understood, the material of the latter four zones form portions which are not visible in the completely constructed and installed shingles of the invention. Accordingly, the granules deposited on these four zones suitably are low cost materials.
[0041] As illustrated in FIG. 1, after the stream of granules is discharged from applicator box 31 onto sheet 10 , the sheet goes around a slate drum 32 which functions to embed the granular material in the top asphalt coating. In the continued passage of the surfaced sheet 10 , excess granules fall off from the sheet into applicator box 31 from which they are reapplied onto the sheet. The back of the sheet then comes under hopper 33 containing fine back-surfacing material, such as talc, mica dust, fine grit, sand or other composition capable of rendering the back of the sheet non-cementitious. The material from hopper 33 is uniformly distributed over the back of the sheet by means of a distributing roll 34 . The coated roof sheet at this point generally weighs from about 80-100 lbs/100 ft. 2
[0042] Sheet 10 next passes through a cooling section 35 which may simply involve a water spray or a series of cooling rolls 36 around which sheet 10 is looped. At the finish looper station 37 , the sheet is fed over a series of rolls 38 which control its speed as it advances to the slitting station (see FIG. 3). After embedment of the granular material on sheet 10 by slate drum 32 and prior to slitting of the sheet, adhesive strips (not shown) are desirably applied to the front or back of the sheet. In the final roof covering, this adhesive material acts as a self-sealing means for attaching the shingles in one horizontal course to those in the next upper or lower course. At this interval during shingle production, release tape (also not shown) should be affixed to those sheet portions which in the finished and packaged shingles will come in contact with the above-mentioned adhesive strips of adjacent shingles. Sticking in the package is thereby prevented.
[0043] As shown at the right-hand side of FIG. 3, the cooled sheet is pulled by rolls 40 and 41 and divided lengthwise at a slitting station 39 , utilizing two cutters, into three portions, a wide sheet 10 a and two narrow sheets 10 b and 10 d . The cutting may be accomplished by any suitable means, such as by cutting wheels. More than two cutting wheels could be utilized for the production of shingles having four or more layered tabs. Advantageously, the original 38 inch wide sheet of the preferred embodiment of FIG. 2 is cut along the lines separating zones A and E from the remainder of sheet 10 or more specifically from zones B through D. Accordingly, for this embodiment, slitting station 39 cuts sheet 10 into a sheet 10 a (zones B through D) which is 24 inches wide and two sheets 10 b (zone A) and 10 d (zone E) which are each 7 inches wide. At this point both the main sheet 10 a and the narrow strips 10 b and 10 d have granules embedded on their upper surfaces.
[0044] Sheets 10 a and 10 b are pulled and guided along by conventional rollers 42 - 44 . The wide sheet 10 a is fed over a back coater 45 which comprises a tray 46 containing adhesive, such as asphalt, and a drum 47 , whose lower surface rotates in the adhesive-containing tray 46 . Drum 47 applies adhesive from the tray to the back side of zone C of the wide sheet 10 a to form an adhesive coating zone about the width of the narrow strip 10 b (zone A) or 10 d (zone E), e.g., about 7 inches wide, to receive strip 10 b . The adhesive may be applied as a continuous layer or as strips.
[0045] Strip 10 b passes up over a guide bar 48 and then across to another guide bar 49 . In its passage from guide bar 48 to guide bar 49 , strip 10 b is shifted underneath strip 10 a so that the centerline of the narrower strip is below and coincident with the centerline of zone C of the wider strip. With their centerlines so aligned and their granule-covered surfaces both facing upwardly, the two strips are brought into contact and strip 10 b is pressed against the adhesive-coated underside of main strip 10 a by laminating rolls 50 to form a composite 10 c of the two strips. In a further embodiment of the invention, strip 10 b is twisted in its passage from guide bar 48 to guide bar 49 so that its bottom without granules faces upwardly for bonding to the back side of strip 10 a . This results in the formation of a laminated composite of the two strips having one layer of granules surfacing the composite's upper surface and another layer of granules surfacing the lower surface of strip 10 b.
[0046] Trilaminate 10 e of the invention is formed by essentially repeating the process carried out in forming bilaminate 10 c , as shown in FIG. 3. The wide sheet composite 10 c is fed over a back coater 45 ′ comprising an adhesive-containing tray 46 ′ and a drum 47 ′. Drum 47 ′ applies the adhesive, e.g., asphalt, to the downwardly facing, backside surface of strip 10 b (original zone A) which constitutes the lower surface of the laminated portion of sheet 10 c.
[0047] Strip 10 d passes up over a guide bar 48 ′ and then across to another guide bar 49 ′. In its passage from guide bar 48 ′ to guide bar 49 ′, strip 10 d is twisted so that it is turned upside down (180°) and its back without granules faces upwardly for bonding to the laminated portion of the backside of strip 10 c . Strip 10 d is then shifted underneath strip 10 c so that the centerline of the narrower strip is below and coincident with the centerline of the wider strip 10 c . With their centerlines so aligned, the two strips are brought into contact and the asphalt coated underside of strip 10 c is pressed against the top side (originally bottom side) of narrow strip 10 d by laminating rolls 50 ′ to form a composite 10 e of the two strips having one layer of granules surfacing the composite's upper surface and another layer of granules surfacing the lower surface of strip 10 d . By instead again carrying out the embodiment involving not twisting the lower laminae, a trilaminate will result with granules on the composite's upper surface and the upper surface of each lower layer.
[0048] As shown in FIG. 3, laminated combination 10 e is fed into a cutting station 51 which is equipped to make one lengthwise cut along this laminate. The cutter suitably comprises a lower cutting wheel and an upper anvil roll. The path of the lengthwise cut is illustrated in FIG. 4. While it is not illustrated in FIG. 4, cutting station 51 also profitably makes transverse cuts in laminate 10 e to form the individual inventive shingles, one of which is shown in FIG. 5. In FIG. 4, the centerlines of strips 10 b and 10 d are shown aligned with the centerline of main sheet 10 a and the lengthwise cut performed at cutting station 51 is shown as an angularly offset line forming tabs 52 and 52 ′. The cut separates the laminated sheet 10 e into two lengthwise parts 10 f and 10 g , which comprise two complementary, interlocking-tab strips, each of which is cut transversely of its length into shingles of the desired length by transverse cutters or any other suitable cutting mechanism. An appropriate length F for each shingle is 40 inches, as shown in FIG. 2 for two portions of sheet section 29 . In a preferred embodiment, all shingles cut from strip 10 f have the same shape and all those cut from strip 10 g have the same shape, and the average surface area of all the shingles cut from strip 10 f is the same or approximately the same as that of all the shingles cut from strip 10 g.
[0049] With reference to zones A to E of sheet 10 shown in FIG. 2, it is seen that the topmost layers of strips 10 f and 10 g are derived from zones B, C and D, and the underlying layers are derived from zones A and E. Each of strips 10 f and 10 g has tabs which are three layers thick because of the previous laminations of zones A and E underneath the central portion of zones B, C and D. Advantageously, strips 10 f and 10 g are each 12 inches wide or greater. The resulting shingles are conveyed for packaging to stations 53 and 53 ′.
[0050] [0050]FIG. 5 shows a perspective view of a final shingle 54 with an upper main sheet 55 having granules 56 on top and two strips 57 , 57 ′ adhered along the angularly shaped edge thereof. Strip 57 ′ has exposed granules on its side facing downwardly. As shown in FIG. 5, shingle 54 comprises a headlap portion 58 , which is approximately rectangular in shape, and a butt portion 59 , which is divided into the series of spaced-apart tabs 52 which are integral with and extend from the headlap portion 58 . A lower longitudinal section of headlap 58 is seen to form part of the top layer of the tri-level portion of shingle 54 . The tabs 52 are spaced apart from each other at a distance which will ensure that a considerable portion of an underlying tab(s) will be viewable when an array of the shingles is installed on a roof. The spacing between the tabs may vary and is preferably greater than two inches and more preferably is greater than 2½ inches, such as from about 3 to 7 inches. The tabs 52 may be of equal and/or unequal widths and each width typically is in the same range as that of the spaces therebetween. The tabs may have various shapes.
[0051] [0051]FIG. 6 illustrates a roof covered with a plurality of successive offset courses of laminated shingles 54 . The triply thick marginal edge of the butt portion of each shingle of a given course abuts the likewise triply thick marginal edge of the adjacent shingle of that course. Furthermore, as illustrated in FIG. 6, the shingles of a course 60 are offset from the shingles of an immediately subjacent course 61 by a first longitudinal distance and the shingles of course 61 are, in turn, offset from the shingles of the next immediately subjacent course 62 by a second longitudinal distance, the first and second longitudinal distances desirably being unequal to each other. The longitudinal distances may be equal and/or unequal over the entire surface of the roof.
[0052] The respective courses of shingles of the FIG. 5 embodiment may be offset from each other at any distance less than the length of a shingle and such distance may be varied at random without adversely affecting the appearance of the ultimate roof covering. Contrarily, the arrangement of the inventive shingles on a roof produces an appealingly variegated look with strikingly deep wells throughout the extent of the roof. As is evident in FIG. 6, a view of the exposed lower edges of the butt portions of shingles of one course in conjunction with the directly lower exposed butt edges of the shingles of a successive course reveals thicknesses which are three times (see 63 ) and six times (see 64 ) greater than the thickness of the granule-covered sheet material from which the shingles are made.
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A multi-layered shingle adapted to be positioned with other similar shingles in an overlapping arrangement on a roof to yield a simulated wooden shake roof covering comprising a headlap portion and a butt portion. The butt portion comprises a series of multi-layered tabs. All the tabs have the same number of layers and each multi-layered tab (a) is separated from the next adjacent multi-layered tab or tabs by a space or spaces, respectively, and (b) comprises an uppermost layer and at least two layers underlying the uppermost layer. Each underlying layer is laminated to the layer above it to form a multi-layered laminated composite. The laminated composite is integral with the headlap portion and the top surface of the uppermost layer of each tab is coplanar with the top surface of the headlap portion. The invention also includes an apparatus and a process for the continuous manufacture of the shingles of the invention.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] Embodiments of the present invention generally relate to tools and methods for hanging and/or expanding liner strings.
[0003] 2. Description of the Related Art
[0004] In wellbore construction and completion operations, a wellbore is initially formed to access hydrocarbon-bearing formations (i.e., crude oil and/or natural gas) by the use of drilling. Drilling is accomplished by utilizing a drill bit that is mounted on the end of a drill support member, commonly known as a drill string. To drill within the wellbore to a predetermined depth, the drill string is often rotated by a top drive or rotary table on a surface platform or rig, or by a downhole motor mounted towards the lower end of the drill string. After drilling to a predetermined depth, the drill string and drill bit are removed and a section of casing is lowered into the wellbore. An annulus is thus formed between the string of casing and the formation. The casing string is temporarily hung from the surface of the well. A cementing operation is then conducted in order to fill the annular area with cement. The casing string is cemented into the wellbore by circulating cement into the annulus defined between the outer wall of the casing and the borehole. The combination of cement and casing strengthens the wellbore and facilitates the isolation of certain areas of the formation behind the casing for the production of hydrocarbons.
[0005] It is common to employ more than one string of casing or liner in a wellbore. In this respect, the wellbore is drilled to a first designated depth with a drill bit on a drill string. The drill string is removed. A first string of casing is then run into the wellbore and set in the drilled out portion of the wellbore, and cement is circulated into the annulus behind the casing string. Next, the wellbore is drilled to a second designated depth, and a second string of casing or liner, is run into the drilled out portion of the wellbore. If the second string is a liner, the liner string is set at a depth such that the upper portion of the second liner string overlaps the lower portion of the first string of casing. The second liner string is then fixed, or “hung” off of the existing casing using a liner hanger to fix the new string of liner in the wellbore. The second liner string is then cemented. A tie-back casing string may then be landed in a polished bore receptacle (PBR) of the second liner string so that the bore diameter is constant through the liner to the surface. This process is typically repeated with additional liner strings until the well has been drilled to total depth. As more casing or liner strings are set in the wellbore, the casing or liner strings become progressively smaller in diameter in order to fit within the previous casing string. In this manner, wells are typically formed with two or more strings of casing and/or liner of an ever-decreasing diameter.
[0006] The process of hanging a liner off of a string of surface casing or other upper casing string involves the use of a liner hanger. The liner hanger is typically run into the wellbore above the liner string itself. The liner hanger is actuated once the liner is positioned at the appropriate depth within the wellbore. The liner hanger is typically set through actuation of slips which ride outwardly on cones in order to frictionally engage the surrounding string of casing. The liner hanger operates to suspend the liner from the casing string. However, it does not provide a fluid seal between the liner and the casing. Accordingly, a packer may be set to provide a fluid seal between the liner and the casing.
[0007] During the wellbore completion process, the packer is typically run into the wellbore above the liner hanger. A threaded connection typically connects the bottom of the packer to the top of the liner hanger. Known packers employ a mechanical or hydraulic force in order to expand a packing element outwardly from the body of the packer into the annular region defined between the packer and the surrounding casing string. In addition, a cone is driven behind a tapered slip to force the slip into the surrounding casing wall and to prevent packer movement. Numerous arrangements have been derived in order to accomplish these results.
[0008] The cementing process typically involves the use of liner wipers and drill-pipe plugs. A liner wiper is typically located inside the top of a liner, and is lowered into the wellbore with the liner at the bottom of a working string. The liner wiper plug typically defines an elongated elastomeric body used to separate fluids pumped into a wellbore. The wiper has radial wipers to contact and wipe the inside of the liner as the wiper travels down the liner. The liner wiper has a cylindrical bore through it to allow passage of fluids.
[0009] After a sufficient volume of cement has been placed into the wellbore, the plug is deployed. Using a displacement fluid, such as drilling mud, the plug is pumped into the working string. As the plug travels downhole, it seats against the liner wiper, closing off the internal bore through the liner wiper. Hydraulic pressure above the plug forces the plug and the wiper to dislodge from the bottom of the working string and to be pumped down the liner together. This forces the circulating fluid or cement that is ahead of the wiper plug and dart to travel down the liner and out into the liner annulus.
SUMMARY OF THE INVENTION
[0010] Embodiments of the present invention generally relate to tools and methods for hanging and/or expanding liner strings. In one embodiment, a method of hanging a liner assembly from a previously installed tubular in a wellbore includes: running the liner assembly and a setting tool into the wellbore using a run-in string. The setting tool includes an isolation valve and the liner assembly includes a liner hanger and a liner string. The method further includes sending an instruction signal from the surface to the isolation valve. The isolation valve closes in response to the instruction signal and isolates a setting pressure in the setting tool from the liner string. The method further includes increasing fluid pressure in the setting tool, thereby setting the liner hanger.
[0011] In another embodiment, a setting tool for hanging a liner assembly from a previously installed tubular in a wellbore, includes a tubular mandrel having a bore therethrough and a port formed through a wall thereof; a piston in fluid communication with the port and operable to set a liner hanger of the liner assembly; a latch operable to couple the liner assembly to the mandrel; a seal configured to isolate an annulus between the liner assembly and the setting tool; and an isolation valve. The isolation valve is operable to receive an instruction signal from the surface and close in response to receiving the instruction signal.
[0012] In another embodiment, a method of hanging a liner assembly from a previously installed tubular in a wellbore includes running the liner assembly and a setting tool into the wellbore using a run-in string. The setting tool includes a piston and an electric actuator and the liner assembly includes a liner hanger and a liner string. The method further includes sending an instruction signal from a surface to the electric actuator. The actuator supplies fluid pressure to the piston in response to the instruction signal, thereby setting the liner hanger.
[0013] In another embodiment, a setting tool for hanging a liner assembly from a previously installed tubular in a wellbore, includes: a tubular mandrel having a bore therethrough; a piston coupled to the mandrel and operable to set a liner hanger of the liner assembly; a latch operable to couple the liner assembly to the mandrel; a seal configured to isolate an annulus between the liner assembly and the setting tool and; an electric actuator. The actuator is operable to receive an instruction signal from a surface and supply fluid pressure to the piston.
[0014] In another embodiment, a method of expanding a liner in a wellbore, includes running the liner assembly and an expander assembly into the wellbore using a run-in string. The expander assembly includes an electric actuator and a two-position expander. The method further includes sending an instruction signal from a surface to the actuator; forming a launcher in the liner for the expander; shifting the two-position expander from a contracted position to an expanded position in the launcher by the actuator in response to the signal; and expanding the liner.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] So that the manner in which the above recited features of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to embodiments, some of which are illustrated in the appended drawings. It is to be noted, however, that the appended drawings illustrate only typical embodiments of this invention and are therefore not to be considered limiting of its scope, for the invention may admit to other equally effective embodiments.
[0016] FIGS. 1A and 1B are cross-sections of a setting tool, a liner assembly, and a wiper assembly, according to one embodiment of the present invention.
[0017] FIG. 2 is a cross-section of an isolation valve of the setting tool. FIG. 2A illustrates a coupling between a piston and retaining rod of the isolation valve. FIG. 2B illustrates a flapper of the isolation valve.
[0018] FIGS. 3A-D illustrate installation of the liner assembly.
[0019] FIG. 4 is a cross-section of an isolation valve, according to another embodiment of the present invention. FIGS. 4A-C illustrate operation of the isolation valve. FIG. 4D illustrates an alternative embodiment of the isolation valve.
[0020] FIG. 5 is a cross-section of an isolation valve, according to another embodiment of the present invention.
[0021] FIG. 6 is a cross-section of an isolation valve, according to another embodiment of the present invention. FIG. 6A illustrates an electronics package of the isolation valve. FIG. 6B illustrates surface equipment for generating pressure pulses for the electronics package. FIG. 6C illustrates the computer/PLC of the surface equipment.
[0022] FIG. 7 is a cross-section of a portion of a setting tool and a liner assembly, according to another embodiment of the present invention. FIG. 7A is an enlarged view of a piston actuator of the setting tool. FIGS. 7B and 7C illustrate an expander assembly of the setting tool according to an embodiment of the invention.
[0023] FIG. 8A illustrates a radio-frequency identification (RFID) electronics package, according to another embodiment of the present invention. FIG. 8B illustrates an active RFID tag. FIG. 8C illustrates a passive RFID tag.
[0024] FIG. 9A is a sectional view of an expandable liner system disposed in a wellbore proximate a lower end of a string of casing, according to another embodiment of the present invention. FIG. 9B is a sectional view illustrating the reforming or unfolding of a corrugated liner to form a launcher of the expandable liner system. FIG. 9C is a sectional view of the expansion system after positioning a two-position expander in the launcher. FIG. 9D is a sectional view of the expandable liner system illustrating the expansion of the corrugated liner section. FIG. 9E is a sectional view of the expandable liner system illustrating the expansion of the upper liner section. FIG. 9F is a sectional view of the completed wellbore.
[0025] FIG. 10 is a cross section of a valve of the expandable liner system.
[0026] FIG. 11 illustrates an alternative expansion assembly, according to another embodiment of the present invention.
[0027] FIG. 12 is a half section of a portion of a setting tool, according to another embodiment of the present invention.
[0028] FIGS. 13A-D are half-sections of an isolation valve and illustrate the operation of the isolation valve, according to another embodiment of the invention. FIGS. 13A-1 , 13 B- 1 , 13 C- 1 and 13 D- 1 illustrate a J-slot arrangement of the isolation valve and operation thereof. FIGS. 13A-2 and 13 B- 2 illustrate coupling between a ball and sleeve of the isolation valve and operation thereof.
[0029] FIGS. 14A-C are half-sections of an isolation valve and illustrate the operation of the isolation valve, according to another embodiment of the invention.
[0030] FIGS. 15A-D are half-sections of an expansion assembly of an expandable liner system and illustrate the operation of the system, according to another embodiment of the invention. FIG. 15A-1 illustrates a piston and valve of the expandable liner system. FIGS. 15C-1 , 15 D- 1 , 15 D- 2 are half-sections of a release mechanism of the expandable liner system and illustrate the operation of the system.
DETAILED DESCRIPTION
[0031] FIGS. 1A and 1B are cross-sections of a setting tool 1 , a liner assembly 100 , and a wiper assembly 150 , according to one embodiment of the present invention. The setting tool 1 , liner assembly 100 , and wiper assembly 150 may be run into a wellbore using a run-in string 685 (see FIG. 6 ). The run-in string 685 may include a string of tubulars, such as drill pipe, longitudinally and rotationally coupled by threaded connections. The liner assembly 100 may include an expandable liner hanger 105 , a polished bore receptacle (PBR) 110 , one or more adapters 115 , and a liner string 125 . The setting tool 1 may be operable to radially and plastically expand the liner hanger 105 into engagement with a casing or liner string 305 (see FIG. 3A ) previously installed in the wellbore. Non-sealing members of the setting tool 1 and liner assembly 100 may be made from a metal or alloy, such as steel or stainless steel. Alternatively, the PBR 110 may be disposed between the liner hanger and the run-in string.
[0032] The setting tool 1 may include a connector sub 2 , a mandrel 3 , one or more piston assemblies 10 a, b , an expander assembly 25 , a latch assembly 50 , an isolation valve 200 , and a seal assembly 75 . The connector sub 2 may be a tubular member including a threaded coupling for connecting to the run-in string and a longitudinal bore therethrough. The connector sub 2 may also include a second threaded coupling engaged with a threaded coupling of the mandrel 3 . One or more fasteners, such as set screws may secure the threaded connection between the connector sub 2 and the mandrel 3 . The mandrel 3 may be a tubular member having a longitudinal bore therethrough and may include one or more segments connected by threaded couplings.
[0033] The piston assemblies 10 a,b may include pistons 11 a,b , sleeves 12 - 14 , caps 15 a,b , inlets 16 a,b , outlets 17 a,b , and ratchet assembly 18 . The pistons 11 a, b may each be T-shaped annular members. An inner surface of each piston 11 a,b may engage an outer surface of the mandrel 3 and may include a recess having a seal, such as an o-ring disposed therein. The inlets 16 a,b may be formed radially through a wall of the mandrel 3 and provide fluid communication between a bore of the mandrel 3 and first sides of the pistons 11 a,b . The sleeves 12 , 13 may be longitudinally coupled to the pistons 11 a,b by threaded connections. Seals, such as o-rings, may be disposed between the pistons 11 a,b and the sleeves 12 , 13 . Each of the sleeves 12 - 14 may be a tubular member having a longitudinal bore formed therethrough and may be disposed around the mandrel, thereby forming an annulus therebetween. The caps 15 a,b may be annular members, disposed around the mandrel, and longitudinally coupled thereto by a threaded connection. The caps 15 a,b may also be disposed about a shoulder formed in or disposed on an outer surface of the mandrel 3 . Seals, such as o-rings, may be disposed between the caps 15 a,b and the mandrel 3 and between the caps 15 a,b and the sleeves 12 , 13 .
[0034] An end 12 a of the sleeve 12 may be exposed to an exterior of the setting tool 1 . The end 12 a of the sleeve 12 may further include a profile formed therein or fastened thereto by a threaded connection. The profile may mate with a corresponding profile formed on an outer surface of the ratchet assembly 18 , thereby longitudinally coupling the ratchet 18 and the sleeve 12 when the pistons are actuated. The sleeve profile may engage the ratchet profile by compressing a spring, such as a c-ring. The c-ring may then expand to lock in a groove of the sleeve profile. Teeth formed on inner and outer surfaces of a lock ring of the ratchet assembly 18 respectively engage corresponding teeth formed on an outer surface of the mandrel 3 and an inner surface of a ring housing, thereby longitudinally locking the sleeve 12 and thus the expander assembly 25 once the sleeve 12 engages the ratchet assembly 18 .
[0035] The outlet 17 a may be formed through an outer surface of the piston 11 a and may provide fluid communication between a second side of the piston 11 a and the exterior of the setting tool 1 . The sleeves 13 , 14 may be longitudinally coupled to the piston 11 b by a threaded connection. The outlet 17 b may be formed through a wall of the sleeve 14 and may provide fluid communication between a second side of the piston 11 b and the exterior of the setting tool 1 . An end 14 a of the sleeve 14 may be longitudinally coupled to an expander assembly 25 by a threaded connection and one or more set screws. The sleeve 14 may also be temporarily longitudinally coupled to the mandrel at 14 b by one or more frangible members, such as shear screws.
[0036] The expander assembly 25 may include a body 26 , upper cone retainer 27 , a plurality of cones 28 a,b , cone base 29 , lower cone retainer 30 , sleeve 31 , and shoe 32 , pusher 33 , and one or more frangible members, such as shear screws 34 . The expander assembly 25 may be operable to radially and plastically expand the hanger 105 into engagement with a previously installed liner or casing. The expander assembly 25 may be driven through the expandable hanger 105 by the pistons 11 a,b . The pusher 33 may longitudinally coupled to the sleeve 14 by a threaded connection and one or more fasteners, such as set screws. The pusher 33 may be longitudinally coupled to the body 26 by the shear screws 34 . The cones 28 a,b may each include a lip at each end thereof in engagement with respective lips formed at a bottom of the upper retainer 27 and a top of the lower retainer 30 , thereby radially coupling the cones to the retainers. An inner surface of each cone may be inclined for mating with an inclined outer surface of the cone base 29 , thereby holding each cone radially outward into engagement with the retainers.
[0037] The body 26 may be tubular, disposed along the mandrel 3 , and longitudinally movable relative to the mandrel. The upper retainer 27 may be longitudinally coupled to the body 26 by a threaded connection and one or more fasteners, such as set screws. The retainers, sleeve, and shoe may be disposed along the body. The upper retainer 27 may abut the cone base 29 and the cones 28 a,b . The cones may abut the lower retainer 30 . The lower retainer 30 may abut the sleeve 31 and the sleeve 31 may abut the shoe 32 . The shoe 32 may be longitudinally coupled to the body 26 by a threaded connection and one or more fasteners, such as set screws.
[0038] In operation (see FIG. 3C ), movement of the sleeve 14 longitudinally toward the upper retainer 27 may fracture the shear screws 34 since the body 26 may be retained by engagement of the cones 28 a,b with a top of the liner hanger 105 . Failure of the shear screws 34 may free the pusher 33 for relative longitudinal movement toward the upper retainer until a bottom of the pusher abuts a top of the upper retainer. Continued movement of the sleeve 14 may then push the cones 28 a,b through the liner hanger 105 , thereby expanding the liner hanger 105 into engagement with the previously installed casing/liner 305 . When removing the setting tool 1 ( FIG. 3D ), a top of the override 59 may engage a bottom of the body 26 , thereby carrying the expander assembly 25 with the mandrel 3 .
[0039] The expandable liner hanger 105 may include a tubular body made from a ductile material, such as a metal or alloy, such as steel or stainless steel. The hanger may include one or more seals 105 a disposed around an outer surface of the body. The seals 105 a may be made from a soft material, such as lead or a polymer, such as an elastomer. The hanger may have teeth 105 b embedded in the one or more of the seals 105 a for engaging an inner surface of the previously installed casing/liner and/or supporting the seals 105 a . Alternatively, a hard material 705 b (see FIG. 7 ) may be disposed along an outer surface of the hanger and/or the seals 105 a to penetrate an inner surface of the previously installed casing or liner, thereby securing the hanger 105 to the casing or liner. The hard material may be a ceramic, such as a carbide, such as tungsten carbide and disposed on the seals as dust and/or disposed on the hanger as teeth or blades.
[0040] The liner assembly 100 may be longitudinally and rotationally coupled to the mandrel 3 by the latch assembly 50 . The latch assembly 50 may include a piston 51 , a stop 52 , a release 53 , a collet 54 , a cap 55 , a retainer 56 , a biasing member, such as a spring 57 , one or more frangible members, such as shear screws 58 , an override 59 , a body 60 , one or more fasteners 61 a,b , and a catch 62 . Alternatively, the latch assembly 50 may include dogs (see dogs 77 ) instead of a collet.
[0041] The override 59 and the body 60 may each be tubular, have a bore therethrough, and include a threaded coupling at each end. The override 59 may be longitudinally and rotationally coupled to the mandrel 3 by one of the threaded couplings at a top thereof and one or more fasteners, such as set screws, and longitudinally and rotationally coupled to the body 60 by one of the threaded couplings and one or more fasteners, such as set screws 61 a . The body 60 may be longitudinally coupled to a seat 95 by one of the threaded couplings at a bottom thereof. Seals, such as o-rings, may be disposed between the override 59 and the mandrel 3 , between the override and the body 60 , and between the body and the seat 95 . The release 53 may be longitudinally and rotationally coupled to the override 59 by a threaded connection and one or more frangible members (not shown), such as shear screws. The threaded connection may be oppositely oriented (i.e. left-hand) relative to other threaded connections of the setting tool 1 . The release 53 may be longitudinally biased away from the override 59 by engagement of the spring 57 with fasteners 61 b.
[0042] The collet 54 may have a plurality of fingers each having a profile formed at a bottom thereof. The fingers 54 f may engage a corresponding profile formed in an inner surface of the adapter 115 . The collet 54 , case 56 , and cap 55 may be longitudinally movable relative to the body 60 between the stop 52 and a top of the piston 51 . When weight of the liner assembly 100 is applied to the collet 54 , the collet may move downward along the body 60 until the fingers seat against a profile 95 a formed in a top of the seat 95 , thereby longitudinally coupling the liner assembly 100 to the setting tool 1 . Keys 53 k and keyways may be formed in an outer surface of the release 53 . The keys 53 k and keyways may engage respective keyways and keys 115 k formed in a top of the adapter 115 , thereby rotationally coupling the liner assembly 100 and the setting tool 1 .
[0043] The piston 51 may be fluidly operable to release the fingers 54 f when actuated by a predetermined pressure. The piston 51 may be longitudinally coupled to the body 60 by the shear screws 58 . Once the liner hanger 105 has been expanded into engagement with the casing/liner 305 (see FIG. 3C ) and weight of the liner assembly is supported by the liner hanger 105 and/or setting the liner 125 onto a bottom of the wellbore 300 , fluid pressure may be increased. The fluid pressure may push the piston 51 and fracture the shear screws 58 , thereby releasing the piston 51 . The piston 51 may then move upward toward the collet 51 until the piston 51 abuts a bottom of the collet 54 . The piston 51 may continue upward movement while carrying the collet 54 (and fingers 54 f ), case 56 , and cap 55 upward until a bottom of the release abuts the fingers 54 f , thereby pushing the fingers 54 f radially inward. The catch 62 may be a split ring biased radially inward and disposed between the collet 54 and the case 56 . The body 60 may include a recess formed in an outer surface thereof. During upward movement of the piston 51 and members 54 - 56 , the catch 62 may align and enter the recess, thereby forming a downward stop preventing reengagement of the fingers 54 f . Movement of the piston and members 54 - 56 may continue until the cap 55 abuts the stop 52 , thereby ensuring complete disengagement of the fingers 54 f.
[0044] In the event that the liner assembly 100 becomes stuck in the wellbore 300 during run-in, the override 59 may be operated to release the fingers 54 f from the liner assembly 100 . The override 59 may be operated by setting down weight of the run-in string 685 onto the liner assembly 100 , thereby moving the collet 54 upward along the body 60 and the fingers 54 f from engagement with the profile 95 a . The run-in string may then be rotated, thereby rotating the override, fracturing the shear screws, and freeing the release from the override. The spring 57 may then move the release 53 toward the fingers 54 f until the release 53 disengages the fingers 54 f from the adapter.
[0045] The seal assembly 75 may include a lock 76 , a plurality of dogs 77 , dog retainer 78 , a cap 79 , fasteners, such as screws 80 , a catch 81 , a body 82 and one or more seal stacks 83 a,b . Each of the seal stacks 83 a,b may include first and second end adapters (not shown), one or more first seals (not shown), a center adapter (not shown), and one or more second seals (not shown). The first seals may be directional (i.e., chevron rings), and may be disposed between the first end adapter and the center adapter. The second seals may be directional and disposed between the center adapter and the second end adapter with an orientation opposing the first seals. The body 82 may be tubular, have a bore therethrough, and include a threaded coupling at each end. The body 82 may be longitudinally coupled to the housing 214 by one of the threaded couplings at a top thereof and longitudinally coupled to the catch 81 by one of the threaded couplings and one or more fasteners, such as set screws. A seal, such as an O-ring, may be disposed between the body 82 and the catch 81 . The dogs 77 may be radially movable between an extended position and a retracted position. The dogs 77 may be disposed in respective recesses formed in the dog retainer 78 and a lip of each dog may engage a respective lip of the retainer 78 in the extended position, thereby keeping the dogs 77 disposed in the recesses.
[0046] The dogs 77 may be held in the extended position by abutment of protrusions of a profile formed in an inner surface of the dog with respective protrusions of a profile formed in an outer surface of the lock 76 . The dogs 77 may engage a groove formed in an inner surface of the adapter 115 in the extended position, thereby longitudinally coupling the dogs and the adapter. Each screw 80 may be received by a threaded opening formed through the retainer 78 . An end of each screw 80 may extend into a respective slot formed through the lock 76 , thereby coupling the lock and the retainer while allowing limited longitudinal movement therebetween. The cap 79 may be longitudinally coupled to the block retainer 78 by a threaded connection. Inner seal stack 83 a may be disposed radially between the dog retainer and the body and longitudinally between a lower surface of the cap and a shoulder formed in the dog retainer. Outer seal stack 83 b may be disposed radially between the dog retainer and the adapter 115 and longitudinally between a bottom of the cap and a shoulder formed in the dog retainer. The seal stacks 83 a,b may fluidly isolate a bore of the liner 125 from an annulus formed between the setting tool 1 and the rest of the liner assembly 100 .
[0047] To release the lock 76 (see FIG. 3D ), the body 82 may be moved upward carrying the catch 81 toward the lock 76 until a top of the catch 81 abuts a bottom of the lock and pushes the lock 76 upward toward the dog retainer 78 until recesses in the lock profile align with protrusions in the dog profile. A lower portion of the body 82 may include one or more grooves formed in an outer surface thereof for pressure equalization as the catch moves toward the lock. Alignment of the profiles allows the dogs to move from the extended position to the retracted position, thereby freeing the dogs from the adapter 115 .
[0048] The setting tool 1 may further include the seat 95 . The seat 95 may have a tapered inner surface 95 s for receiving a ball or plug (not shown) and one or more ports 95 p formed radially therethrough. The ports 95 p may be isolated from the setting tool-adapter annulus by seals, such as O-rings, disposed between the seat and the adapter 115 and longitudinally straddling the ports 95 p . The ball or plug may be deployed as a safeguard or in response to failure of the isolation valve 200 . The ball may be released from the surface a predetermined distance behind the top plug (se FIG. 3A ) so that the ball may be substantially pumped to the seat 95 by the displacement fluid (the ball may have to free fall a small depth once the top plug has seated against the wiper). Alternatively, should the isolation valve 200 fail, a plug may be delivered to the seat via wireline (not shown) or the ball may be deployed after the top plug has seated by free-falling to the seat 95 . As with the isolation valve 200 , landing of the ball or plug may fluidly isolate the mandrel bore from the liner bore. When the setting tool is being removed from the liner assembly 100 and the seat is removed from the liner assembly, the port seals may no longer engage a sealing surface due to the larger inside diameter of the previously installed casing or liner, thereby opening the ports 95 p . The ports 95 p may then provide fluid communication between the setting tool bore and the wellbore, allowing drainage of the displacement fluid from the setting tool 1 and the run-in string 685 as the setting tool 1 travels to the surface. A bottom of the seat 95 may be longitudinally coupled to the housing 201 by a threaded connection.
[0049] The wiper assembly 150 may include a body 151 , a wiper 152 , and one or more frangible members, such as shear screws 153 . The body 151 may be longitudinally coupled to the catch 81 by the shear screws 153 . The body 151 may be tubular and have a profile 151 p formed along an inner surface thereof for receiving a top plug 320 (see FIG. 3A ). The top plug 320 may include a latch for engaging the profile 151 p . Additionally, the wiper assembly 150 may be a top wiper assembly and the setting tool may further include a bottom wiper assembly (not shown). The bottom wiper assembly may be longitudinally coupled to the body 151 by shear screws and have an inner diameter less than an inner diameter of the top wiper assembly 150 . In this manner a bottom plug (not shown) may be deployed before the cement is pumped for isolating the cement from circulation fluid and may be pumped through the body 151 and seat in the bottom wiper assembly. The bottom plug may include a diaphragm or valve.
[0050] FIG. 2 is a cross-section of the isolation valve 200 . The isolation valve may be longitudinally coupled to the mandrel 3 by a threaded connection. The isolation valve may include one or more housings 201 , 208 , 211 , 214 , one or more seals, such as o-rings 202 , 204 , 207 , 212 , one or more frangible members, such as shear screws 203 and rupture disk 216 , a piston 205 , a retaining rod 206 , one or more nuts 209 , one or more locator rings 210 , a valve member such as a flapper 213 , and one or more biasing members, such as springs 215 , 218 , and one or pins 217 , 219 . Alternatively, the valve member may be a ball (not shown).
[0051] The piston 205 may be longitudinally coupled to the flapper 213 via the retaining rod 206 . The piston 205 may be longitudinally coupled to the retaining rod 206 via the pins 217 . The piston 205 may be biased away from the flapper 213 by spring 215 and longitudinally and rotationally coupled to the housing 208 by shear screws 213 . The retaining rod 206 may hold the flapper 213 in the open position. The flapper 213 may be biased towards the closed position by the spring 218 disposed on a mount, such as the pin 219 . A chamber housing the piston 205 and the spring 215 may be sealed at the surface with air at atmospheric pressure. In operation, when it is desired to close the flapper 213 , pressure may be increased in bores of the housings 201 , 208 , 211 , 214 until a predetermined pressure is reached. The rupture disk 216 may then fracture, thereby providing fluid communication between the housing bores and a bottom of the piston 205 . The resulting fluid force may fracture the shear screws 203 and (along with the spring 215 ) move the piston 205 away from the flapper 213 , thereby allowing the flapper 213 to close.
[0052] FIGS. 3A-D illustrate installation of the liner assembly 100 . In operation, the setting tool 1 , liner assembly 100 , and wiper assembly 150 may be run into the wellbore 300 until the liner hanger 105 overlaps an end of the previously installed casing or liner 305 distal from the surface. A bottom of the liner 125 may or may not rest on a bottom of the wellbore. Prior to run-in, fluid, such as drilling mud, may be circulated to ensure that all of the cuttings have been removed from the wellbore. A surge reduction valve (not shown), if used, may be closed. Circulation may then be established by pumping fluid, such as drilling mud, down the run-in string and up the liner annulus. The liner assembly 100 may be reciprocated and/or rotated during circulation. If auto-fill equipment (not shown) is used, it may be released. If a bottom wiper assembly (not shown) is used, then the bottom plug may be launched.
[0053] Cement slurry 315 may then be pumped from the surface into the run-in string. The liner assembly 100 may be reciprocated and/or rotated during injection of the cement. A spacer fluid (not shown) may be pumped in ahead of the cement 315 . Once a predetermined quantity of cement 315 has been pumped, a top plug 320 may be pumped down the run-in string using a displacement fluid 310 , such as drilling mud. The bottom plug may seat in the bottom wiper assembly, free the bottom wiper assembly from the setting tool, and land in the float collar/shoe. The diaphragm may then rupture or the valve may open due to a density differential between the cement and the circulation fluid and/or increased pressure from the surface.
[0054] Pumping of the displacement fluid 310 may continue and the top plug 320 may seat in the wiper body 151 , thereby closing the bore through the wiper body 151 ( FIG. 3A ). The displacement fluid 310 may have a density substantially less than the density of the cement, thereby placing the liner 125 in compression. A latch of the plug 320 may engage the profile 151 p and hydraulic pressure may fracture the shear screws 153 , thereby freeing the wiper assembly 150 and the plug 320 . The wiper/plug 150 , 320 may then be pumped down the liner 125 , thereby forcing the cement 315 through the liner and out into the liner annulus. Pumping may continue until the wiper/plug 150 , 320 seat against a landing or float collar (not shown), thereby indicating that the cement 315 is in place in the liner annulus.
[0055] The pressure may then be increased until the rupture disk 216 in the isolation valve 200 fractures, thereby moving the piston 205 and allowing the flapper 213 to close ( FIG. 3B ). The flapper 213 may isolate the mandrel bore from the liner bore. Pressure may then be increased to fracture the shear screws 14 b and operate the pistons 11 a,b , thereby pushing the expander assembly 25 through the expandable liner hanger 105 ( FIG. 3C ). Once the hanger 105 is expanded into engagement with the previously installed casing or liner 305 , the latch assembly 50 may be released from the liner assembly 105 and the setting tool 1 removed ( FIG. 3D ). Before retrieval to the surface, the setting tool 1 may be raised and fluid, such as drilling mud, may be reverse circulated (not shown) to remove excess cement above the hanger before the cement sets.
[0056] FIG. 4 is a cross-section of an isolation valve 400 , according to another embodiment of the present invention. The isolation valve 400 may be used instead of the isolation valve 200 . The isolation valve 400 may include one or more housings 401 , 409 , 412 , 416 , 419 , 422 , one or more seals, such as o-rings 402 , 403 , 405 , 408 , 420 , one or more plugs 404 , one or more frangible members, such as shear screws 413 , one or more pistons 406 , 410 , an actuator 414 , a retaining rod 415 , a choke 407 , one or more nuts 417 , one or more locator rings 418 , a valve member, such as a flapper 421 , and one or more biasing members, such as springs 411 , 424 , and 218 (see FIG. 2B ), one or more check valves 423 , and one or pins 217 , 219 (see FIGS. 2A and 2B ).
[0057] A top of the piston 405 may be in fluid communication with a bore of the housings 401 , 416 via fluid path 430 defined between the housings 401 , 416 . A chamber housing spring 411 may be in fluid communication with the liner annulus via vent 432 . A hydraulic fluid, such as oil, may be disposed between a shoulder 406 s of the piston 406 and a top of the piston 410 . The housing 409 may include fluid ports 409 a,b longitudinally formed therethrough. The fluid ports 409 a,b may provide limited fluid communication between an upper hydraulic chamber formed between the shoulder 406 s and a top of the housing 409 and a lower hydraulic chamber formed between a bottom of the housing 409 and the top of the piston 410 .
[0058] The check valve 423 may be disposed in the path 409 b and operable to prevent flow of the hydraulic fluid from the upper hydraulic chamber to the lower hydraulic chamber and allow flow from the lower hydraulic chamber to the upper hydraulic chamber. The choke 407 may be disposed in the path 409 a and operable to restrict hydraulic flow from the upper hydraulic chamber to the lower hydraulic chamber. The choke 407 may also restrict flow from the lower hydraulic chamber to the upper hydraulic chamber but this restriction may be negated by the open check valve 423 . The piston 410 may be longitudinally coupled to the piston 406 by incompressibility of the hydraulic fluid. A bottom of the piston 410 may be in fluid communication with the liner annulus via the vent 432 . The piston 410 may be biased toward the housing 409 by the spring 411 .
[0059] The actuator 414 may be longitudinally coupled to the flapper 421 via the retaining rod 415 . The actuator 414 may be longitudinally coupled to the retaining rod 415 via the pins 217 . The retaining rod 415 may hold the flapper 421 in the open position. The flapper 421 may be biased towards the closed position by the spring 218 disposed on a mount, such as the pin 219 . The actuator 414 may be longitudinally coupled to the housing 416 by the shear screws 413 .
[0060] FIGS. 4A-C illustrate operation of the isolation valve 400 . Once pressure in the bore of the housings 401 , 416 exceeds pressure in the liner annulus by an amount sufficient to overcome the bias of the spring 411 (threshold pressure), the piston 406 begins to move longitudinally downward toward the housing 409 ( FIG. 4A ). Since movement of the piston is dampened by the choke 407 , the increased pressure must be sustained for a predetermined period of time, else once the pressure is reduced, the biasing member will return the piston 406 to the position of FIG. 4A . Once sustained threshold pressure has been applied to the top of the piston 406 , a bottom of the piston 406 abuts a top of the actuator 414 and fractures the shear screws 413 ( FIG. 4B ). Pressure may be then reduced to the annulus pressure or relieved at the surface, thereby allowing the spring 411 to return the piston 406 to the position of FIG. 4A . The spring 424 may then longitudinally move the actuator 414 and retaining rod 420 longitudinally upward away from the flapper 421 , thereby releasing the flapper and allowing the spring 218 to close the flapper ( FIG. 4C ).
[0061] The choke 407 may time the movement of the piston 406 so that threshold pressure must be sustained for the piston to reach the actuator 414 . For example, when running the liner assembly 100 into the wellbore, a surge pressure may exceed the threshold pressure but may not be sustained to fully move the piston 406 . However, once the top plug 320 seats against the wiper 315 , then the threshold pressure may be applied for the sustained period. If pressure is relieved from the run-in string at the surface, the flapper 421 may allow annulus pressure to also be relieved. However, once pressure is reapplied to set the liner hanger 105 , the flapper 421 will close and isolate the liner 125 from setting pressure applied to the setting tool 1 .
[0062] FIG. 4D illustrates an alternative embodiment of the isolation valve 400 . In this alternative, the piston 406 is initially longitudinally restrained by one or more frangible members, such as shear pins 455 . The shear pins 455 may keep the piston 406 from moving until a predetermined pressure has been reached. The shear pins 455 may avoid unintentional operation of the piston 406 during circulation and cementing operations.
[0063] FIG. 5 is a cross-section of an isolation valve 500 , according to another embodiment of the present invention. The isolation valve 500 may be used instead of the isolation valve 200 . The isolation valve may include one or more housings 501 , 510 , 512 , 513 , 518 , 521 , 524 one or more seals, such as o-rings 503 , 504 , 506 , 509 , 522 one or more plugs 505 , one or more frangible members, such as shear screws 514 , one or more pistons 507 , 511 , an actuator 515 , 516 , a retaining rod 517 , a choke 508 , one or more nuts 519 , one or more locator rings 520 , a valve member such as a flapper 523 , and one or more biasing members, such as springs 502 , 526 , and 218 (see FIG. 2B ), one or more check valves 525 , and one or pins 217 , 219 of (see FIGS. 2A and 2B ). In operation, the spring 502 is used to slowly engage a release mechanism so the running of the liner and cementing of the liner can be completed before the valve closes.
[0064] The actuator may include a head 516 and a ring 515 . The head 516 and the ring 515 may be longitudinally and rotationally coupled to the housing 518 by the shear screws 514 . The head 516 may be longitudinally coupled to the flapper 523 via the retaining rod 517 . The head 516 may be biased away from the flapper 523 by the spring 526 . The head 516 may be longitudinally coupled to the retaining rod 517 via the pins 217 . The retaining rod 517 may hold the flapper 523 in the open position. The flapper 523 may be biased towards the closed position by the spring 218 disposed on a mount, such as the pin 219 .
[0065] A top of the piston 507 may be in fluid communication with a bore of the housings 501 , 518 via fluid path 530 defined between the housings 501 , 518 . A hydraulic fluid, such as oil, may be disposed between a shoulder 507 s of the piston 507 and a top of the piston 511 . The housing 510 may include fluid ports 510 a,b longitudinally formed therethrough. The fluid ports 510 a,b may provide limited fluid communication between an upper hydraulic chamber formed between the shoulder 507 s and a top of the housing 510 and a lower hydraulic chamber formed between a bottom of the housing 510 and the top of the piston 511 .
[0066] The check valve 525 may be disposed in the path 510 b and operable to prevent flow of the hydraulic fluid from the upper hydraulic chamber to the lower hydraulic chamber and allow flow from the lower hydraulic chamber to the upper hydraulic chamber. The choke 508 may be disposed in the path 510 a and operable to restrict hydraulic flow from the upper hydraulic chamber to the lower hydraulic chamber. The choke 510 a may also restrict flow from the lower hydraulic chamber to the upper hydraulic chamber but this restriction may be negated by the open check valve 525 . The piston 511 may be longitudinally coupled to the piston 507 by incompressibility of the hydraulic fluid. The piston 507 may be biased longitudinally downward toward the housing 510 by the spring 502 . A chamber 535 between the housing 518 and the head 516 , a chamber 537 between the housings 513 , 518 , and a chamber 539 between the housing 512 and the piston 507 may be sealed at the surface with air at atmospheric pressure.
[0067] In operation, once the isolation valve 500 is assembled, the spring 502 may begin to move the piston 507 longitudinally downward toward the flapper 523 . Since movement of the piston 507 is dampened by the choke 508 , the piston 507 may require a predetermined period of time before a bottom of the piston 507 abuts a top of the ring 515 and fractures the shear screws 514 . The predetermined period may be selected so the liner assembly 100 may be run into the wellbore and cemented before the flapper 523 closes.
[0068] Alternatively, the spring 502 may be omitted and fluid pressure exerted on a top of the piston via flow path 530 may be used to operate the piston 507 .
[0069] FIG. 6 is a cross-section of an isolation valve 600 , according to another embodiment of the present invention. The isolation valve 600 may be used instead of the isolation valve 200 . The isolation valve 600 may include one or more housings 601 , 607 , 610 , 612 , 617 , 620 , 623 , 630 , a pick 602 , one or more seals, such as o-rings 604 , 605 , 608 , 611 , 621 , one or more plugs 606 , one or more frangible members, such as shear screws 613 and rupture disk 603 , one or more pistons 609 , an actuator 614 , 615 , a retaining rod 616 , one or more nuts 618 , one or more locator rings 619 , a valve member such as a flapper 622 , one or more biasing members, such as springs 624 , 218 (see FIG. 2B ), one or pins 217 , 219 (see FIGS. 2A and 2B ), and an electronics package 650 .
[0070] The actuator may include a head 615 and a ring 614 . The head 615 and the ring 614 may be longitudinally and rotationally coupled to the housing 617 by the shear screws 613 . The head 615 may be longitudinally coupled to the flapper 622 via the retaining rod 616 . The head 615 may be biased away from the flapper 622 by the spring 624 . The head 615 may be longitudinally coupled to the retaining rod 616 via the pins 217 . The retaining rod 616 may hold the flapper 622 in the open position. The flapper 622 may be biased towards the closed position by the spring 218 disposed on a mount, such as the pin 219 .
[0071] An upper chamber between housings 601 and 630 , an intermediate chamber between a bottom of the housing 606 and a top of the piston 609 , and a lower chamber between a shoulder 609 s of the piston 609 and a top of the housing 612 may be sealed at the surface with air at atmospheric pressure. The housing 606 may have a first fluid port 606 a extending radially and longitudinally between a bore therethrough to the upper chamber. The rupture disk 603 may seal the first fluid port 606 a . The housing 606 may further have a second fluid port 606 b longitudinally extending therethrough between the upper and intermediate chambers. The housing 617 may have a vent 632 formed radially therethrough providing fluid communication between a bore formed therethrough and a chamber 635 between the housing 617 and the head 615 . The chamber 635 may be in fluid communication with a chamber 637 between the housings 612 , 617 via flow path 634 formed between ring 614 and housing 617 .
[0072] FIG. 6A illustrates the electronics package 650 . The electronics package 650 may include a pressure sensor 652 , a signal amplifier 654 , a noise filter 656 , a signal detector 658 , a microprocessor 660 , a battery pack 662 , and a solenoid 664 . Pressure pulses transmitted from the surface to the isolation valve 600 via the run-in string may be transformed by the pressure sensor 652 into an electrical signal. The electrical signal may then be amplified by the signal amplifier 654 and filtered by the noise filter 656 . The filtered signal may then be demodulated by the signal detector 658 into a format usable by the microprocessor 660 . The demodulated signal may be analyzed by the microprocessor 660 to determine if the signal matches a predetermined instruction signal for closing the flapper 622 . If so, then the microprocessor may energize the solenoid, thereby longitudinally moving the pick 602 to fracture the rupture disk 603 . The pick 602 may then be retracted from the fractured rupture disk 603 by a spring (not shown) or reversing polarity to the solenoid.
[0073] Once the rupture disk 603 has been fractured, circulation fluid from the bore of the isolation valve 600 may flow through the port 607 a into the upper chamber. Fluid may then flow from the upper chamber through the port 607 b into the intermediate chamber, thereby moving the piston 609 longitudinally downward toward the flapper 622 . Since lower chamber was sealed at the surface, minimal pressure may be exerted on the shoulder 609 s . The piston 609 may move until a bottom of the piston 609 abuts the ring 614 and fractures the shear screws 613 , thereby releasing the head 615 . The spring 624 may then move the head 615 (and the rod 616 ) longitudinally upward away from the flapper 622 , thereby releasing the flapper. The spring 218 may then close the flapper 622 , thereby fluidly isolating the liner 125 from the setting tool 1 . The setting tool 1 may then be operated and the liner hanger 105 expanded.
[0074] FIG. 6B illustrates surface equipment for generating pressure pulses. The pressure pulses may be generated at the surface using the displacement fluid 310 . The displacement fluid 310 may be stored in a surge tank 677 . The surge tank 677 may include a fluid barrier, such as a diaphragm 678 , separating a chamber of the tank 677 into a displacement fluid chamber and a gas chamber. A fluid line 684 may be in communication with a mud pump of the rig to fill the displacement fluid chamber. A gas line 682 may be in fluid communication with a gas source, such as a portable cylinder, and include a pressure regulator for filling and maintaining the gas chamber at a predetermined pressure. The gas 679 may be nitrogen. The pressure pulses may be applied and released from a bore of the run-in string 685 after the top plug 320 and the wiper 325 have landed in the float or landing collar. The pressure pulses may be generated by opening an inlet control valve, such as a solenoid operated ball valve 680 i , thereby providing fluid communication between the displacement fluid chamber of the surge tank 677 and the run-in string 685 . The valve 680 i may be electrically, pneumatically, or hydraulically operated. After a predetermined period of time, the valve 680 i may be closed while opening an outlet control valve 680 o , thereby relieving fluid pressure from the run-in string to a mud pit or tank (not shown) of the rig. Control of the valves 680 i,o may be performed by a computer or programmable logic controller (PLC) 690 located at the surface to generate the predetermined instruction signal to close the isolation valve 600 .
[0075] FIG. 6C illustrates the computer/PLC 690 . The computer/PLC may be disposed in an operator interface (not shown), such as a console. The interface may include indicator lights R, G to provide visual feedback to the operator. A first light, such as a green light G, may indicate that the computer/PLC is ready to transmit the instruction signal. The console may further include a pushbutton operable to signal the computer to begin transmission of the instruction signal. A second light, such as a red light R, may indicate that the computer is transmitting the instruction signal. The computer/PLC 690 may be in electrical communication with solenoids of the valves 680 i,o.
[0076] Alternatively, instead of mud pulse, the electronics package 650 may include an electromagnetic (EM) receiver or transceiver (not shown) or any other wireless telemetry system. An EM telemetry system is discussed in U.S. Pat. No. 6,736,210, which is hereby incorporated by reference in its entirety.
[0077] FIG. 7 is a cross-section of a portion of a setting tool 700 and a liner assembly, according to another embodiment of the present invention. The remaining portion of the setting tool 700 and liner assembly may be similar to the setting tool 1 and liner assembly 100 except that the PBR 710 may be moved to between the expandable liner hanger and the run-in string and the isolation valve 200 may be omitted.
[0078] The setting tool 700 may include a mandrel 703 , a piston 711 , a damping chamber 714 , a choke 716 , an atmospheric chamber 718 , a piston actuator, and an expander assembly 725 . The mandrel 703 may be a tubular member including a threaded coupling for connecting to the run-in string 685 and a longitudinal bore therethrough. Although shown as one piece, the mandrel 703 may include a plurality of pieces connected by threaded connections and seals to facilitate manufacture and assembly thereof. The piston 711 may be a tubular member having a longitudinal bore therethrough. Although shown as one piece, the piston 711 may include a plurality of pieces connected by threaded connections to facilitate manufacture and assembly thereof. The piston 711 may be disposed between inner and outer walls of the mandrel 703 . The piston 711 may include a head formed at a top thereof. One or more seals, such as O-rings, may be disposed between an inner surface of the head and the inner wall and between an outer surface of the head and the outer wall.
[0079] The chambers 714 , 718 may be formed between the piston 711 and the outer wall of the mandrel 703 . The mandrel may include a partition dividing the chambers 714 , 718 . A seal, such as an O-ring may be disposed between the piston 711 and the partition. One or more chokes 716 may be disposed in the partition. The chokes 716 may provide limited fluid communication between the chambers 714 , 718 , thereby damping longitudinal movement of the piston. The chambers 714 , 718 may be sealed at the surface under atmospheric pressure. The damping chamber 714 may be filled with a hydraulic fluid, such as oil. The atmospheric chamber 718 may be filled with a gas, such as air.
[0080] The expander assembly 725 may include an actuator 726 , one or more frangible members, such as shear screws 727 , a pusher 728 , a mandrel 729 , a collet 730 , a biasing member, such as a spring 731 , one or more retainers 732 , and a spacer 733 . The expander mandrel 729 may be tubular and disposed along an outer surface of the setting mandrel 703 so that the expander mandrel is longitudinally movable relative to the setting mandrel 703 . The expander mandrel may include a shoulder formed at a bottom thereof. The collet 730 may be disposed along an outer surface of the expander mandrel and include a base ring formed at a bottom thereof.
[0081] The spring may be disposed between the base ring and the expander mandrel shoulder, thereby biasing the collet 730 longitudinally away from the expander mandrel shoulder. The collet 730 may include a plurality of radially split cones 730 c each extending longitudinally from the base ring. The cones 730 c may be radially split so that the cones may be radially movable between an expanded position (shown) and a retracted position. An inner surface of the cones 730 c may be held in the expanded position by abutment with the spacer 733 . An outer surface of the cones may abut the liner hanger 705 . A top of the cones 730 c may abut a bottom of the pusher 728 . The spacer 733 may be longitudinally coupled to the actuator 726 by one or more fasteners, such as screws. The pusher 728 may be longitudinally coupled to the actuator 726 by the shear screws 727 .
[0082] The actuator 726 may be tubular and have a head formed at a top thereof. The actuator may further have one or more windows formed through a wall thereof. One of the retainers 732 may be disposed through each window. Each retainer may be received by a groove formed in an outer surface of the expander mandrel and fastened to the expander mandrel. Each retainer may also be disposed through a respective opening formed through a wall of the pusher. The retainers may be blocks and longitudinally couple the pusher to the mandrel. The windows may be sized to allow relative longitudinal movement of the actuator relative to the blocks should the shear screws fail. The collet 730 may have a recessed inner surface formed between the base ring and the cones 730 c for receiving a lower portion of the actuator and the spacer 733 should the shear screws fail. The bottom shoulder of the piston may also include a recessed inner surface for receiving an upper portion of the expander mandrel should the shear screws fail. The actuator head may abut the bottom shoulder of the piston 711 .
[0083] In operation, longitudinal movement of the piston 711 may push the expander assembly 725 downward along the hanger 705 , thereby expanding the hanger into engagement with the previously set liner/casing. If the annulus between the hanger 705 and the liner/casing is sufficient, the hanger 705 may expand as forced by the expanded cones 730 c . However, if the annulus is insufficient, the reaction force may increase to fracture the shear screws 727 . As shown in FIG. 7B , the actuator 726 and the spacer 733 may then be free to move longitudinally relative to the rest of the expander assembly, thereby moving the spacer 733 from the inner surface of the cones and replacing the spacer 733 with the outer surface of the actuator 726 which may have a reduced outer diameter. The reduced outer diameter may allow the cones to move radially inward to the retracted position. Movement of the actuator 726 may continue until a lower surface of the actuator head abuts a top of the pusher 728 , thereby resuming movement of the expander assembly 725 downward through the hanger 705 . The reduced outer diameter of the cones 730 c may reduce the expanded outer diameter of the hanger 705 which may suitable for the smaller annulus.
[0084] As illustrated in FIG. 7C , after expansion of the liner hanger 705 into engagement with an existing casing 735 or at some other point during operation of the setting tool 700 , when the expander assembly 725 is removed from the liner assembly the cones 730 c are operable to collapse into an even further reduced outer diameter configuration. The spacer 733 may be releasably coupled to the actuator 726 by one or more frangible members, such as shear screws 734 . The cones 730 c , which are seated on the outer surface of the actuator 726 , may be forced against the end of the spacer 733 to shear the shear screws 734 and allow the cones 730 c to move relative to the actuator 726 . The cones 730 c may then be moved off of the actuator 726 outer surface until the cones 730 and the spacer 733 are seated on the outer surface of the mandrel 729 , thereby further reducing the outer diameter of the cones 730 c . In one embodiment, during retrieval of the expansion assembly 725 , a restriction, such as an inner diameter shoulder of a component of the liner assembly or a narrowed inner diameter portion of the existing casing 735 may engage the cones 730 c and obstruct passage theretherough. An upward or pull force applied to the run-in string and/or the mandrel 703 may cause a reaction force to be applied to the cones 730 c against the restriction. The reaction force may be transferred through the cones 730 c and applied to the spacer 733 until the shear screws 734 release engagement with the actuator 726 . The reaction force may then move the cones 730 c and the spacer 733 relative to the actuator 726 onto the outer surface of the mandrel 729 , thereby reducing the outer diameter of the cones 730 c and allowing the expander assembly 725 to be moved past the restriction.
[0085] FIG. 7A is an enlarged view of the piston actuator. The piston actuator may include the electronics package 650 , one or more heating coils 706 , one or more ports 708 , one or more retainers, such as fusible rods 715 , and a plug 712 . The ports may provide fluid communication between the wellbore and a first chamber formed in the mandrel 703 . The plug may be disposed in a passage between the first chamber and a second chamber in communication with a top of the piston head. The second chamber may be sealed at the surface under atmospheric pressure and be filled with a gas, such as air. One or more seals, such as O-rings, may be disposed between each plug and the passage. Each plug may be longitudinally restrained in the passage by a respective rod.
[0086] In operation, when the electronics package detects an instruction signal from the surface, the microprocessor may supply electricity to the heating coil, thereby heating the rod. The increased temperature of the rod may weaken the rod until hydrostatic pressure exerted on a top of the plug fractures the rod, thereby freeing the plug. The plug may be pushed into the second chamber by wellbore fluid, thereby opening the passage. Wellbore fluid may enter the second chamber through the open passage and exert hydrostatic pressure on the top of the piston head, thereby longitudinally moving the piston downward toward the expander assembly. The piston head may push the oil through the choke 716 and into the atmospheric chamber 718 , thereby controlling a rate of movement of the piston. As discussed above, movement of the piston may operate the expander assembly 725 , thereby setting the hanger 705 . Cementing may occur as discussed above in relation to FIGS. 3A-3D .
[0087] Since the mud pulse signal can be varied, several difference devices can be operated down hole each with a unique signal, e.g. a surge reduction valve (see U.S. Pat. No. 6,834,726, which is hereby incorporated by reference in its entirety) that allows for faster run in of the liner before cementing can be closed prior to cementing; setting the liner hanger with a vacuum operated jack system—note several vacuum chambers can be operated in series if the hydrostatic pressure is too low for a single vacuum chamber jack to set the liner hanger; releasing the running tool from the liner hanger after the liner hanger is set; etc.
[0088] FIG. 8A illustrates a radio-frequency identification (RFID) electronics package 800 , according to another embodiment of the present invention. FIG. 8B illustrates an active RFID tag 850 a . FIG. 8C illustrates a passive RFID tag 850 p . The RFID electronics package 800 may be used instead of the electronics package 650 in the isolation valve 600 and/or the electronics package 750 in the setting tool 700 . The electronics package 800 may communicate with a passive RFID tag 850 p or an active RFID tag 850 a . Either of the RFID tags 850 a,p may be embedded in the top plug 320 so that the electronics package 800 may detect passage of the top plug 320 thereby. Alternatively, either of the RFID tags may be embedded in a ball, plug, bar or some other device used to initiate the release of a downhole valve.
[0089] The RFID electronics package 800 may include a receiver 802 , an amplifier 804 , a filter and detector 806 , a transceiver 808 , a microprocessor 810 , a pressure sensor 812 , battery pack 814 , a transmitter 816 , an RF switch 818 , a pressure switch 820 , and an RF field generator 822 . If the active RFID tag 850 a is used, the components 816 - 822 may be omitted.
[0090] If a passive tag 850 p is used, once the isolation valve 600 or setting tool 700 is deployed to a sufficient depth in the wellbore, the pressure switch 820 may close. The pressure switch may remain open at the surface to prevent the electronics package 800 from becoming an ignition source. The microprocessor may also detect deployment in the wellbore using pressure sensor 812 . The microprocessor 810 may delay activation of the transmitter for a predetermined period of time to conserve the battery pack 814 . The microprocessor may then begin transmitting a signal and listening for a response. Once the top plug is pumped into proximity of the transmitter 816 , the passive tag 850 p may receive the signal, convert the signal to electricity, and transmit a response signal. The electronics package 800 may receive the response signal, amplify, filter, demodulate, and analyze the signal. If the signal matches a predetermined instruction signal, then the microprocessor 810 may monitor pressure for a predetermined threshold indicative that the top plug 320 has seated against the wiper and/or wait a predetermined period for the top plug to seat. Once the predetermined threshold is detected and/or the time period has passed, the microprocessor may close the isolation valve or operate the setting tool.
[0091] If the active tag 850 a is used, then the tag 850 a may include its own battery, pressure switch, and timer so that the tag 850 a may perform the function of the components 816 - 822 .
[0092] Since the tags send out unique signals, multiple receivers may be used. For example one receiver may be used to close a surge reduction valve; another receiver may start a sequence leading to the operation of the setting tool 700 to set the liner hanger and release the running tool.
[0093] FIG. 9A is a sectional view of an expandable liner system 900 disposed in a wellbore 910 proximate a lower end of a string of casing 920 , according to another embodiment of the present invention. The system 900 may include a liner assembly 925 and an expander assembly 950 . The expandable liner system 900 may be run-into the wellbore 910 using the run-in string 685 . The wellbore section below the casing 920 may be drilled without an underreamer. The liner assembly 925 may be set in the casing 920 by positioning an upper portion of the liner assembly 925 in an overlapping relationship with a lower portion of the casing 920 . Thereafter, the expansion assembly 950 may be employed to expand the liner assembly 925 into engagement with the casing 920 and the surrounding wellbore 910 .
[0094] The liner assembly 925 may include a tubular section 930 at an upper end thereof and a shaped or a corrugated liner section 935 disposed at the lower end thereof. It must be noted that the shape or corrugation of the liner section 935 is optional such that the liner section 935 is substantially cylindrical. Alternatively, the corrugated liner section 935 may be located at any position along the liner assembly 925 . A cross section of a suitable corrugated liner section may be found at FIG. 2G of U.S. Pat. No. 7,121,351, which is herein incorporated by reference in its entirety. The corrugated liner section 935 and the substantially cylindrical liner section 930 may be connected by a threaded connection or may be one continuous tubular body. The corrugated liner section 935 may be fabricated from a drillable material, such as aluminum or a pliable composite. The corrugated liner section 935 may have a folded wall having an initial inner diameter which may be reformed to define a larger second folded inner diameter and subsequently may be expanded to an even larger unfolded diameter. The corrugated liner section 935 may be folded or deformed prior to insertion into the wellbore 910 , to a non-tubular-shape, such as a hypocycloid, so that grooves are formed along the length of the corrugated liner section 935 . The grooves may be symmetric or asymmetric.
[0095] The liner assembly 925 may further include a shoe 940 at the lower end thereof. The shoe 940 may be longitudinally coupled to the corrugated portion, such as by a threaded connection. The shoe 940 may be a tapered or bullet-shaped and may guide the liner assembly 925 toward the center of the wellbore 910 . The shoe 940 may minimize problems associated with hitting rock ledges or washouts in the wellbore 910 as the liner assembly 925 is lowered into the wellbore. An outer portion of the shoe 940 may be made from steel. An inner portion of the shoe 940 may be made of a drillable material, such as cement, aluminum or thermoplastic, so that the inner portion may be drilled through if the wellbore is to be further drilled. A bore may be partially formed longitudinally through the shoe 940 and in fluid communication with one or more ports radially formed through the shoe. A sleeve 970 may be disposed in the bore and longitudinally movable between an open position exposing the ports and a closed position covering the ports, thereby fluidly isolating the ports from the bore. The sleeve 970 may be restrained in the open position by one or more frangible members 972 , such as shear screws.
[0096] Alternatively, the sleeve may have one or more ports formed radially therethrough and aligned with the shoe ports in the open position. The sleeve may be restrained in the open position by the threaded coupling between the valve 1000 and the shoe 940 and biased toward the closed position by a spring. Unthreading of the valve 1000 from the shoe 940 may release the sleeve, thereby allowing the spring to move the sleeve so that a solid portion of the sleeve covers the ports, thereby fluidly isolating the ports from the bore.
[0097] The expander assembly 950 may be disposed in the liner assembly 925 . The expander assembly 950 may include a tubular mandrel 955 . An upper end of the mandrel 955 may be connected to the work string 685 by a threaded connection and a lower end of the mandrel 955 may be releasably connected to the shoe 940 , such as by a threaded connection. The mandrel 955 may have a bore 990 formed therethrough in fluid communication with the surface of the wellbore 910 via a bore of the run-in string 685 . The mandrel 955 may support the liner assembly 925 during run-in.
[0098] The expander assembly 950 may further include a seal 960 longitudinally coupled to the mandrel 955 and engaged with an inner surface of the tubular portion 930 . The seal 960 may be fabricated from a pliable material, such as an elastomer. The seal 960 may act as a piston to move the expansion assembly 950 through the tubular section 930 upon introduction of fluid pressure below the seal 960 . Additionally or alternatively, tension from the run-in string may 685 be used to move the expansion assembly 950 through the tubular section 930 .
[0099] The expander assembly 950 may further include a two-position expander 975 . Detailed views of a suitable two-position expander may be found at FIGS. 3A and 3B of U.S. Pat. No. 7,121,351. The two-position expander may include a first assembly and a second assembly. The first assembly may include a first end plate and a plurality of first cone segments and the second assembly may include a second end plate and a plurality of second cone segments. Each end plate may be substantially round and have a plurality of T-shaped grooves formed therein. Each groove may match a T-shaped profile formed at an end of each cone segment.
[0100] An outer surface of each cone segment may include a first taper and an adjacent second taper. The first taper may have a gradual slope to form the leading shaped profile of the two-position expander 975 . The second taper may have a relatively steep slope to form the trailing profile of the two-position expander 975 . The inner surface of each cone segment may have a substantially semi-circular shape to allow the cone segments to slide along an outer surface of the mandrel 955 . A track portion may be formed on each first cone segment. The track portion may be used with a mating track portion formed on each second cone segment to align and interconnect the cone segments. The track portions may be a tongue and groove arrangement.
[0101] The first assembly and the second assembly may be urged longitudinally toward each other along the mandrel. As the first assembly and the second assembly approach each other, the first and second cone segments may be urged radially outward. As the first and second segments travel longitudinally along respective track portions, a front end of each second cone segment wedges the first cone segments apart, thereby causing the first shaped profiles to travel radially outward along the first shaped grooves of the first end plate. Simultaneously, a front end of each first cone segment wedges the second cone segments apart, thereby causing the second shaped profiles to travel radially outward along the second shaped grooves of the second end plate. The radial and longitudinal movement of the cone segments continues until each front end contacts a stop surface on each end plate, respectively. In this manner, the two-position expander 975 is moved from a retracted position having a first diameter to an expanded position having a second diameter that is larger than the first diameter.
[0102] FIG. 10 is a cross section of an electric valve 1000 . The expander assembly may further include the valve 1000 . The valve 1000 may include a body 1005 having a bore 1010 therethrough. The body 1005 may include an upper sub 1021 , a lower sub 1022 , and a sliding sleeve 1025 disposed therebetween. The upper and lower subs 1021 , 1022 may include threaded couplings for connection to the mandrel 955 and shoe 940 , respectively. A series of ports 1015 may be formed through a wall of the body 1005 for fluid communication between the interior and the exterior of the valve 1000 . One or more seals 1030 may be provided to prevent leakage between the sleeve 1025 and the subs 1021 , 1022 . The sliding sleeve 1025 may be longitudinally movable relative to the body 1005 for selectively opening and closing the ports 1015 .
[0103] The valve 1000 may further include an actuator 1045 for moving the sliding sleeve 1025 . The actuator 1045 may be a linear actuator. The valve may further include the RFID electronics package 800 for operating the actuator in response to instruction from a ball 995 having one of the RFID tags 850 p,a embedded therein. Alternatively, the electronics package 650 may be used instead. The sub 1022 may include a ball seat 1040 disposed therein and longitudinally movable relative thereto for receiving the RFID ball 995 , thereby closing the bore 1010 and longitudinally moving a longitudinal end of the ball seat 1040 into engagement with the sleeve 970 .
[0104] The expandable liner system 900 may be lowered into the wellbore 910 while receiving displaced wellbore fluid through the shoe 940 . Alternatively or additionally, fluid may be circulated to remove debris from the wellbore. After the system 900 is positioned within the wellbore 910 , the RFID ball 995 may be pumped from the surface through the run-in string 685 and the bores 990 , 1005 to the seat 1040 . Once the ball 995 has seated, fluid pressure may increase and cause the seat 1040 to push the sleeve 970 , thereby fracturing the shear screws 972 and closing the shoe ports.
[0105] The RFID ball 995 may include instructions for the electronics package 850 to open the ports 1015 after a predetermined time sufficient to sufficient for the sleeve 970 to close the shoe ports and/or after detecting a pressure sufficient to close the sleeve 970 .
[0106] FIG. 9B is a sectional view illustrating the reforming or unfolding of the corrugated liner 935 to form a launcher. The launcher may be formed to house the unactuated two-position-expander 975 prior to expanding the liner assembly 925 into contact with the wellbore 910 . The mandrel 955 may be released from the shoe 940 , such as by rotation of the mandrel from the surface. Fluid may then be pumped from the surface through the bore 990 and into the liner assembly 925 via the open ports 1015 . As fluid pressure increases in the liner assembly 925 , the corrugated liner section 935 may start to reform or unfold from the folded diameter to the larger folded diameter due to the fluid pressure. In this manner, the launcher is formed in the liner assembly 925 .
[0107] FIG. 9C is a sectional view of the expansion system 900 after positioning the two-position expander 975 in the launcher. After the launcher is formed, the fluid pressure below the seal 960 may be released by allowing fluid to exit through the tubular member 955 . The expander 975 may then be lowered into the launcher. The electronics package 850 may close the ports 1015 after a predetermined time sufficient to sufficient for the launcher to be formed and pressure to be relieved and/or after detecting the pressure sequence for forming the launcher and relieving pressure from the liner assembly.
[0108] FIG. 9D is a sectional view of the expandable liner system 900 illustrating the expansion of the corrugated liner section 935 . Once the ports 1015 have been closed, pressure in the bore 990 may be increased to activate a hydraulic actuator (not shown). The hydraulic actuator may move the expander 975 from the retracted position to the expanded position. The hydraulic actuator may be similar to any of the hydraulic actuators used in any of the isolation valves or setting tools discussed herein.
[0109] The electronics package 850 may open the ports 1015 after a predetermined time sufficient for actuation of the expander 975 to the expanded position and/or after detecting pressure sufficient for actuation of the expander 975 to the expanded position.
[0110] Once the expander 975 has been moved to the expanded position and the ports 1015 have opened, additional fluid pressure may be introduced through the bore 990 and the ports 1015 and into the liner assembly 925 (below the seal 960 ) to move the expander assembly 950 relative to the liner assembly 925 . The two-position expander 975 may expand the corrugated liner section 935 from the folded diameter to the unfolded diameter. During expansion, the two-position expander 975 may “iron out” the crinkles in the corrugated liner section 935 so that the corrugated liner section 935 is substantially reformed into its initial, substantially tubular shape. Reforming and subsequently expanding allows further overall expansion of the corrugated liner section 935 than would be possible with a tubular shape.
[0111] FIG. 9E is a sectional view of the expandable liner system 900 illustrating the expansion of the upper liner section 930 . Additional fluid may be introduced through the bore 990 and the ports 1015 and into the liner assembly 925 (below the seal 960 ) to continue the movement of the expansion assembly 950 relative to the liner assembly 925 until substantially the entire length of liner sections 930 , 935 are expanded into contact with the surrounding wellbore 910 and the casing 920 .
[0112] FIG. 9F is a sectional view of the completed wellbore 910 . Once the expander 975 has reached the bottom of the casing and expanded the overlapping liner into engagement with the bottom of the casing, the expander assembly 950 may be removed from the wellbore. A drill string (not shown) having a drill bit disposed on a lower end thereof may be deployed into the wellbore 910 and a lower portion of the liner 935 and the shoe 940 may be drilled through. Drilling of the wellbore 910 may then be continued. Cementing of the expanded liner assembly 935 may not be required. Alternatively, cement may be employed (before unfolding the corrugated portion and expanding the liner) to seal an annulus formed between the liner sections 930 , 935 and the surrounding wellbore 910 .
[0113] FIG. 11 illustrates an alternative expansion assembly 1150 , according to another embodiment of the present invention. Instead of the hydraulic actuator and valve 1000 used in the expansion assembly 950 , the expansion assembly may include an electric motor 1102 operated by the RFID electronics package 800 . The sleeve 970 may be replaced by a ball seat. The RFID ball 995 may then be pumped to the ball seat in the shoe. The electronics package 800 may then wait for the launcher to be formed and the expander 1175 to be moved into the launcher. The electronics package may then operate the motor 1102 . A portion of the expander 1175 may be longitudinally coupled to a gear (not shown), such as a worm gear, rotationally coupled to the motor 1102 such that rotation of the motor may move the portion of the expander longitudinally relative to another portion of the expander, thereby moving the expander between the retracted and expanded positions.
[0114] Alternatively, the corrugated portion 935 may be formed into the launcher using a lower cone (not shown) instead of or in addition to fluid pressure. Such an expansion system is illustrated in FIGS. 5A-D of the '351 patent. The alternative expansion system may utilize a hydraulic actuator to drive the lower cone into the corrugate portion 935 similar to FIGS. 9A-9F or the electric motor 1102 . Alternatively, the expansion system 550 illustrated in FIGS. 5A-D of the '351 patent may be used instead of the expansion systems 950 , 1150 and modified by replacing the hydraulic valve 555 with the electric valve 1000 in order to selectively open and close hydraulic ports 520, 565. A second actuator may be added to the electric valve and the ball seat 1040 may be replaced by the sleeve that closes port 565 in FIGS. 5A-D of the '351 patent. The second actuator may then move the sleeve to close the port. The first actuator 1045 and the ports 1015 may replace the ports 520 of the hydraulic valve 555. The shoe 590 may be modified to include a ball seat for catching the RFID ball 995 . The rest of the operation of the modified expansion system may be similar to that of the expansion system 555 discussed and illustrated in the '351 patent.
[0115] FIG. 12 is a half section of a portion of a setting tool 1200 , according to another embodiment of the present invention. The remainder of the setting tool 1200 may be similar to the setting tool 1 or the setting tool 700 except that the isolation valve 200 may be omitted.
[0116] The setting tool 1200 may include a connector sub 1202 , a mandrel 1203 , a piston assembly 1210 a , a pump 1205 , and the electronics package 800 . The connector sub 1202 may be a tubular member including a threaded coupling for connecting to the run-in string 685 and a longitudinal bore therethrough. The connector sub 1202 may also include a second threaded coupling engaged with a threaded coupling of the mandrel 1203 . One or more fasteners, such as set screws may secure the threaded connection between the connector sub 1202 and the mandrel 1203 . The mandrel 1203 may be a tubular member having a longitudinal bore therethrough and may include one or more segments connected by threaded couplings.
[0117] The piston assembly 1210 may include piston 1211 , sleeves 1212 , 1214 , housing 1215 , inlets 1216 , flow path 1209 , and ratchet assembly 1218 . The piston 1211 may be an annular member. An inner surface of the piston 1211 may engage an outer surface of the mandrel 1203 and may include a recess having a seal, such as an o-ring disposed therein. The inlet 1216 may be formed radially through a wall of the mandrel 1203 and provide fluid communication between a bore of the mandrel 1203 and an inlet of the pump 1205 . The sleeves 1212 , 1214 may be longitudinally coupled to the piston 1211 by threaded connections. A seal, such as an o-ring, may be disposed between the piston 1211 and the sleeves 1212 . Each of the sleeves 1212 , 1214 may be a tubular member having a longitudinal bore formed therethrough and may be disposed around the mandrel 1203 , thereby forming an annulus therebetween. The housing 1215 may be a tubular member, disposed around the mandrel 1203 , and longitudinally coupled thereto by a threaded connection. The housing 1215 may also be disposed about a shoulder formed in or disposed on an outer surface of the mandrel 1203 . Seals, such as o-rings, may be disposed between the housing 1215 and the mandrel 1203 and between the housing 1215 and the sleeve 1212 .
[0118] An end of the sleeve 1212 may be exposed to an exterior of the setting tool 1200 . The end of the sleeve 1212 may further include a profile formed therein or fastened thereto by a threaded connection. The profile may mate with a corresponding profile formed on an outer surface of the ratchet assembly 1218 , thereby longitudinally coupling the ratchet 1218 and the sleeve 1212 when the piston 1211 is actuated. The sleeve profile may engage the ratchet profile by compressing a spring, such as a c-ring. The c-ring may then expand to lock in a groove of the sleeve profile. Teeth formed on inner and outer surfaces of a lock ring of the ratchet assembly 1218 respectively engage corresponding teeth formed on an outer surface of the mandrel 1203 and an inner surface of a ring housing, thereby longitudinally locking the sleeve 1212 and thus the expander assembly 25 once the sleeve 1212 engages the ratchet assembly 1218 .
[0119] The pump 1205 and the electronics package may be disposed in the housing 1215 . The housing 1215 may include an inlet providing fluid communication between an inlet of the pump and the mandrel inlet. The housing may include an outlet providing fluid communication between an outlet of the pump and the flow path 1209 . The flow path 1209 may be formed between a recessed outer surface of the housing 1215 and an inner surface of the sleeve 1212 . The flow path 1209 may provide fluid communication between an outlet of the pump 1205 and a top of the piston 1211 .
[0120] In operation, one of the RFID tags 850 a,p may be embedded in the top plug 320 . When the top plug passes the electronics package 800 , the microprocessor may receive an instruction signal from the tag 850 a,p . The microprocessor 810 may then wait a predetermined period of time and/or detect a pressure indicative of seating of the top plug against the float collar/shoe. The microprocessor may then supply electricity from the battery pack 814 to an electric motor of the pump 1205 . The pump may intake the displacement fluid from the mandrel bore via inlet 1216 , pressurize the displacement fluid, and discharge the pressurized displacement fluid into the flow path 1209 , thereby longitudinally moving the piston 1211 and setting the hanger 105 .
[0121] Additionally, the microprocessor 810 may detect setting of the hanger 105 , such as by including a switch (not shown) in the ratchet assembly that is closed when the sleeve 1212 engages the ratchet assembly or a flow meter or stroke counter in the pump 1205 . Once the microprocessor 810 detects setting of the hanger 105 , the microprocessor may cease the electricity supply to the pump 1205 and then intermittently supply and cease electricity to the pump 1205 , thereby creating pressure pulses that may be detected at the surface. Alternatively, the microprocessor may intermittently supply and cease reversed polarity electricity to the pump, thereby reversing flow through the pump.
[0122] If the latch 50 does not release upon application of pressure in the mandrel bore, then a ball may be dropped through the run-in string and the mandrel bore to the ball seat, thereby isolating the liner from the mandrel bore. Pressure may then be further increased to release the latch.
[0123] Alternatively, the latch 50 may include an actuator, such as any of the actuators discussed above for the isolation valves, setting tools, or expanders, and the electronics package 650 . The microprocessor 660 may detect the pressure pulses and operate the actuator, thereby releasing the latch 50 and allowing the setting tool 1200 to be removed from the wellbore. Instead of the electronics package 650 , the latch actuator may be in electrical communication with the microprocessor 850 via a wire (not shown) extending through a wall of the mandrel 1203 .
[0124] FIGS. 13A-D illustrate a cross-section of an isolation valve 1300 , according to one embodiment of the invention. The isolation valve 1300 may be used instead of the isolation valve 200 described above. The isolation valve 1300 may include an upper adapter 1305 , a lower adapter 1395 , one or more couplers 1335 , one or more housings 1310 , 1340 , 1360 , one or more seals, such as o-rings 1301 , 1302 , 1303 , 1306 , 1307 , 1308 , 1309 , 1311 , 1312 , 1313 , 1314 , an upper piston member 1345 , a lower piston member 1347 , one or more sleeves 1315 , one or more pins 1317 , 1319 , an upper retaining member 1320 , a lower retaining member 1325 , an upper seat 1321 , a lower seat 1327 , one or more valve members, such as a ball 1330 , and one or more biasing members, such as a spring 1350 , and one or more lug rings 1365 .
[0125] FIG. 13A illustrates an open position of the isolation valve 1300 . The upper and lower adapters 1305 , 1395 may include cylindrical members having flow bores therethrough to provide fluid communication to the isolation valve 1300 . In one embodiment, the upper and lower adapters 1305 , 1395 include threaded ends configured to couple the isolation valve 1300 to the setting tool 1 and the wiper assembly 150 , respectively, as described above. In one embodiment, the isolation valve 1300 may be located in the setting tool 1 below the seal assembly 75 . The housing 1310 is coupled to the exterior surface of the upper adapter 1305 and the upper retaining member 1320 is coupled to the interior surface of the upper adapter 1305 , such that the sleeves 1315 are movably disposed between the housing 1310 and the upper retaining member 1320 . The sleeves 1315 may include cylindrically shaped bodies that are spaced apart and/or include grooves on their outer surfaces to provide fluid passages between the sleeves 1315 and the housing 1310 for fluid communication with one or more chambers 1329 disposed above the upper piston member 1345 . The upper and lower retaining members 1320 , 1325 are configured to retain the ball 1330 within the housing 1310 , as well as retain the upper and lower seats 1321 , 1327 into a sealed engagement with the outer surface of the ball 1330 , using one or more retainers 1323 (shown in FIG. 13A-2 ). The ball 1330 includes a spherical shape having a cylindrical bore disposed therethrough. The one or more pins 1317 may be connected to the ball 1330 and may extend into a slot in the sleeve 1315 . The one or more pins 1319 may be connected to the sleeve 1315 and may extend into an opening in the ball 1330 (shown in FIG. 13B-2 ). The sleeve 1315 , ball 1330 , and one or more pins 1317 , 1319 are configured to provide rotational movement of the ball 1330 upon relative axial movement of the sleeve 1315 , thereby opening and closing fluid communication through the bore of the isolation valve 1300 . As the sleeve 1315 moves relative to the ball 1330 , the pin 1319 moves the ball 1330 and uses the pin 1317 located in the slot of the sleeve 1315 as a pivot point to rotate the ball 1330 . The bore of the ball 1330 is rotated into and out of alignment with the bore of the isolation valve 1300 to open and close fluid communication therethrough.
[0126] The lower end of the sleeve 1315 is coupled to the upper end of the upper piston member 1345 to allow limited relative movement therebetween and further permit the piston member 1345 to move the sleeve 1315 relative to the ball 1330 . The upper piston member 1345 is disposed within the housings 1310 , 1340 , which are connected together using the coupler 1335 , such as with threaded connections. The upper piston member 1345 is coupled to the lower piston member 1347 , such as with a threaded connection. The lower piston member 1347 includes an upper shoulder that engages the spring 1350 , which is retained at its opposite end by the housing 1360 , which is coupled to the lower end of the housing 1340 . The spring 1350 is surrounded by the housing 1340 and is located within a chamber 1353 that is in fluid communication with the bore of the isolation valve 1300 via an opening 1349 in the wall of the lower piston member 1347 . The lower piston member 1347 extends through the housing 1360 and is coupled to the lower adapter 1395 . A nozzle 1343 may be disposed in the bore of the isolation valve 1300 above the opening 1349 to restrict the flow fluid therethrough prior to communicating with the opening 1349 and to create a pressure differential across the upper and lower ends of the isolation valve 1300 .
[0127] The upper piston member 1345 , the lower piston member 1347 , and the lower adapter 1395 are movable relative to the housings 1310 , 1340 , 1360 , and may be controlled using a J-slot arrangement that is provided between the housing 1360 and the lower piston member 1347 . The J-slot arrangement includes a channel 1363 machined in the inner wall of the housing 1360 . The channel 1363 is shown in FIG. 13A-1 in a “rolled-out,” flattened orientation. This pattern is preferably formed three times in the wall of housing 1360 so that each complete J-slot cycle covers 120 degrees of arc of the inner surface of housing 1360 . The lower piston member 1347 includes a recessed shoulder that carries one or more rotatable lug rings 1365 . The lug rings 1365 include an annular ring base which carries a projecting lug portion thereon.
[0128] FIG. 13A illustrates a first operational position of the isolation valve 1300 having both fluid pressure and flow through the bore of the isolation valve 1300 . As the isolation valve 1300 is pressurized, fluid pressure is communicated to the chambers 1329 , which generates a force (greater than the spring 1350 force) on the upper end of the upper piston member 1345 , thereby moving the upper piston member 1345 , the lower piston member 1347 , and the lug rings 1365 relative to the housing 1360 until a shoulder on the upper piston member 1345 abuts the coupler 1335 . The spring 1350 is compressed between the lower piston member 1347 and the housing 1360 , and the lug rings 1365 are moved in an extended portion of the channel 1363 to the position shown in FIG. 13A-1 . A shoulder on the upper end of the upper piston member 1345 engages a shoulder on the lower end of the sleeves 1315 and moves the sleeves 1315 and thus the pins 1317 , 1319 to rotate the ball 1330 so that the bore of the ball 1330 permits fluid flow through the bore of the isolation valve 1300 .
[0129] As illustrated in FIG. 13B , when the pressure in the isolation valve 1300 is reduced, the spring 1350 returns the lower piston member 1347 , the upper piston member 1345 , and the sleeves 1315 , so that the ball 1330 is rotated using the pins 1317 , 1319 into a closed position to prevent fluid flow through the bore of the isolation valve 1300 . The lower piston member 1347 moves the lug rings 1356 relative to the housing 1360 , and the lug rings 1356 are rotated and directed by the channel 1363 into the position shown in FIG. 13B-1 , which may also stop the retraction of the spring 1350 . As illustrated in FIG. 13C , pressure may then be applied above and to the isolation valve 1300 to conduct another operation, such as actuation of the expander assembly 25 described above, without opening fluid communication through the bore of the isolation valve 1300 . The upper piston member 1345 is moved within a recess of the sleeve 1315 a limited distance relative to the sleeve 1315 until the lug rings 1365 are moved by the lower piston member 1347 and are rotated and directed by the channel 1363 into the position shown in FIG. 13C-1 , which may prevent the upper piston member 1345 from moving the sleeves 1315 and potentially re-opening fluid communication through the isolation valve 1300 . As illustrated in FIG. 13D , when the pressure in the isolation valve 1300 is reduced or removed, the spring 1350 returns the upper piston member 1345 back to the position shown in FIG. 13B . However, the lower piston member 1347 moves the lug rings 1356 into the channel 1363 to the position shown in FIG. 13D-1 . From the position illustrated in FIG. 13D-1 , when the isolation valve 1300 is pressurized again, the lug rings 1365 will be directed into an extended portion of the channel 1363 (similar to the position shown in FIG. 13A-1 ) to permit movement of the sleeve 1315 via the upper and lower piston members 1345 , 1347 , thereby moving the ball 1330 and opening fluid communication through the bore of the isolation valve 1300 . The isolation valve 1300 can be opened and closed indefinitely by following this procedure.
[0130] FIGS. 14A-C illustrate a cross-section of an isolation valve 1400 , according to one embodiment of the invention. The isolation valve 1400 may be used instead of the isolation valve 200 described above. The isolation valve 1400 may include an upper housing 1410 , a lower housing 1420 , an upper mandrel 1430 , a lower mandrel 1440 , a retainer 1417 , one or more seals, such as o-rings 1403 , 1405 , 1407 , 1409 , 1411 , 1413 , one or more biasing members, such as a spring 1450 , a flapper valve insert 1460 , a flapper valve 1465 , an adapter 1470 , and one or more frangible members, such as shear screws 1475 .
[0131] The upper mandrel 1430 may include a cylindrical body having a bore disposed therethrough and one or more check valves 1435 located through the body of the upper mandrel 1430 . The check valve 1435 may optionally include a removable plug 1437 to prevent fluid from escaping through the top end of the upper mandrel 1430 . The upper mandrel 1430 may be coupled to the upper end of the upper housing 1410 , which may also include a cylindrical body having a bore disposed therethrough. The retainer 1417 may include a snap ring disposed within the inner surface of the upper housing 1410 and may be operable to retain the upper mandrel 1430 within the upper housing 1410 . The lower mandrel 1440 is disposed in the upper housing 1410 and extends through the lower housing 1420 , and further includes a cylindrical body having a bore disposed therethrough that sealingly engages the upper mandrel 1430 .
[0132] The lower mandrel 1440 includes a shoulder that sealingly engages the upper housing 1410 and has one or more check valves 1445 disposed through the wall of the shoulder. A chamber 1480 is formed between the bottom end of the upper mandrel 1430 , the inner surface of the upper housing 1410 , the outer surface of the lower mandrel 1440 , and the top end of the shoulder of the lower mandrel 1440 . The chamber 1480 is filled with a hydraulic fluid, such as silicon oil. The upper housing 1410 includes a shoulder at its lower end that sealingly engages the lower mandrel 1440 and the lower housing 1420 and has one or more check valves 1415 disposed through the wall of the shoulder. A chamber 1455 is formed between the bottom end of the shoulder of the lower mandrel 1440 , the inner surface of the upper housing 1410 , top end of the shoulder of the upper housing 1410 , and the outer surface of the lower mandrel 1440 . The chamber 1455 is filled with a hydraulic fluid, such as silicon oil. The check valve 1415 may be configured to allow some of the fluid to escape from the chamber 1455 as an increase in temperature may cause expansion of the fluid. The check valve 1445 may be configured to direct the fluid from the chamber 1455 into the chamber 1480 and prevent fluid flow in the reverse direction. The spring 1450 is housed in the chamber 1455 and is operable to telescope apart the lower mandrel 1440 and the upper housing 1410 .
[0133] The lower housing 1420 is coupled to the upper housing 1410 , such as through a threaded connection, and includes a cylindrical body having a bore disposed therethrough. A recess in the inner surface of the lower housing 1420 is configured to retain the flapper valve insert 1460 , which supports the flapper valve 1465 and abuts the bottom end of the upper housing 1410 . The flapper valve insert 1460 and the flapper valve 1465 are further retained by the outer surface of the lower mandrel 1440 . The lower end of the lower mandrel 1440 is positioned to maintain the flapper valve 1465 in an open position, which includes a spring member configured to bias the flapper valve 1465 into a closed position when unrestrained. The lower mandrel 1440 is releaseably coupled to the adapter 1470 via the one or more shear screws 1475 below the lower housing 1420 . The adapter 1470 includes a solid cylindrical member that provides a closed end of the isolation valve 1400 and is operable to couple the isolation valve 1400 to a device, such as a dart 1490 (shown in FIG. 14C ) or a cement plug.
[0134] In operation, the isolation valve 1400 is coupled to the dart 1490 via the adapter 1470 . The dart 1490 and the isolation valve 1400 may then be dropped from the surface of a wellbore into the setting tool 1 , the liner assembly 100 , or the wiper assembly 150 located in the wellbore. The dart 1490 may guide the isolation valve 1400 into the setting tool 1 , the liner assembly 100 , or the wiper assembly 150 until a shoulder 1425 of the lower housing 1420 engages and seals on a seat, such as a shoulder disposed in the bore of the seat 95 , the seal assembly 75 , the wiper assembly 150 , or other similar component. In an optional embodiment, the isolation valve 1400 may also include a c-ring coupled to the outer surface of the lower housing 1420 that is operable to engage a corresponding shoulder or recess to secure the isolation valve 1400 within the setting tool 1 , the liner assembly 100 , or the wiper assembly 150 . In one embodiment, the upper end of the upper housing 1410 may include a tapered shoulder configured to engage and seal on a seat, such as a shoulder disposed in the bore of the seat 95 , the seal assembly 75 , the wiper assembly 150 , or other similar component.
[0135] After the isolation valve 1400 is secured, pressure above the isolation valve 1400 may be applied against the top of the adapter 1470 to shear the shear screws 1475 and release the adapter 1470 and the dart 1490 from the lower mandrel 1440 and open fluid communication through the isolation valve 1400 . The release of the adapter 1470 and the dart 1490 from the lower mandrel 1440 allows the spring 1455 to move the lower mandrel 1440 to remove its lower end from preventing the flapper valve 1465 to bias into a closed position, as illustrated in FIG. 14B . The fluid in the chamber 1480 and the check valves 1435 , 1445 provide a configuration operable to delay the closure of the flapper valve 1465 after the adapter 1470 is released from the lower mandrel 1440 . As the chamber 1480 is collapsed between the upper mandrel 1430 and the lower mandrel 1440 , the fluid in the chamber 1480 is prevented from flowing into the chamber 1455 by the check valve 1445 but is allowed to be slowly dissipated through the check valve 1435 into the bore of the isolation valve 1400 . The pressure developed in the chamber 1480 after release of the lower mandrel 1440 may first release the plug 1437 from the flow path of the check valve 1435 to open fluid communication therethrough. As the fluid is ejected from the chamber 1480 , the portion of the fluid remaining in the chamber 1480 provides a resistance to the force of the spring 1450 and slows the movement of the lower mandrel 1440 . The sizing of the check valve 1435 may determine the rate at which the fluid is removed from the chamber 1480 and the sizing of the chamber 1480 may determine the amount of fluid which can be filled in the chamber 1480 . These two factors may be used to provide a predetermined timed resistance against the force of the spring 1450 to delay the movement of the lower mandrel 1440 away from the flapper valve 1465 and thus the closure of the flapper valve 1465 . During the time delayed closing of the flapper valve 1465 , the released adapter 1470 and dart 1490 may be directed through the remaining assembly, such as the liner assembly 100 , to facilitate removal of any remaining fluids, such as cement, from the assembly. As illustrated in FIG. 14C , the dart 1490 may include a c-ring 1493 and a seal 1495 , such as an o-ring, configured to engage and seal with the body 151 of the wiper assembly 150 , the operation of which may then begin as described above after engagement with the dart 1490 and during the time delayed closing of the flapper valve 1465 . After the flapper valve 1465 closes fluid communication through the isolation valve 1400 , pressure may then be applied above and to the isolation valve 1400 to conduct another operation, such as actuation of the expander assembly 25 described above, without opening fluid communication through the bore of the isolation valve 1400 .
[0136] FIG. 15A is a sectional view of an expandable liner system 1500 disposed in a wellbore 1510 according to one embodiment of the invention. The expandable liner system 1500 may be run-into the wellbore 1510 using the run-in string 685 . The system 1500 may include a liner assembly 1525 and an expander assembly 1550 . In one embodiment, the expandable liner system 1500 may be located proximate a lower end of a string of casing and the liner assembly 1525 may be set in the casing by positioning an upper portion of the liner assembly 1525 in an overlapping relationship with a lower portion of the casing. Thereafter, the expansion assembly 1550 may be employed to expand the liner assembly 1525 into engagement with the casing and/or the surrounding wellbore 1510 .
[0137] The liner assembly 1525 may include a tubular section 1530 at an upper end thereof and a shaped or a corrugated liner section 1535 disposed at the lower end thereof. It must be noted that the shape or corrugation of the liner section 1535 is optional such that the liner section 1535 is substantially cylindrical. Alternatively, the corrugated liner section 1535 may be located at any position along the liner assembly 1525 . A cross section of a suitable corrugated liner section may be found at FIG. 2G of U.S. Pat. No. 7,121,351, which is herein incorporated by reference in its entirety. The corrugated liner section 1535 and the substantially cylindrical liner section 1530 may be connected by a threaded connection or may be one continuous tubular body. The corrugated liner section 1535 may be fabricated from a drillable material, such as aluminum or a pliable composite. The corrugated liner section 1535 may have a folded wall having an initial inner diameter which may be reformed to define a larger second folded inner diameter and subsequently may be expanded to an even larger unfolded diameter. The corrugated liner section 1535 may be folded or deformed prior to insertion into the wellbore 1510 , to a non-tubular-shape, such as a hypocycloid, so that grooves are formed along the length of the corrugated liner section 1535 . The grooves may be symmetric or asymmetric.
[0138] The liner assembly 1525 may further include a shoe 1540 at the lower end thereof. The shoe 1540 may be longitudinally coupled to the corrugated portion, such as by a threaded connection. The shoe 1540 may be a tapered or bullet-shaped and may guide the liner assembly 1525 toward the center of the wellbore 1510 . The shoe 1540 may minimize problems associated with hitting rock ledges or washouts in the wellbore 1510 as the liner assembly 1525 is lowered into the wellbore. An outer portion of the shoe 1540 may be made from steel. An inner portion of the shoe 1540 may be made of a drillable material, such as cement, aluminum or thermoplastic, so that the inner portion may be drilled through if the wellbore is to be further drilled. A bore may be partially formed longitudinally through the shoe 1540 and in fluid communication with the wellbore 1510 .
[0139] The expander assembly 1550 may be disposed in the liner assembly 1525 . The expander assembly 1550 may include a tubular mandrel 1555 . An upper end of the mandrel 1555 may be connected to the run-in string 685 by a threaded connection and a lower end of the mandrel 1555 may be releasably connected to the shoe 1540 , such as by a threaded connection. The mandrel 1555 may have a bore formed therethrough in fluid communication with the surface of the wellbore 1510 via a bore of the run-in string 685 . The mandrel 1555 may support the liner assembly 1525 during run-in.
[0140] The expander assembly 1550 may further include one or more seals 1560 longitudinally coupled to the mandrel 1555 and engaged with an inner surface of the tubular portion 1530 . The seals 1560 may be fabricated from a pliable material, such as an elastomer. The seals 1560 may act as a piston to move the expansion assembly 1550 through the tubular section 1530 upon introduction of fluid pressure below the seals 1560 . Additionally or alternatively, tension from the run-in string may 685 be used to move the expansion assembly 1550 through the tubular section 1530 .
[0141] The expander assembly 1550 may further include a piston member 1570 disposed between the tubular section 1530 and the mandrel 1555 and movable relative to the tubular section and the mandrel. As illustrated in FIG. 15A-1 , the piston member 1570 may form one or more vacuum chambers 1513 and one or more piston chambers 1515 with the mandrel 1555 . One or more seals, such as o-rings 1511 , 1512 , and 1514 may be used to seal the chambers 1513 and 1515 . The mandrel 1555 may include a shoulder disposed on its outer surface having a flow path 1557 providing fluid communication between the bore of the mandrel 1555 and the piston chamber 1515 . A valve 1559 , such as a rupture disk, may be located in the flow path 1557 to control fluid communication to the piston chamber 1515 .
[0142] The expander assembly 1550 may further include a valve 1600 having a member 1610 , such as a pick, configured to actuate the valve 1559 to open fluid communication between the mandrel 1555 bore and the piston chamber 1515 for actuation of the piston member 1570 . In one embodiment, the valve 1600 may include the electronics package 650 or the RFID electronic package 800 described above. The valve 1600 may be actuated using an active or passive RFID tag embedded in a device, such as a dart 1580 , shown in FIG. 15B , or using mud pulses received from the surface. In one embodiment, alternative means of operating the valve 1600 may include a spring force, a gas spring, or an electric motor. In one embodiment, actuation of the valve 1600 may cause the member 1610 , such as a pick, to fracture the valve 1590 , such as a rupture disk, thereby opening fluid communication between the bore of the mandrel 1555 and the piston chamber 1515 .
[0143] The expansion assembly 1550 further includes a two-position expander 1575 and a cone 1577 . The cone 1577 is a tapered member that is operatively attached to the piston member 1570 , whereby movement of the piston member 1570 in relation to the liner assembly 1525 will also move the cone 1577 . Adjacent to the cone 1577 is the two-position expander 1575 . During run-in, both the two-position expander 1575 and the cone 1577 are disposed adjacent an end of the corrugated liner section 1535 .
[0144] Detailed views of a suitable two-position expander may be found at FIGS. 3A and 3B of U.S. Pat. No. 7,121,351. The two-position expander 1575 may include a first assembly and a second assembly. The first assembly may include a first end plate and a plurality of first cone segments and the second assembly may include a second end plate and a plurality of second cone segments. Each end plate may be substantially round and have a plurality of T-shaped grooves formed therein. Each groove may match a T-shaped profile formed at an end of each cone segment.
[0145] An outer surface of each cone segment may include a first taper and an adjacent second taper. The first taper may have a gradual slope to form the leading shaped profile of the two-position expander 1575 . The second taper may have a relatively steep slope to form the trailing profile of the two-position expander 1575 . The inner surface of each cone segment may have a substantially semi-circular shape to allow the cone segments to slide along an outer surface of the mandrel 1555 . A track portion may be formed on each first cone segment. The track portion may be used with a mating track portion formed on each second cone segment to align and interconnect the cone segments. The track portions may be a tongue and groove arrangement.
[0146] The first assembly and the second assembly may be urged longitudinally toward each other along the mandrel. As the first assembly and the second assembly approach each other, the first and second cone segments may be urged radially outward. As the first and second segments travel longitudinally along respective track portions, a front end of each second cone segment wedges the first cone segments apart, thereby causing the first shaped profiles to travel radially outward along the first shaped grooves of the first end plate. Simultaneously, a front end of each first cone segment wedges the second cone segments apart, thereby causing the second shaped profiles to travel radially outward along the second shaped grooves of the second end plate. The radial and longitudinal movement of the cone segments continues until each front end contacts a stop surface on each end plate, respectively. In this manner, the two-position expander 1575 is moved from a retracted position having a first diameter to an expanded position having a second diameter that is larger than the first diameter.
[0147] In operation, the expandable liner system 1500 may be lowered into the wellbore 1510 adjacent an area of interest, such as an end of an existing casing section. Wellbore fluids may flow up through the bore of the mandrel 1555 and the run-in string 685 as the system 1500 is run into the wellbore 1510 . A dart 1580 may be dropped from the surface of the wellbore 1510 , directed through the expandable liner system 1500 , and seated in the shoe 1540 , thereby closing fluid communication between the wellbore 1510 and the bore of the mandrel 1555 . The dart 1580 may include an embedded RFID tag used to communicate with the valve 1600 . A radio frequency communication may be directed between the dart 1580 and the valve 1600 to actuate the valve 1600 and move the member 1610 to open the valve 1559 . The pressure in the bore of the mandrel 1555 may be increased and communicated to the piston chamber 1513 via the flow path 1557 to move the piston member 1570 . The piston member 1570 causes the two-position expander 1575 and the cone 1577 to move relative to the mandrel 1555 and the liner assembly 1525 , thereby allowing the cone 1577 to reform the corrugated liner section 1535 . The cone 1577 reforms the corrugated liner section 1535 and may engage a shoulder disposed on the outer surface of the mandrel 1555 or the end of the shoe 1540 , which prevents further movement of the cone 1577 . Fluid pressure continues to be introduced into the piston chamber 1515 , thereby causing the two-position expander 1575 to move closer to the cone 1577 to begin the activating process. As the fluid pressure continues to urge the two-position expander 1575 against the cone 1577 , the first and second cone segments of the two-position expander 1575 move radially outward into contact with the surrounding liner 1535 (actuation of the two-position expander 1575 was described above).
[0148] FIG. 15C illustrates the two-position expander 1575 expanding the corrugated liner section 1535 and the liner section 1530 . As shown, the two-position expander 1575 has expanded a portion of the liner section 1535 from the folded diameter to the unfolded diameter. In other words, during the expansion process, the two-position expander 1575 basically “irons out” the crinkles in the corrugated liner section 1535 so that the liner section 1535 is substantially reformed into its initial tubular shape. Reforming and subsequently expanding allows further expansion of the liner section 1535 than was previously possible because the reformation process may not use up the 25% limit on expansion past the elastic limit. Subsequently, the expansion assembly 1550 is rotated in one direction to release the connection between the mandrel 1555 and the shoe 1540 and/or dart 1580 . At this point, the expansion assembly 1550 and the liner assembly 1525 are disconnected, thereby unlocking the one or more seals 1560 . As additional fluid pressure is introduced through the bore of the mandrel 1555 , the entire expansion assembly 1550 is moved relative to the liner assembly 1525 as fluid pressure acts upon seals 1560 . In this manner, substantially the entire length of liner sections 1530 and 1535 are expanded into contact with the surrounding wellbore 1510 .
[0149] FIG. 15D illustrates the removal of the expander assembly 1550 from the liner assembly 1525 . As illustrated, a device 1590 , such as a ball, may be dropped from the surface of the wellbore 1510 and landed into a seat of the mandrel 1555 , thereby closing fluid communication between the bore of the mandrel 1555 and the surrounding annulus of the wellbore 1510 . Pressure may then be increased in the expander assembly 1550 and used to collapse the two-position expander 1575 into an unexpanded (reduced outer diameter) position to facilitate removal of the expander assembly 1550 . The cone segments of the two-position expander 1575 may be retracted to provide a reduced outer diameter of the expansion assembly 1550 to allow the assembly to be removed from the liner assembly 1525 and/or the wellbore 1510 .
[0150] FIGS. 15C-1 , 15 D- 1 , and 15 D- 2 illustrate an embodiment of the expander assembly 1550 having a release mechanism 1700 used to retract the two-position expander 1575 into an unexpanded position as stated above. The release mechanism 1700 is configured to retract the two-position expander 1575 into an unexpanded position using fluid pressure and/or mechanical rotation of the expander assembly 1550 . The release mechanism 1700 may be disposed between the two-position expander 1575 and the cone 1577 of the expansion assembly 1550 .
[0151] The release mechanism 1700 may include an adapter 1710 coupled to the two-position expander 1575 at an upper end and rotatively coupled to a first inner mandrel 1715 via one or more screws 1719 . The screws 1719 may reside in a slot in the body of the adapter 1710 to allow relative axial movement between the adapter 1710 and the first inner mandrel 1715 . The adapter 1710 and the first inner mandrel 1715 may include cylindrical members having bores disposed through the bodies of the members. The first inner mandrel 1715 may similarly be coupled at its upper end to a mandrel 1717 , which is disposed between the two-position expander 1575 and the mandrel 1555 and is operable to facilitate make-up of the expander assembly 1500 and the release mechanism 1700 .
[0152] The release mechanism 1700 may include an upper sleeve 1720 , a middle sleeve 1725 , and a lower sleeve 1730 , each comprising cylindrical members having bores located through the bodies of the members. The upper sleeve 1720 may abut a shoulder disposed on the outer surface of the adapter 1710 and may be releaseably coupled to the middle sleeve 1725 via one or more frangible members, such as shear screws 1721 . An opening 1731 is disposed through the body of the upper sleeve 1720 , which is in communication with a chamber formed between the upper sleeve 1720 and the middle sleeve 1725 . The chamber is sealed using one or more seals, such as o-rings 1754 , 1753 , 1756 , and 1752 . The chamber is also in communication with an opening 1733 disposed through the body of the first inner mandrel 1715 , which is further in communication with an opening 1734 disposed through the body of the mandrel 1555 and thus the inner bore of the expander assembly 1550 . When the inner bore of the expander assembly 1550 is pressurized, the fluid pressure is directed to the chamber via the openings 1734 , 1733 , 1731 , which then telescopes apart the upper sleeve 1720 and the middle sleeve 1725 to shear the shear screws 1721 and allow relative movement between the upper and middle sleeves. The pressure also telescopes apart the adapter 1720 and the upper and middle sleeves 1720 , 1725 relative to the first inner mandrel 1715 .
[0153] As illustrated in FIG. 15C-1 , a set of dogs 1735 may be located in a slot of the upper sleeve 1720 and may extend into recesses disposed on the outer surface of the first inner mandrel 1715 . The dogs 1735 may include a cylindrical member having one or more shoulder portions extending from the inner diameter and one or more recesses disposed on the outer diameter of the member. The dogs 1735 may be surrounded by the lower sleeve 1730 , which is coupled to the upper end of a lower housing 1760 . The lower sleeve 1730 engages the outer surface of the dogs 1735 adjacent the recesses disposed on the outer diameter of the dogs 1735 to prevent the dogs 1735 from releasing engagement with the first inner mandrel 1715 . The dogs 1735 are engaged with the first inner mandrel 1715 to prevent relative movement between the adapter 1710 (via the upper sleeve 1720 ) and the first inner mandrel 1715 , thereby preventing retraction of the two-position expander 1575 . A guide member 1740 is coupled to the lower end of the upper sleeve 1720 to facilitate translation of the upper sleeve 1720 relative to the lower housing 1760 . The housing 1760 may be releasably coupled to a second inner mandrel 1750 via one or more frangible members, such as shear screws 1722 . The second inner mandrel 1750 may also be coupled to the first inner mandrel 1715 at one end and the cone 1577 at the opposite end. A seal, such as a packing element 1751 , may be disposed between the first inner mandrel 1715 , the second inner mandrel 1750 , and the mandrel 1555 .
[0154] As illustrated in FIG. 15D-1 , the device 1590 (shown in FIG. 15D ) may close fluid communication through the expander assembly 1550 and allow the bore of the mandrel 1555 to be pressurized, which may be communicated to the chamber between the upper sleeve 1720 and the middle sleeve 1725 . The shear screws 1721 between the upper sleeve 1720 and the middle sleeve 1725 (and the shear screws 1722 between the lower housing 1760 and the second inner mandrel 1750 ) have been sheared (as described above) and the middle sleeve 1725 is used to direct a shoulder portion on the inner diameter of the lower sleeve 1730 into the recesses on the outer diameter the dogs 1735 . This engagement allows the dogs 1735 to move radially outward away from the first inner mandrel 1715 . The upper sleeve 1720 directs the dogs 1735 axially relative to the first inner mandrel 1715 to allow the dogs to disengage from the recesses in the first inner mandrel 1715 and retract into the middle sleeve 1725 . When the dogs 1735 are disengaged from the first inner mandrel 1715 , the adapter 1710 may move downward relative to the first inner mandrel 1715 to retract and pull apart the two-position expander 1575 . The movement relative to the first inner mandrel 1715 may be stopped when the guide member 1740 abuts the upper end of the second inner mandrel 1750 . The expander assembly 1550 may then be removed from the wellbore with the two-position expander 1775 in the retracted position.
[0155] As illustrated in FIG. 15D-2 , the two-position expander 1575 may be retracted into an unexpanded position by rotation of the mandrel 1555 . Rotation of the mandrel 1555 may be used to induce relative movement between the second inner mandrel 1570 and the lower housing 1760 and thus shear the shear screws 1722 therebetween. Release of the shear screws 1722 allows the middle sleeve 1730 to move relative to the dogs 1735 , which may then retract into the middle sleeve 1730 and radially outward relative to the first inner mandrel 1715 as described above. Relative movement between the upper sleeve 1720 and the first inner mandrel 1715 may allow the lower end of the upper sleeve 1720 to move the dogs 1735 out of the recesses in the first inner mandrel 1715 and release the engagement therebetween to allow retraction of the two-position expander 1775 into the unexpanded position.
[0156] Any of the above discussed setting tools and/or liner assemblies may be installed in a pre-drilled wellbore or drilled in using a drilling with liner operation. Further, any of the above discussed setting tools may be used with a conventional liner hanger, discussed in the Background section. Further, any of the setting tool actuators may be used for the isolation valves and vice versa.
[0157] While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
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Embodiments of the invention generally relate to tools and methods for hanging and/or expanding liner strings. In one embodiment, a method of hanging a liner assembly from a previously installed tubular in a wellbore includes running the liner assembly and a setting tool into the wellbore using a run-in string. The setting tool includes an isolation valve and the liner assembly includes a liner hanger and a liner string. The method further includes sending an instruction signal from the surface to the isolation valve, wherein the isolation valve closes in response to the instruction signal and isolates a setting pressure in the setting tool from the liner string; and increasing fluid pressure in the setting tool, thereby setting the liner hanger.
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CROSS REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of co-pending application Ser. No. 764,721 filed Feb. 2, 1977, now abandoned.
BACKGROUND AND SUMMARY OF THE INVENTION
This invention relates to a new vibration generating mechanism. It will find usage in nearly all equipment where vibration or centrifugal force is used to perform work. This mechanism can be adapted to equipment such as vibratory conveyors, vibratory screens, vibratory feeders, vibratory screeds, vibratory rollers/ compactors, separators, vibratory metal finishing, grain crushers, tamping plates, pile drivers, and pavement breakers. The variable eccentricity, force and amplitude values that are made available by this invention, for every vibrational speed, will be found to increase the versatility of all the equipment listed. In all of these applications it is desirable at times under varying loads and when working with a variety of material to keep the same vibrational frequency and change the amount of generated centrifugal force and vibrational amplitude. On the other hand it is desirable at times to change the freqency without changing the force. Another option with this device is to increase the frequency and decrease the force starting from a given value of frequency and force. Controls can be adapted to use the mechanism as a constant force/variable frequency device that is desirable on certain applications.
This invention relates specifically to a vibration generating mechanism that has a movable weight(s) that is (are) positioned selectively to change the eccentricity of the mechanism. The changes in eccentricity are made by controlling the flow of fluid (liquid or air) to the mechanism. The changes can be made while the mechanism is stationary or rotating. The eccentricity can vary from nearly zero to any reasonable value determined by the designer. The mechanism provides a range of eccentricity values for any speed value. The invention includes a pressure gauge(s) which records the pressure caused by the tendency of the movable weight(s) to move outwardly as the mechanism rotates. This pressure reading can be directly converted to the value of centrifugal force being generated when the dimensions of the weight are known. The eccentricity is determined when the centrifugal force and rotational speed are known. The theoretical amplitude desired is generally used as a given value and a starting point in determining the eccentricity needed in a vibration generating mechanism.
The invention includes a source of fluid (liquid or air) pressure. The pressure source used will depend on the application, material availability and the designer's choice. An air compressor with common components and valving is one choice. A hydraulic pump with proper circuitry is another choice. A fluid cylinder with proper circuitry and actuating means can be used. A grease gun can also be used to position the weight(s). A cylinder with proper circuitry common in the art and actuating means would be a preferred embodiment for many applications because it could be used as valve means and a pressure source.
Various embodiments of the invention are disclosed. The movable weights are different in character and arrangement and are pictorially described in the drawings. All of the weights are positioned and held in position by fluid in the various cylinder means. Pressurized fluid is channeled to and from a cylinder through various common means from a bearing journal passage connected with a rotary coupling connected with a supply line that is connected to valve means and one of the variety of pressure sources listed previously. A pressure gauge is connected to the supply line recording pressure relating directly to the centrifugal force being generated as the mechanism is rotated.
Knowledge of the generated centrifugal force and the amplitude along with the capability of adjusting them without changing the vibrating speed will make the work in many vibrating applications more efficient. The inventor knows of no other vibration generating mechanism that provides this information directly and continuously. Heretofore with most vibratory generating mechanism except as noted herein the only way to adjust the force was to change the vibrating speed. With this invention the force and amplitude can be adjusted between zero and some predetermined maximum rated value fo each effective infinitely variable vibrating speeds. The controls referred to previously in respect to constant force/ variable frequency are an optional feature that will be economically feasible for some applications where constant force is a prime requisite or where limiting the value of centrifugal force is mandatory. These pressure sensitive controls common to the art can be built into or adapted to the valve means and incorporated in all the embodiments. As an option these controls are shown in dashed lines attached to the valve means in the drawings.
The first embodiment includes a rotatable mechanism with a piston like movable weight enclosed in a cylinder. The weight is offset and thus has a tendency to move away from the axis of rotation when the mechanism is rotated. This movement is resisted and restricted by fluid in the cylinder. The positioning of the weight and the amount of force generated for any of the infinitely variable speeds is controlled by forcing fluid into the cylinder decreasing the eccentricity or by allowing fluid to leave the cylinder which increases the eccentricity. The control of this flow is accomplished through valve means and a pressurized fluid source. The valve means with pressure sensitive controls may be used as an option. The mechanism includes a rotary fluid coupling so that the transfer of fluid can be made whether or not the mechanism is rotating. The fluid supply line to the rotary coupling does not rotate. It is connected to valve means and fluid pressure source that are located on a non-vibrated part or on a part from which vibration has been effectively dampened. A significant part of this invention is the pressure gauge connected with the supply line that records the fluid pressure in the cylinder. This value can be converted to generated centrifugal force when the weight and size of the movable weight is known.
A second embodiment incorporates cylinder means with enclosed movable weights as described above. In addition it incorporates a duplex rotary fluid coupling which allows for two separate fluid circuits to pass through the bearing journal nearest to the rotary coupling. One of these circuits controls the weight as in the first embodiment. The other circuit passes through the passage in the opposing bearing journal and the flow therein controls the position of the movable weight in a second similar mechanism that is rotated synchronously with the mechanism that is shown.
A third embodiment incorporates two cylinders with enclosed piston like weights. The movement of the offset weights is resisted and restricted by fluid in the cylinders. The fluid is supplied through a duplex rotary fluid coupling mounted on the end of the mechanism. The duplex rotary fluid coupling has two separate passages and separate supply lines so that the position of the weights inside the cylinders are controlled individually as desired.
A fourth embodiment incorporates a cylinder with an included piston and piston rod. The piston rod extends through one end of the cylinder in a normal manner and is fastened to a weight outside the cylinder. The piston, seals, piston rod and exterior weight combine to make a compound movable eccentric weight. The eccentricity of the center of gravity of the movable weight is controlled by the flow of fluid in and out of the piston rod end of the cylinder.
A fifth embodiment incorporates multiple cylinders as in the fourth embodiment in a extended shaft body. The piston rods extend and are fastened to a common weight. The cylinders are fluidly connected so that the fluid pressure is the same in both and two pistons move as one in response to fluid flow and centrifugal force. A simple linkage is used to assure a square movement of the exterior weight.
A sixth embodiment incorporates a movable cylinder body as the movable eccentric weight. The piston rod is fixed to the shaft body and the location of the cylinder body in relation to the axis of rotation is controlled by the flow of fluid through a piston rod passage. The piston rod is fixedly mounted to the shaft body.
A seventh embodiment incorporates a cylinder fixedly mounted on the shaft body. The piston rod is connected to linkage that controls the motion of dual pivoting weights. The piston, seals, and piston rod, linkage, pins and pivoting weight comprise the compound movable eccentric weight. The eccentricity or location of the center of gravity of the movable weight is controlled by the flow of fluid in and out of the piston end of the cylinder.
An eighth embodiment incorporates a cylinder pivotly mounted on the shaft body. The piston rod is pin connected to a pivoting weight. The piston, seals, piston rod, connecting pin and pivoting weight comprise the compound movable eccentric weight. The eccentricity or location of the center of gravity of the movable weight is controlled by the flow of fluid in and out of the piston rod end of the cylinder.
DESCRIPTION OF THE DRAWINGS
A more complete understanding of the invention may be had by reference to the following Detailed Description when taken in conjunction with the accompanying Drawings wherein:
FIG. 1 is a top view of a variable eccentric mechansim except for the gauge means, valve means and pressure source means.
FIG. 2 is a side view of the mechanism shown in FIG. 1 partially sectioned with parts broken away to illustrate more clearly the construction of the invention. The sectioned view of the shaft has been rotated to provide a clear picture. connecting conduit is pictorially shown to connect with the rotated section.
FIG. 3 is a top view of a variable eccentric mechanism incorporating another embodiment of the invention except for gauge means, valve means and pressure source means.
FIG. 4 is a side view of the mechanism shown in FIG. 3 including the gauge means, the valve means and the pressure source means.
FIG. 5 is a side view of another embodiment partially sectioned to illustrate more clearly the construction of the invention. FIG. 6 is a side view of another embodiment of the invention partially sectioned to illustrate more clearly the construction of the invention.
FIG. 7 is a top view of another embodiment of the invention except for gauge means, valve means, optional control means and pressure source means.
FIG. 8 is a side view of the embodiment shown in FIG. 7.
FIG. 9 is a side view of the embodiment shown in FIGS. 7 and 8 with parts broken away and partially sectioned showing linkage parts of the embodiment which are not shown in FIGS. 7 and 8.
FIG. 10 is a side view of another embodiment of the invention partially sectioned to illustrate more clearly the construction of the invention.
FIG. 11 is a side view of another embodiment with parts broken away and partially sectioned to illustrate more clearly the construction of the invention.
FIG. 12 is an end view of the embodiment shown in FIG. 11 except for the gauge means, valve means, optional control means and pressure source.
FIG. 13 is a top view of the embodiment shown in FIG. 11 and FIG. 12 except for the gauge means, valve means, optional control means and pressure source.
FIG. 14 is a side view of another embodiment with parts broken away and partially sectioned to illustrate more clearly the construction of the invention.
FIG. 15 is an end view of the embodiment shown in FIG. 14 except for the gauge means, valve means, optional control means and pressure source.
FIG. 16 is a sectional view taken generally along the line 16--16 in FIG. 14 is the direction of the arrows.
DETAILED DESCRIPTION
Referring now to the drawings, FIGS. 1 and 2 show the same variable eccentric mechanism 10. The mechanism has a cylinder-like chamber 11 fastened to or being a part with shaft means 12. The shaft means has a drive means 13 shown in this embodiment as an integral splined shaft. The shaft means is journaled at 14 and 15 for the mounting of bearings.
The movable weight 16 is shown in an intermediate eccentric position. It is positioned and held by the fluid 17. Said weight is further positioned by the seals 18 and 19 which engage the weight and contact the interior surface of the chamber 11.
The minimum eccentricity of the mechanism is accomplished when said weight is forced against flange 20 of top cap 21. The eccentricity in this condition approaches zero. The cap 2 is equipped a breather 22 to avoid a pressure or vacuum resistance to the movement of the weight 16. The cap is fastened to the chamber by common means.
The maximum eccentricity of the mechanism is accomplished when said weight is forced against the flange 23 of the bottom cap 24 by gravity and/or centrifugal force.
The fluid 17 that forces and allows movement of the weight enters and leaves the chamber through conduit 25 which is fastened with common fittings to the bottom cap 24 and the bearing journal passage 26. Said passage is connected to rotary coupling 27 through the connecting part 28 that is fastened by common means to the shaft.
Fluid is transferred to and from the rotary coupling through the supply line 29. A pressure gauge 30 is installed by common means in the supply line. The reading on the gauge provides the unit pressure in the supply line, rotary coupling, bearing journal passage, conduit and chamber.
Valve means 31 is located in the supply line to stop the fluid flow and regulate the amount of fluid flow in or out of said chamber through the means provided.
Pressure source 32 provides pressurized fluid as required through the means provided to change the eccentricity.
In FIGS. 1 and 2 a second pressure source 33 is shown to be connected to a circuit similar to the one described previously but without a chamber and weight. Pressure source 33 provides pressurized fluid as required to change the eccentricity of another variable eccentric mechanism similar to the one shown. Fluid is furnished as required to the valve means 34, supply line 35, pressure gauge 36, fluid coupling 37 through connecting part 38 to bearing journal passage 39, through conduit 40 and into bearing journal passage 41. Plug 42 closes this passage when fluid flow is not required to change the eccentricity of another similar variable eccentric mechanism that is connected by common means to turn synchronously with the embodiment shown.
With the second pressure source in mind let us refer to FIGS. 3 and 4. These show a variable eccentric mechanism 43 with two cylinder-like chambers 44 and 45, with a weight that is not shown disposed in each chamber. One pressure source 46, through the circuit provided, moves the weight in chamber 44 and the second pressure source 47 moves the weight in the second chamber 45. The circuitry is the same in embodiment 43 as in 10 except that second pressure source is used to move a second weight within the same mechanism rather than being passed on to a separate variable eccentric mechanism.
FIGS. 1 and 2 show the preferred embodiment. It is preferred because of the versatility evident in the ability to pass control fluid to and from another vibration generating mechanism. Two vibration generating mechanisms often have an advantage because they can develop a synchronized force whose effect can be divided between four supporting bearings rather than two. The obvious advantage is an increase in the life of the bearings. When bearing loads and bearing life are not a problem and enough centrifugal force can be developed from a single movable weight a single passage through one bearing housing and a single rotary coupling would be a more economical mechanism to produce. In that event, pressure source 33, valve means 34, supply line 35, gauge means 36, rotary coupling 37 with its connecting part 38, passage 39, conduit 40, passage 41 and plug 42 would not be used.
In the zero eccentricity mode the mechanism is balanced by the distribution of weight of the total mechanism. The center of gravity of the weight is slightly below the center line of the bearing journals so that it will tend to move radially outward when the shaft is rotating.
It is noted in FIG. 2 that the top cap 21 is much thicker than the bottom cap 24. In this manner it not only serves as a stop in the zero eccentricity mode but counter balances the weight of the chamber that extends further below than above the centerline of the bearing journals.
The eccentricity is increased by using the valve means to allow fluid to flow from the chamber. This allows the weight to assume a more off center position. To decrease the eccentricity the valve means is used to regulate a flow of pressurized fluid into the chamber. This forces the weight toward the center line of the bearing journals.
When the eccentricity is increased at any given rotational speed the centrifugal force and amplitude are increased. Conversely when the eccentricity is decreased at any given rotational speed the centrifugal force and amplitude are decreased. Vibrational amplitude is adjustable from zero to a predetermined value at all effective rotational speeds.
This change in force will register on the pressure gauge as an increase or decrease in pressure. Since the shape of the movable weight is known the pressure will indicate the force through direct conversion. Force = Pressure x Area. The weight is offset from the axis of rotation even when the mechanism is balanced. Pressure will always be generated except when the weight is in its maximum eccentric position and its movement is resisted by a mechanical stop rather than by the presence of fluid and fluid pressure. The fluid pressure will be zero under that condition. At that point the eccentricity of the center of gravity of the movable weight is known and the centrifugal force will vary directly with the second power of the rotational speed. The pressure source will be chosen to be able to develop adequate pressure to force the weight away from the stop back toward the axis of rotation when a reduction in force and eccentricity is desired. In larger mechanisms fluid weight may be significant in calculating the generated centrifugal force. The weight of fluid will always be considered to assure a balanced mechanism in the zero eccentricity mode.
Turning to FIG. 5 there is shown a modification of the mechanism 10 shown in FIGS. 1 and 2. The mechanism 10a incorporates a simple rotary fluid coupling 50 fastened by connecting part 51 to the bearing journal 15 end in place of the duplex rotary fluid coupling made up of parts 27, 28, 37, and 38 shown in FIGS. 1 and 2. The simple rotary fluid coupling allows for a single fluid circuit to pass to the mechanism 10a while the duplex rotary fluid coupling allows for two separate fluid circuits to pass to mechanism 10.
Continuing in FIG. 5 the mechanism 10a incorporates single supply line 29 connected to pressure source 32, valve means 31, pressure gauge 30 and body of the rotary coupling 50. Control means 52, an optional device, is shown in dashed lines, as a part of and adapted to valve means 31. This control means is pressure sensitive to the pressure in the cylinder through the connecting circuit. The control operates the valve means to allow flow in or out of the cylinder. This flow maintains or limits the pressure in the circuit by positioning the movable weight. The control is readily adjustable either manually or by remote control means.
The pressure source 32 is one of various types common in the art that supplies pressurized fluid as required to force the weight to a less eccentric position.
Continuing again in FIG. 5 the mechanism contains movable weight 16, and other features and parts found in the mechanism 10 shown in FIGS. 1 and 2. The zero eccentricity mode and the maximum eccentricity are achieved in the same manner as previously described.
The mechanism 10a shown in FIG. 5 and subsequent mechanisms show the cylinder means as an integral part of a cast or forged shaft body. It is understood to those skilled in the art that the shaft body may be a weldment including the cylinder means. The cylinder means may also be a separate replaceable piece commonly fastened to a cast, forged or fabricated shaft body.
The mechanism is drivenly rotated through drive means 13. Drive means 13 is shown as an external spline. Drive means such as internal splines, shaft and key or other conventional structure may be used.
FIG. 6 describes a mechanism 60 which includes a compound movable eccentric weight. Piston 61, seals 18 and 19, piston rod 62, and exterior weight 63 comprise the compound movable eccentric weight. When the piston 61 is located against the flange 20 of cap 21 the mechanism is essentially balanced and the eccentricity is zero. The center of gravity of the movable weight at the same time is offset towards the cap 24 and flange 66. Flange 66 acts as a stop to limit the travel of the piston which limits the maximum eccentricity. Because the center of gravity of the movable weight is offset it tends to move in the direction of the cap 24. This movement is resisted and restricted by fluid 17 that fills the cylinder below the piston 61 and around the rod 62 as shown. The weight and location of the fluid is considered in calculating balance and centrifugal force. The fluid will restrict the movement until valve means 31 allows fluid to flow from the cylinder 11 through the bearing journal passage 26, through the rotary coupling made of parts 50 and 51, and supply line 29.
In the mechanism 60 shown in FIG. 6 the fluid 17 enters and leaves the cylinder 11 through the bearing journal passage 26 at a point below the top of flange 66.
Control means 52, an optional device, is shown in dashed lines, as a part of and adapted to valve means 31. This control means is pressure sensitive to the pressure in the cylinder through the connecting circuit. The control operates the valve means to allow flow in or out of the cylinder. This flow maintains or limits the pressure in the circuit by positioning the movable weight. The control is readily adjustable either manually or by remote control means.
The pressure source 32 is one of various types common in the art that supplies pressurized fluid as required to force the weight to a less eccentric position.
The eccentricity of the compound weight is adjustable in the same manner as the eccentricity of the weights in mechanism 10 shown in FIGS. 1 and 2. The exterior weight 63 and part of the piston rod 62 are shown in broken lines in a second position to depict a more eccentric position.
The radial movement of the compound weight is slidingly guided by the piston seals 18 and 19 fixed to piston 61 sliding in the cylinder 11 and the sliding contact between the piston rod 62 and the packing 65 fixed in the packing flange 64 which is fastened to cap 24.
The breather 22 in cap 21 avoids a pressure or vacuum resistance to movement of this piston 61 with seals 18 and 19 within the cylinder.
The mechanism is drivenly rotated through drive means 13. Drive means 13 is shown as an external spline. Drive means such as internal splines, shaft and key or other conventional structure may be used.
FIGS. 7, 8 and 9 picture another embodiment of the invention. The mechanism 70 has many primary parts that are like those in mechanism 60. Mechanism 70 has an elongated U shaped shaft body 12 which accomodates two cylinders 11. An elongated exterior weight 72 shown in FIGS. 8 and 9 is fastened to the piston rods 62 from each of the two cylinders. The fluid circuitry is the same except that the two cylinders are fluidly connected by conduit 71 and common fittings (not itemized) shown in FIG. 7. The cylinder 11 in proximity to the rotary coupling 50 is connected with the pressure source 32 as in mechanism 60.
FIG. 9 shows linkage 73 (not shown in FIGS. 7 and 8) that is used in synchronizing the movement of the piston rods 62. The action is obvious to those skilled in the art. The linkage comprises bell cranks pivotly pin connected to the shaft body 12 with pivotal connections to push-pull rods and with the rods being pivotly connected to brackets on the exterior weight. Even though the pressures in the two cylinders are intended to be the same through a common circuit variable resistances between the seals and cylinders and between packings and rods in the sliding action would tend to make one rod move more easily than the other and the elongated weight could move in and out in a position not parallel to the axis of rotation and offer an unpredictable action. It will be understood by those skilled in the art that other apparatus such as gearing, pulleys and cable etc. could be used to synchronize the movement of the rods 62.
The position of the compound movable weight, which includes two sets of seals, pistons, piston rods and exterior weight 72, is controlled through the flow of fluid in and out of the piston rod ends of the cylinders. The flow in and out of the cylinders is controlled by valve means 31 through supply line 29. The pressure sensitive control 52, shown in dashed lines as an option attached to valve means 31, may be used to actuate the valve means 31 controlling the flow of fluid to position the movable weight and regulate the generated centrifugal force.
The pressure source 32 is one of various types common in the art that supplies pressurized fluid as required to force the weight to a less eccentric position.
One of the objectives of the mechanism shown in this embodiment is to provide an elongated mechanism to vibrate a body that has an elongated distance between means to mount bearings in support of the mechanism. Another objective is to divide the resistance to the generated force between two cylinders. In this way the maximum pressure in the cylinders can be halved and the beam loading of the shaft body is such to reduce the maximum bending moment, stresses and deflection of the shaft body. It is understood that more than two cylinders could be used in this embodiment to increase the generated force rating and/or to reduce the fluid pressure requirement.
The mechanism is drivenly rotated through drive means 13. Drive means 13 is shown as an external spline. Drive means such as internal splines, shaft and key or other conventional structure may be used.
FIG. 10 depicts another embodiment of the invention. Mechanism 80 shows a cylinder with attaching parts as the movable eccentric weight. The cylinder is made of barrel 81, cap 24, packing gland 64, packing 65, cap 21 and breather 22. The cylinder is shown in the zero eccentricity mode. The mechanism is essentially balanced with the cylinder in this position. The center of gravity of the cylinder however is slightly off center in the direction of the piston and when the mechanism is rotated it tends to move outwardly in said direction. The broken lines show the cap and breather end when the center of gravity of the cylinder is in a more off center location.
Piston rod 82 is shown fixed to the integral cap of cylinder means 11. It is understood that the cap could be a separate part fastened to the open ended cylinder. The cylinder means 11 is shown as an integral part of shaft body 12. It is understood further that this cylinder means could be a separate part fastened to the shaft body as discussed previously herein. The rod 82 is shown threadly fastened to piston 61. The rod, piston and seals have a fixed position. When the flow of the fluid 17 is allowed out of the cylinder body by valve means 31 through the piston rod fluid passage 83, conduit 25, bearing journal passage 26, connecting part 51, rotary coupling 50 and supply line 29 the cylinder which is the movable weight described earlier moves outwardly slidingly guided by the packing 65 on the piston rod 82, the seals 18 and 19 on the interior of the cylinder barrel 81 and the liner 84 on the outside of the cylinder barrel. The liner 84 is a tight fit in the cylinder means 11 and a loose fit about the outside of the barrel. Other means of construction could be used. The outside of the cylinder barrel 81 or the inside of the cylinder means 11, or both could be treated with an anti-friction coating instead of using liner 84. The choice of liner or protective coating is left to the designer in evaluating the individual application.
In order to decrease the centrifugal force for any given vibrational speed fluid from the pressure source is directed through the valve means 31, supply line 29, rotary coupling 50, connecting part 51, bearing journal passage 26, conduit 25, piston rod passage 83 into the cylinder which is the movable weight. The weight and location of the fluid is considered in calculating balance and centrifugal force. The fluid pressure against the cap 24, packing gland 64, packing 65 moves the weight inward towards the zero eccentricity mode in a regulated manner.
The pressure recorded by gauge means 30 is related directly to the centrifugal force being generated as the mechanism is rotated by the formula, Force = Pressure × Area. The Area in this instance is the surface of cap 24, packing gland 64, and packing 65 in contact with fluid 17.
The mechanism is drivenly rotated through drive means 13. Drive means 13 is shown as an external spline. Drive means such as internal splines, shaft and key or other conventional structure may be used.
The pressure sensitive control 52, shown in dashed lines as an option attached to valve means 31 may be used to actuate the valve means 31 controlling the flow of fluid to position the movable weight and regulate the generated centrifugal force. The valve can be set up without the pressure sensitive control to be operated manually or remotely through cable, electrical or fluid control means depending upon the various application circumstances.
The pressure source 32 is one of various types common in the art that supplies pressurized fluid as required to force the weight to a less eccentric position.
FIGS. 11, 12 and 13 show another embodiment. The mechanism has pressure source, control means, pressure gauge and circuit as described previously in the foregoing embodiment descriptions. The bearing journal passage and conduit to the piston side of the cylinder are not shown. The breather in the piston rod end of the cylinder is understood but not shown.
In the mechanism 90 dual pivoting weights 85 are pivotally connected by pins 86 to shaft body 12. The pivot pins are located generally perpendicular to the axis of rotation. The weights are clevis shaped and pin connected by pins 92 to push-pull rods 87. These push-pull rods being connected at a common joint with the boss of the extended piston rod 62. The three pieces are commonly connected by pin 89. The weights pivot as the piston rod moves in and out.
Broken lines show the outline of one of the weights, some of the linkage and piston rod in the zero eccentricity mode wherein the mechanism is essentially balanced.
The cylinder 11 is fixedly mounted to the shaft body 12 by means of flange 88. The cylinder piston rod extends and retracts radially, generally perpendicular to the axis of rotation.
It will be recognized by those skilled in the art that the cylinder shown or other types of cylinders could be mounted in a variety of attitudes using different mounting techniques without departing from the spirit of the invention.
The weights, rods, pins, piston rod, seals, (not shown) piston, (not shown) make up the compound eccentric weight. When these parts are situated in the zero eccentricity mode indicated by the broken lines as noted they tend to move to an eccentric position shown clearly in FIG. 11. Their position and the generated centrifugal force is regulated as previously discussed.
It is noted that all of the centrifugal force generated as the mechanism is rotated is not transmitted through fluid pressure in the cylinder to the shaft body. The majority of the force is transmitted to the shaft body through weight-shaft pivot pins 86. It is one of the objectives of this embodiment to provide a mechanism with large capacity with a relative low fluid pressure. As in the other embodiments; the weight, shape and geometry of the movable parts is known. The pressure in the cylinder can be directly related to the total centrifugal force. Centrifugal force calculations are made for multiple positions of the compound eccentric weight. Interpolation is used to know the force values for the infinite number of positions available.
Control means 52, an optional device, is shown in dashed lines, as a part of and adapted to valve means 31. This control means is pressure sensitive to the pressure in the cylinder through the connecting circuit. The control operates the valve means to allow flow in or out of the cylinder. This flow maintains or limits the pressure in the circuit by positioning the movable weight. The control is readily adjustable either manually or by remote control means.
The pressure source 32 is one of various types common in the art that supplies pressurized fluid as required to force the weight to a less eccentric position.
FIG. 14, 15 and 16 show another embodiment. The mechanism has a pressure source, control means, pressure gauge and circuit as described previously in the foregoing embodiment descriptions. The bearing journal passage and conduit to the piston rod side of the cylinder are not shown. The breather in the piston end of the cylinder is understood but not shown.
The mechanism is drivenly rotated through drive means 13. Drive means 13 is shown as an external spline. Drive means such as internal splines, shaft and key or other conventional structure may be used.
In the mechanism 100 the pivoting weight 93 is pin connected to hinges 94 of the shaft body 12 by pins 95. Pins 95 are located generally parallel to the axis of rotation. The weight 93 is shown in all three figures in its zero eccentricity mode wherein the mechanism is essentially balanced.
The cylinder 11 is shown pivotly mounted to the shaft body hinge brackets 96 by pin 97. The cylinder piston rod 62 is pivotly connected to weight hinge brackets 98 by pin 99. As the flow of fluid to and from the piston rod side of the cylinder moves the piston rod in and out it controls the position of the weight 93. The breather for the cylinder is not shown. Broken lines outline an eccentric position of the pivoted weight in FIGS. 15 and 16.
The weight 93, pin 99, rod 62, piston (not shown) and seals (not shown) make up the compound eccentric weight. When these parts are situated in the zero eccentricity mode shown in FIGS. 15 and 16 and the mechanism is balanced they tend to move to an eccentric position typified by the broken line outline of the weight in FIGS. 15 and 16. The cylinder and rod pivot as the rod moves in and out describing a plane perpendicular to the axis of rotation. The position of the weights and the generated centrifugal force is regulated as previously discussed.
It is noted that in this embodiment as in mechanism 90, that all of the centrifugal force generated is not transmitted through the fluid pressure to the shaft body and bearing journals. The hinges 94 transmit some force directly to the shaft body and thus to the bearing journals. As before with all things being known the pressure in the cylinder can be directly related to the total centrifugal force generated at any eccentric weight position and any vibratory speed.
Control means 52, an optional device, is shown in dashed lines, as a part of and adapted to valve means 31. This control means is pressure sensitive to the pressure in the cylinder through the connecting circuit. The control operates the valve means to allow flow in or out of the cylinder. This flow maintains or limits the pressure in the circuit by positioning the movable weight. The control is readily adjustable either manually or by remote control means.
The pressure source 32 is one of various types common in the art that supplies pressurized fluid as required to force the weight to a less eccentric position.
The foregoing embodiments describe novel variable eccentric vibration generating mechanisms. An important advantage of the mechanisms is the ability to increase or decrease force without changing the vibrational speed. Vibration can be eliminated without stopping the shaft or changing the rotational speed. Other devices that can vary the force without changing the speed are available but they use liquids for the movable weight. The liquids are forced from one chamber to another by pneumatic and hydraulic means. The chambers and their arrangement are especially bulky. Specific reference is made to U.S. Pat. No. 3,616,730, Nov. 2, 1971, by Boone, Fridley, and Bush (U.S. Cl. 94-50V).
The variable eccentric mechanisms (VEMECH) can be built in a more compact package and at less cost. The size of the package is important because it adds to the versatility of the invention. It makes the invention adaptable in relatively restricted spaces. It is also available in elongated forms as required. In addition the more compact units have less inertia or flywheel effect and require less torque to start and stop and less horsepower to accelerate. The optional pressure sensitive control means is extremely valuable in selected applications. The most important feature of the invention is the ability to record the pressure caused by the rotating eccentric weight and relate this to the centrifugal force being generated. The knowledge of the value of centrifugal force will help in vibrational amplitude regulation and matching vibrational effort to the assigned work. The most productive force value can be repeated accurately without guess work or unnecessary delay. This visible record of the generated centrifugal force through conversion of the pressure recording is not available on any other device known to the inventor. Another advantage is the variety of pressure sources listed previously as hydraulic pumps, air compressors, hydraulic cylinder and grease gun that may be used as the application circumstance dictates. Other advantages of this invention will be obvious to those skilled in the art.
Preferred embodiments of the invention have been illustrated in the accompanying Drawings and described in the foregoing Detailed Description and Summary. It will be understood that the invention is not limited to the embodiments shown and described.
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A rotatable vibration generating mechanism includes a movable eccentric weight. Said weight is variably positioned to change the eccentricity of the mechanism by the controlled flow of fluid (liquid or air) when the mechanism is stationary or rotating. More than one weight may be used and a combination of movable parts may be used as a compound movable weight. The fluid pressure resisting the movement of the weight is recorded and thus the centrifugal force generated is known through calculation, since the weight, shape, geometric configuration, and positioning of the eccentric weight is known. The centrifugal force can be changed without changing the rotating speed through the use of valve means regulating fluid flow to change the position of the eccentric weight. Pressure sensitive controls may be adapted to the valve means to make the flow control automatic so that the centrifugal force can be held constant or limited through a specified vibrational speed range. A choice of a variety of fluid pressure source means may be used to force the movement of the weight.
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FIELD OF INVENTION
[0001] The present invention involves a containment system which is employed in the removal and investigation of hazardous substances from the ground. More specifically, the present invention involves a transportable field containment system that includes a transparent hood that more efficiently and effectively facilitates the removal and investigation of hazardous substances from the ground.
BACKGROUND
[0002] It seems that hazardous waste sites are frequently discovered in and around military bases and manufacturing facilities, particularly those that existed before the public became environmentally aware of the toxicity of the various substances that were being handled at these locations. Before the Government began regulating these hazardous substances, it was common place to bury these substances underground or store them in containers underground. Over the years, these substances have leached into and contaminated the surrounding soil, exposing the public to these harmful substances. The safe, efficient and effective removal and investigation of these hazardous substances are important environmental and public safety issues. For ease of discussion, the removal, or excavation, and investigation, or sampling, of these substances are individually and collectively referred to herein as “the work.”
[0003] The current practice, when dealing with these circumstances, is to evacuate a large area around the contaminated site to avoid even greater public exposure to the hazardous compounds or, in some cases, large tent-like structures are erected over and around the contaminated site. These large tent-like structures are often referred to as tension fabric structures. Setting them up and breaking down tensioned fabric structures can be very time consuming and, in some cases, it can take weeks. In addition, they are expensive to purchase, rent and transport.
[0004] These tent-like structures are designed to prevent the public from being exposed to hazardous substances. However, they are not designed to protect the remediation technicians that must enter the tent-like structures in order to conduct the work. Accordingly, the remediation technicians must then wear a personal protective ensemble (PPE) that is specially chosen for each application. While the PPE will protect the technician, it is typically cumbersome and uncomfortable, making it difficult for the technician to perform the work.
[0005] Finally, these tent-like structures, due in part to their relatively large size, require a great deal of power to operate the equipment necessary to maintain the blower-filtration system used in conjunction with these tent-like structures. Providing the power necessary to operate this equipment can be costly.
[0006] The alternative to these large tent-like structures is to evacuate an even larger area around the work site and employ no containment system. Clearly, neither of these solutions is optimal. Accordingly, there is a need for a smaller, more economic structure that is portable, minimizes or eliminates the need to evacuate the zone around the work site, and better protects the technicians that are charged with conducting the work while allowing them to be even more comfortable and productive in conducting the work.
SUMMARY OF INVENTION
[0007] The present invention is directed to a transportable field containment system with transparent hood. An exhaust component or sub-system creates negative pressure in the containment area under the hood, thereby drawing air, that may contain hazardous substances, from the containment area away from the remediation technician and through off-gas filters. Unlike the prior art solutions described above, the transportable field containment system with transparent hood, according to the present invention, provides containment and exhaust treatment over a relatively small work site, protects the remediation technician, can be set up and broken down in less than an hour, and is man-portable.
[0008] In general, the present invention provides engineering control for the protection of workers and the general public. The engineering control provides this protection by detecting, containing and filtering hazardous analytes that might be released while the work is being conducted. Engineering control provides a higher level of compliance with OSHA regulations than other forms of control, such as work practice control, which might involve the use of exclusion zones (evacuation areas) and contamination reduction zones, or the use of PPE. In accordance with exemplary embodiments of the present invention, negative air pressure is maintained in a containment area under the transparent hood. This, in turn, ensures that any directional air movement is from the clean air environment outside the hood, into the containment area, and not the reverse. The exhaust from the hood is directed to a filter-blower system, for example, a carbon filter-blower system, which treats the contaminated air. In this regard, the hood provides protection for the remediation technician because he or she is able to perform the excavation from outside the hazardous containment area, without having to wear a cumbersome hazmat suit.
[0009] One advantage of the transportable field containment system with transparent hood, according to exemplary embodiments of the present invention, is that it is relatively small and man-transportable.
[0010] Another advantage of the transportable field containment system with transparent hood, according to exemplary embodiments of the present invention, is that it minimizes the evacuation zone around the work site.
[0011] Still another advantage of the transportable field containment system with transparent hood, according to exemplary embodiments of the present invention, is that it requires much less power than current systems, due its relatively small size.
[0012] Yet another advantage of the transportable field containment system with transparent hood, according to exemplary embodiments of the present invention, is that it is relatively less costly to operate due, in part, to the aforementioned reduced power requirements, and due to the fact that it is easily transportable and, therefore, repeatedly reusable.
[0013] Another advantage of the transportable field containment system with transparent hood, according to exemplary embodiments of the present invention, is that it provides greater protection for the remediation technician who works outside the containment area in a clean environment.
[0014] Another advantage of the transportable field containment system with transparent hood, according to exemplary embodiments of the present invention, is that it allows the remediation technician to work without wearing a cumbersome hazmat suit. This increases worker productivity, decreases labor cost, and eliminates safety hazards associated with the suit such as limited visibility and heat exposure.
[0015] In accordance with one aspect of the present invention, the aforementioned and other advantages are achieved by a transportable field containment system. The system comprises an exhaust component and a transparent hood. The transparent hood is capable of covering a containment area over a work site on the ground. The transparent hood comprises a front panel having an opening there through and one or more door panels capable of closing the opening.
[0016] In accordance with another aspect of the present invention, the aforementioned and other advantages are achieved by a transparent hood for use in a transportable field containment system. The hood covers a containment area over a work site on the ground and it comprises a front panel having a containment area access opening there through; a plurality of side panels attached to the front panel; and one or more door panels capable of closing the opening.
BRIEF DESCRIPTION OF DRAWINGS
[0017] The present invention will be understood, in part, from the following figures, in which:
[0018] FIG. 1 . illustrates an overview of a transportable field containment system with transparent hood, in accordance with a preferred embodiment of the present invention;
[0019] FIG. 2 illustrates the transparent hood in greater detail, in accordance with the preferred embodiment of the present invention; and
[0020] FIG. 3 illustrates a number of monitoring devices that may be employed in the transportable field containment system.
DETAILED DESCRIPTION OF INVENTION
[0021] The present invention will now be described in terms of a preferred embodiment. However, it will be understood that the embodiment, though preferred, is exemplary. Those of ordinary skill in the art will understand that certain modifications to the preferred embodiment are possible without departing from the spirit of the invention. Such modifications are, therefore, considered within the scope of the present invention.
[0022] FIG. 1 illustrates the main components of a transportable field containment system 10 with transparent hood, in accordance with the preferred embodiment of the present invention. As shown, the system comprises, among other things, a transparent hood 15 , an exhaust plenum 20 , exhaust hose 25 , off-gas filters 30 , exhaust blowers 35 and sealing skirt 40 . In addition, there are one or more monitoring devices 45 that are better illustrated in FIG. 3 , which is described in more detail below.
[0023] FIG. 2 shows, in greater detail, the transparent hood 15 . In general, the hood 15 covers and, therefore, isolates the containment area under the hood from the clean environment outside the hood. The hood 15 is physically separable from the other system components. This contributes to the transportability of the system as a whole.
[0024] In the preferred embodiment, the hood 15 is made of a non-ferrous, non-magnetic, heavy duty, yet lightweight plastic, such as clear polycarbonate. This permits the remediation technician and/or others to view the containment area under the hood 15 from many different angles, yet remain outside the containment area, protected from any hazardous substances while performing the work.
[0025] Further, in accordance with the preferred embodiment, the hood 15 comprises a plurality of sliding door panels 100 . In this embodiment, there are six sliding door panels 100 ( a )- 100 ( f ), three sliding door panels 100 ( a )- 100 ( c ) on the left and three sliding door panels 100 ( d )- 100 ( f ) on the right. It will be appreciated, however, that more than six or fewer than six door panels are possible.
[0026] While installed, the door panels 100 rest in tracks 115 . The tracks 115 permit the remediation technician to slide each of the door panels 100 horizontally and independently. Because the technician can independently slide each of the door panels 100 , there are infinite degrees of freedom with respect to the horizontal positioning of the door panels, relative to each other. Therefore, the size of the opening in the hood, through which the technician has access to the containment area, is adjustable. It will be further noted that more than one opening through the hood and other configurations for mounting and adjusting the position of the door panels are possible.
[0027] In accordance with the preferred embodiment, the door panels 100 are also removable. That is, the technician can slide each of the door panels 100 horizontally until they are free of the tracks 115 and completely detached from the hood 15 . The ability to remove and then stack the door panels 100 allows the hood 15 to be disassembled easily and quickly, and this, in turn, further facilitates transportability.
[0028] Still further in accordance with the preferred embodiment, the hood 15 comprises a front panel 120 and side panels 125 and 130 . In addition, the side panels 125 and 130 are rotatably attached to the front panel 120 by hinged edge brackets 135 . These hinged edge brackets permit the technician to fold the side panels 125 and 130 relative to the front panel 120 so that the hood is collapsible and essentially flat when disassembled, even further facilitating transportability of the hood and the system as a whole. Alternatively, the side panels 125 and 130 may be detachable from the front panel 120 . The ability to detach the side panels 125 and 130 from the front panel 120 would also facilitate transportability.
[0029] FIG. 2 also shows, in greater detail, the exhaust plenum 20 . The exhaust plenum 20 is a transition component positioned adjacent to the hood 15 . The exhaust plenum 20 serves as an outlet through which air is drawn from the containment area under the hood 15 and directed towards the exhaust hose 25 . In the preferred embodiment, the plenum 20 and the hood 15 are configured in such a way that there is no leakage of air there between when the two components are assembled and the system is functioning. For example, the outer portion or periphery of the side surface of plenum 20 facing the transparent hood 15 may include a groove having a size and/or shape designed to accommodate the rear edge of the transparent hood, thus providing a seal between transparent hood 15 and the plenum 20 to prevent the leakage of air.
[0030] The plenum 20 is further configured to house one or more filters 140 . In the preferred embodiment, the filters 140 are made of fabric. The filters 140 remove dust and other relatively large particles from the air before the air enters the off-gas filters 30 . When dirty or damaged, the technician can remove the filters 140 from the plenum 20 and either clean or replace the filters 140 .
[0031] The plenum 20 also includes one or more ports. In the preferred embodiment, one or more x-grommet port 145 are located on the top side of the plenum 20 . The port 145 serves as an insertion point for air monitoring sensors and/or other instruments necessary for monitoring the conditions in the containment area. More will be said about the air monitoring sensors below.
[0032] Referring back to FIG. 1 , the transportable field containment system 10 comprises exhaust and filtration components, including an exhaust hose 25 , off-gas filters 30 , and exhaust blowers 35 . In the preferred embodiment illustrated in FIG. 1 , there are two off-gas filters 30 and two exhaust blowers 35 . One skilled in the art, however, will realize that more or less than two off-gas filters 30 and more or less than two exhaust blowers 35 are possible.
[0033] Each of the two exhaust blowers 35 comprises, for example, an electric motor and a fan. In FIG. 1 , each of the two exhaust blowers 35 are located on a respective one of the off-gas filters 30 . When the exhaust blowers 35 are operating, they create negative air pressure in the containment area under the hood 15 , thereby drawing air from the containment area under the hood 15 , through the fabric filters 140 in the plenum 20 , through the exhaust hose 25 and into and through the two off-gas filters 30 . The negative air pressure actually causes air movement from the outside, clean environment into the containment area under the hood 15 . The movement of air into the containment area from the outside, clean environment is illustrated in FIG. 1 by the dashed arrows. Maintaining the movement of air in this direction is important because it not only facilitates the removal of dirt and dust particles from the air, and the removal of hazardous substances from the air, it also protects the technician by continuously moving these hazardous substances in a direction away from the technician.
[0034] In an alternative embodiment, the power and/or speed of the exhaust blowers 35 is variable. In other words, the exhaust blowers 35 are adjustable. For example, if the technician increases the size of the opening through the front panel 120 by sliding open one or more of the door panels 100 , and the exhaust blowers 35 are not adjustable, the air pressure in the containment area may drop. However, if the exhaust blowers 35 are adjustable, the exhaust blowers 35 may work harder or faster in response to the drop in negative air pressure, thereby maintaining the desired level of negative air pressure and minimizing the risk of any hazardous substances escaping from the containment area and jeopardizing the safety of the technician. In one embodiment, the exhaust blowers 35 may be manually adjustable. In another embodiment, the exhaust blowers 35 may be automatically variable based on a feedback signal from the air pressure monitor described below.
[0035] In the preferred embodiment, the off-gas filters 30 take the form of canisters, each of which contain carbon. As the air passes through the carbon, the carbon treats the exhaust by removing any hazardous substances in the exhaust. Although it is not shown in FIG. 1 , each of the off-gas carbon filters 30 may have wheels or casters to further facilitate the transportability of the system as a whole.
[0036] One reason there are two off-gas filters 30 and two exhaust blowers 35 in the preferred embodiment is that having more than one off-gas filter 30 and one exhaust blower 35 insures at least single-fault tolerance. In other words, if one blower fails while the work is being conducted, there is some redundancy in that at least one exhaust blower remains operational to maintain the air flow in the aforementioned direction, from the outside, clean environment to the containment area, away from the technician, thereby minimizing the risk of exposing the remediation technician to hazardous substances in the air within the containment area.
[0037] In accordance with the preferred embodiment of the present invention, the transportable field containment system 10 with transparent hood further includes a sealing skirt 40 , as illustrated in FIG. 1 . The primary purpose of the sealing skirt 40 is to prevent air from leaking through any space between the ground and the underside of the transparent hood 15 , due in part to any unevenness of the ground, which might otherwise adversely affect the negative air pressure in the containment area.
[0038] Preferably, the shape of the sealing skirt 40 is adaptable so that it compliments the contour of the ground below the hood 15 and around the plenum 20 . The sealing skirt 40 can then fill all of the open space that might otherwise exist between the ground and the hood 15 . In the exemplary embodiment of FIG. 1 , the sealing skirt 40 comprises one or more sandbags; however, one skilled in the art will appreciate the fact that the sealing skirt 40 may involve something other than sandbags.
[0039] FIG. 3 illustrates an exemplary number of monitors 45 . The monitors 45 are primarily used to detect the presence of one or more hazardous analytes and activate an alarm if any of these analytes are in fact detected. The monitors include a first monitor 45 - 1 for monitoring the conditions in the containment area under hood 15 and activating an alarm if one or more hazardous analytes are detected. A second monitor 45 - 2 is employed for monitoring the work zone immediately outside the containment area. The primary purpose of monitor 45 - 2 is to protect the technician performing the work by activating an alarm if certain hazardous analytes are detected outside the containment area in the work space around the technician. A third monitor 45 - 3 is used for monitoring the exhaust, that is, monitoring the exhaust gas after it passes through the off-gas filters 30 to verify the effectiveness of the off-gas filters 30 for removing the target analytes. A fourth monitor 45 - 4 is for monitoring an area downwind of the work zone, while a fifth monitor 45 - 5 is for monitoring an area upwind of the work zone. The purpose of monitors 45 - 4 and 45 - 5 is to protect the general population in close proximity to the work zone by activating an alarm if any analyte migrates outside the work zone. There are known instruments that may be used for the monitors 45 - 1 through 45 - 5 . Although the embodiment illustrated in FIG. 3 shows five monitors, one skilled in the art will understand that more or fewer monitors may be employed.
[0040] FIG. 3 also shows that, in accordance with the preferred embodiment of the present invention, the transportable field containment system 10 with transparent hood further comprises a pressure gauge 50 . There are also known instruments for implementing the pressure gauge 50 . In one exemplary embodiment, the pressure gauge 50 is connected to a pressure transducer located in the containment area under the transparent hood 15 . The purpose of pressure gauge 50 is allow the technician to continuously monitor the air pressure in the containment area under the hood 15 , to insure that the exhaust fans 35 are maintaining the negative air pressure. The pressure gauge 50 may activate an alarm if it determines that the air pressure drops below a predetermined threshold. As explained above, maintaining negative air pressure in the containment area provides protection by isolating the technician from any hazardous substances in the air within the containment area.
[0041] The present invention has been described in accordance with a preferred embodiment, including certain alternatives thereto. One skilled in the art will understand that other modifications and embodiments consistent with the scope and spirit of the present invention are possible.
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A transportable field containment system with transparent hood. The transportable field containment system being easily and rapidly deployable and transportable by virtue of its relatively small size and light weight, a collapsible transparent hood that covers the containment area over a work site on the ground, the hood including detachable or folding side panels and removable door panels. The system preferably includes an exhaust component that creates negative air pressure in the containment area under the hood, thereby drawing air that contains hazardous substances, that may be released while the work is being conducted, through one or more off-gas filters.
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RELATED APPLICATIONS
This application is a divisional of U.S. application Ser. No. 09/542,631 filed Apr. 4, 2000 and entitled “Apparatus and Method for Forming a Composite Structure,” that issued as U.S. Pat. No. 6,692,817 on Feb. 17, 2004.
This application is related to U.S. application Ser. No. 09/248,172 filed Feb. 9, 1999 and entitled “Acid Impervious Coated Metal Substrate Surface and Method of Production,” that issued as U.S. Pat. No. 6,124,000 on Sep. 26, 2000.
TECHNICAL FIELD OF THE INVENTION
This invention relates generally to the field of materials construction and, more specifically, to an apparatus and method for forming a composite structure.
BACKGROUND OF THE INVENTION
Composite structures are desirable in many industries for many applications. The aerospace industry, for example, uses composite structures extensively because, among other desirable attributes, composites have high strength-to-weight ratios. Because of the ever increasing use of composite structures throughout industry, manufacturers are continually searching for better and more economical ways of forming composite structures.
In the forming of composite structures many manufacturing steps are performed. One such step that is usually required is an elevated-temperature curing step. A composite structure is placed on a tool, which is normally the tool that was used to shape the composite structure, and then placed in an oven for a period of time. After the curing cycle the composite structure is removed from the tool. Most composite materials have a tendency to adhere to the tool, which may cause harm to the shape or surface of the composite structure when being removed. This is the reason release agents were developed. Before placing a composite structure on a tool, a release agent is applied to the tool surface to allow the composite structure to be easily removed from the tool after curing. This release agent needs to be reapplied to the tool before every curing cycle, which takes time. In addition, typical release agents are organic solvent-based, which emit pollution. Furthermore, some of the release agent transfers to the composite structure, which results in a time-consuming sanding step of the surface of the composite structure before painting.
The challenges in the field of forming composite materials continue to increase with demands for more and better techniques having greater flexibility and adaptability. Therefore, a need has arisen for a new apparatus and method for forming a composite structure.
SUMMARY OF THE INVENTION
In accordance with the present invention, an apparatus and method for forming a composite structure is provided that substantially eliminates or reduces disadvantages and problems associated with previously developed apparatuses and methods.
An apparatus for forming a composite structure is disclosed. The apparatus comprises a tool having a surface that is substantially covered by a primer and a coating. More specifically, the primer may be a powdered primer, and the coating may be a powdered fluorinated organic compound.
A method for forming a composite structure is disclosed. The method comprises four steps. Step one calls for applying a primer to a surface of a tool. Step two requires applying a coating to the primer. Step three calls for curing the primer and coating that are applied to the tool. The last step calls for forming the composite structure on the tool.
In accordance with another aspect of the present invention, a method for forming a composite structure is disclosed. The method comprises six steps. Step one calls for cleaning a surface of a tool with an environmentally friendly solvent. Step two requires covering a peripheral portion of the surface with, for example, masking tape. The third step calls for applying a powdered primer to the uncovered portion of the surface. Step four calls for applying a powdered coating to the primer. Step five requires the curing of the primer and coating that are applied to the tool. The last step allows for forming the composite structure on the tool.
A technical advantage of the present invention is the elimination of having to apply a release agent each time a composite structure is cured. The powdered primer and powdered coating will result in a more durable tool that can be used for numerous curing cycles. This will save time and money.
Another technical advantage of the present invention is that emissions from traditional release agents will be eliminated. The powdered primer and powdered coating are environmentally friendly, and will allow a manufacturer to meet tightening environmental regulations. This will also eliminate any permit and compliance issues associated with the current use of release agents.
An additional technical advantage of the present invention is that the number of times a composite structure has to be sanded before being painted will be substantially reduced. This will save time and money.
Other technical advantages are readily apparent to one skilled in the art from the following figures, descriptions, and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the invention, and for further features and advantages, reference is now made to the following description, taken in conjunction with the accompanying drawings, in which:
FIG. 1A is an elevation view of a tool useful in the practice of the present invention;
FIG. 1B is a fragmented view of a metallic tool useful in the practice of the present invention showing, in greater detail, the primer, coating, and surface of the metallic tool;
FIG. 1C is a fragmented view of a composite tool useful in the practice of the present invention showing, in greater detail, the primer, coating, and surface of the composite tool; and
FIG. 2 is a flowchart demonstrating one method of forming a composite structure in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The preferred embodiments of the present invention and its advantages are drawings, in which like numerals refer to like parts.
FIG. 1A is an elevation view of a tool 100 useful in the practice of one embodiment of the present invention. Tool 100 has a surface 102 in which there is a primer 104 and a coating 106 applied thereto. Tool 100 , along with the applied primer 104 and coating 106 , is used for the forming of composite structures. Solely for convenience, tool 100 is shown in FIG. 1A to be separated into two halves, each half being constructed of a different material. As illustrated by FIG. 1A , Tool 100 may be constructed of a metallic material, or tool 100 may be constructed of a composite material. Other types of materials are also contemplated by the present invention. Furthermore, the shape of tool 100 as shown in FIG. 1A is only one of many shapes that are possible. Depending on the final composite structure desired, tool 100 can be any shape imaginable.
Surface 102 is the “working surface” of tool 100 . In other words, surface 102 is where the composite structure will be formed and, hence, where primer 104 and coating 106 will be applied. Surface 102 is normally prepared before the application of primer 104 and coating 106 by cleaning with an environmentally-friendly solvent, such as isopropyl alcohol. This solvent is then allowed to dry before the application of primer 104 and coating 106 . It may be, however, unnecessary to clean surface 102 depending on its initial condition. On the other hand, before cleaning surface 102 with a solvent, surface 102 may be abraded with, for example, a Scotchbrite and a jitter bug sander. In the case of tool 100 being constructed of a composite material, there may be an additional preparation step after cleaning the surface with a solvent. This would be a step of applying a surfactant solution, which may be any of a myriad of commercially-available soaps. This surfactant solution is also allowed to dry on surface 102 before application of primer 104 and coating 106 .
In another embodiment of the present invention, the preparation of surface 102 may also include a covering of the periphery of surface 102 with a tape 108 . Tape 108 may be a masking tape or any other tape that is adequate to protect the periphery of surface 102 when applying primer 104 and coating 106 . This covering of the periphery of surface 102 is for any subsequent sealant that would be used for vacuum bag forming of a composite structure.
FIG. 1B is a fragmented view of one embodiment of the present invention showing tool 100 constructed of metallic material. In this embodiment, primer 104 is a fluorinated powdered primer used for fluorinated compounds, and is used to obtain a good bond between coating 106 and tool 100 . As examples, primer 104 may be tetrafluoroethylene or an ethylene polymer blended with epoxy. Other fluorinated hydrocarbons are contemplated by the present invention for use as primer 104 . The thickness of primer 104 will generally be 2–3 mils. However, depending on the type of material used, and the method of application, other thicknesses are contemplated. Primer 104 is typically sprayed onto surface 102 of tool 100 by an electrostatic powder spray gun 110 as illustrated in FIG. 1A . Electrostatic powder spray guns are well known in the art of material coatings. Other methods of applying primer 104 to surface 102 of tool 100 are contemplated by the present invention.
FIG. 1C is a fragmented view of another embodiment of the present invention showing tool 100 constructed of composite material. In this embodiment, primer 104 is a nylon-powdered primer. Nylon is used because it has release properties of its own. Other types of primer 104 are contemplated by the present invention. Once again, primer 104 is typically sprayed onto surface 102 of tool 100 by an electrostatic powder spray gun 110 . However, other methods of applying primer 104 are contemplated.
Referring to either FIG. 1B or FIG. 1C , coating 106 is shown. Coating 106 is used as the release agent when constructing a composite structure with tool 100 . Coating 106 is a fluorinated hydrocarbon in powdered form, and is commercially available. Examples of coating 106 are Dyher 820 by Whifford Inc., Teflon manufactured by DuPont and distributed by Intech, and Halar by Ausimont USA, Inc. Other types of fluorinated powdered hydrocarbons are also contemplated by the present invention. The thickness of coating 106 will generally be 2–3 mils. However, depending on the type of material used, and the method of application, other thicknesses are contemplated. A conventional corona electrostatic coating process, using electrostatic powder spray gun 110 , may be used to apply coating 106 to primer 104 . Coating 106 will chemically or mechanically bond to primer 104 after application. Using powdered fluorinated hydrocarbons for coating 106 eliminates emission problems typical of the traditional release agents, such as Frecote 44NC, used in constructing composite structures. This will allow manufacturers to meet tightening environmental regulations, and will eliminate any permit and compliance issues associated with the use of traditional release agents.
After the application of both primer 104 and coating 106 to surface 102 of tool 100 , a curing cycle is typically performed. Tool 100 is coupled to a heat source, such as an oven, for a certain period of time depending on the type of coating 106 used. The temperature used in the curing process varies depending on the type of material used for tool 100 , but will generally be greater than approximately 450° F. Solely as an example, if Halar is used as a coating for tool 100 made of steel, tool 100 would be cured at approximately 535° F. for approximately twenty minutes. After the curing cycle, tool 100 is allowed to cool down to ambient temperature. Tool 100 is then ready for forming composite structures.
In an embodiment where tool 100 is made of composite material, as shown in FIG. 1C , the nylon-powdered primer will melt during the curing cycle, and the nylon will flow around the fluoropolymer particles contained in coating 106 and mechanically lock them into place. A durable coating 106 will result. No matter what type of material tool 100 is constructed of, a smooth, tack-resistant surface of coating 106 also results. This means that when forming a composite structure using tool 100 , many cycles of use can be accomplished before having to inspect surface 102 of tool 100 for recoating. This eliminates the traditional step of having to apply a release agent each time a composite structure is cured, which will save time and money. In addition, more time and money will be saved by the use of primer 104 and coating 106 because of the elimination of a sanding step that is typical with the use of traditional release agents. Using traditional release agents results in a transfer of some of the release agent into the composite tool being formed, which means the composite structure has to be sanded before being painted. With the present invention, there is no transfer of primer 104 and/or coating 106 to composite structures during the curing cycle.
FIG. 2 is a flowchart demonstrating one method of forming a composite structure in accordance with the present invention. In one embodiment, surface 102 of tool 100 is cleaned with an environmentally compliant solvent at step 200 . If tool 100 is constructed of composite material, then a surfactant solution is also applied to surface 102 and allowed to dry at step 220 . In any case, the next step is to cover a peripheral portion of surface 102 with tape 108 at step 202 . Then powdered primer 104 can be applied to the uncovered portion of surface 102 at step 204 . In the case of tool 100 being made of composite material, powder primer 104 will comprise a nylon-powdered primer. After the application of powdered primer 104 , coating 106 , which comprises a powdered fluorinated organic compound, is applied to primer 104 at step 206 . Tool 100 is then cured in an oven for a period of time at step 208 and a composite structure is coupled to tool 100 and formed at step 210 .
Although an embodiment of the invention and its advantages are described in detail, a person skilled in the art could make various alternations, additions, and omissions without departing from the spirit and scope of the present invention as defined by the appended claims.
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A method for forming a composite structure is disclosed. The method includes four steps. Step one calls for applying a primer ( 104 ) to a surface ( 102 ) of a tool ( 100 ). Step two requires applying a coating ( 106 ) to primer ( 104 ). Step three calls for curing primer ( 104 ) and coating ( 106 ). The last step calls for forming the composite structure on tool ( 100 ). More specifically, primer ( 104 ) may be a powdered primer, and coating ( 106 ) may be a powdered fluorinated organic compound.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to paper machine components and in particular to paper machine dry sections having a plurality of drying cylinders and guide rolls looped about by an endless carrier belt.
2. Description of Related Technology
Dryer sections of paper machines are disclosed, for example, in Kade et al., U.S. Pat. No. 5,050,317 and Preisetanz et al., U.S. Pat. No. 5,177,880. These patents disclose dryer sections with single-row dryer groups in which a plurality of dryer cylinders are disposed in a row and a suction-deflection roll is provided between two neighboring dryer cylinders. An endless carrier or support belt, also known as a dryer wire, loops in alternating fashion around the suction-deflection rolls and the dryer cylinders. During operation, a paper web to be dried is guided by the carrier belt as the paper and the belt travel about a dryer cylinder. The paper web is sandwiched between the surface of the dryer cylinder and the carrier belt.
Normally, a dryer section contains several dryer groups so that a paper web is transferred from one dryer group to the next during its passage through the paper machine.
At an initial region of the dryer section, the paper web has a relatively high water content and thus a relatively low strength. Therefore, the paper web is always supported by the carrier belt of a particular dryer group. The dryer groups are arranged such that the paper web is fully supported at transfer regions between the dryer groups. In such a transfer region, the web comes into contact with a carrier belt of a next dryer group positioned directly downstream with respect to a direction of travel of a paper web through the paper machine, but at the same time remains in contact for a small distance with the carrier belt of the previous (i.e., upstream) dryer group. Thus, the paper web is sandwiched between the two carrier belts for a short time.
However, due to the paper web low strength mentioned above, tearing of the paper web often occurs. Also, large amounts of waste may be produced within a short time due to the high velocity of travel of the paper web through the paper machine. The waste must be removed as fast as possible so that it does not cause damage to the guide rolls, dryer cylinders or dryer screens.
In order to be able to remove paper jam as fast as possible, the transfer region between dryer groups is preferably designed so that it can be "opened" rapidly. This is achieved, for example, by moving a dryer wire of a first dryer group away from a guide roll of a neighboring dryer group via corresponding displacement of a guide roll in the transfer region, so that the waste can fall into a machine cellar. The guide roll can be a suction roll which is located during normal operation within the wire loop of the neighboring dryer group and which is disposed near a last dryer cylinder of the previous (i.e., upstream) dryer group. See, for example, FIG. 1 of U.S. Pat. No. 5,177,880 which shows a suction guide roll near a dryer cylinder 13. FIG. 2 of U.S. Pat. No. 5,050,317 shows a dryer section arrangement in which a guide roll 194 can be displaced so that a dryer wire 174 of a dryer group can be moved away from a dryer wire 175 of the next (i.e. downstream with respect to a direction of travel of a web through the dryer groups) dryer group.
Displacement of guide rolls generally results in a change of the tension of a cooperating dryer wire. To keep the tension constant, tension rolls may be provided within each dryer wire loop. The tension rolls receive signals from tension sensors which first record a change in wire tension and then give an appropriate command to the tension roll. However, as described above, a dryer wire becomes displaced during an "opening" process of a transfer region between dryer groups, as well as during a corresponding closing process of the region, which can lead to significant interruption of the operation of the dryer section and also to continual tearing of the paper web.
In dryer sections known in the art described herein, application of tension to a dryer wire, after it becomes slack, does not take place fast enough. This is due to a certain inertia of the tension roll sensor system and of the tension roll control system.
SUMMARY OF THE INVENTION
It is an object of the invention to overcome one or more of the problems described above. It is also an object of the invention to provide a component of a paper machine, especially a dryer group of a dryer section of a paper machine wherein the tension of an endless belt that loops about the dryer group always remains the same, even during the opening and closing processes of a transfer region between dryer groups, and does not change even for short time periods.
According to the invention, a paper machine dryer group has a plurality of rolls, including a guide roll and a tension roll, and a carrier belt traveling over the rolls and forming a continuous loop. The guide roll can be displaced to a location parallel to its axis and at an angle to the direction of movement of the carrier belt. The guide roll and the tension roll are coupled to each other in such a way that, when the guide roll is displaced, the tension roll is simultaneously displaced in such a direction and to such an extent that the carrier belt tension remains at least approximately constant.
Other objects and advantages of the invention will be apparent to those skilled in the art from the following detailed description taken in conjunction with the drawings and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic sectional view of a dryer section according to the invention.
FIG. 2 is a schematic sectional view of a second embodiment of a dryer section according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
According to the invention, a dryer group includes a guide roll and a tension roll coupled to each other such that when the guide roll is displaced, the tension roll is also displaced simultaneously in such a direction and to such an extent that the tension of the endless belt cooperating with the guide and tension rolls remains approximately constant. Although U.S. Pat. No. 5,050,317 describes a displaceable guide roll 192 or 194 supported on a common frame together with a tension roll 170 (column 7, lines 29-34, in connection with FIG. 2), it does not follow from this disclosure that the two rolls are coupled with each other so that simultaneous displacement of the rolls occurs.
The invention is explained in more detail in the drawings. FIG. 1 shows a portion of a dryer section of a paper machine. A paper web loops in succession about dryer components or groups generally designated A and B.
The dryer group A includes three dryer cylinders 2, 3, and 4, disposed in succession and neighboring suction guide rolls 5, 6, 7, and 8. The dryer group A also includes a series of guide rolls 30, 31, 32, 33, 34, and 35. An endless support belt or dryer wire 9 travels over the cylinders 2, 3, and 4 and the rolls 30, 31, 32, 33, 34, and 35 in a continuous loop and moves in a direction indicated by an arrow 11.
Similar to the dryer group A, the dryer group B has three dryer cylinders 12, 13, and 14, three suction guide rolls 15, 16, and 17, five guide rolls 40, 41, 42, 43, and 44, and a continuous belt or dryer wire 10 looped thereabout. The wire 10 moves around the cylinders and rolls in a direction indicated by an arrow 20.
As shown in FIG. 1, a connecting line running through the dryer cylinders of the first dryer group A forms a V with a connecting line running through the dryer cylinders of the second dryer group B.
A rocker 50 supports the suction guide roll 8, and the guide rolls 30 and 31. The rolls 8, 30 and 31 assist in maintaining the wire 9 under tension, and thus also function as tension rolls. The rocker 50 can be swiveled around an axis 51 thereof. The axis 51 is parallel to longitudinal axes of the dryer cylinders as well as to longitudinal axes of the other rolls. The position of the rocker 50 shown by a solid line in FIG. 1 is a working position of the rocker 50.
Another dryer component or group (not shown) is connected before the dryer group A, i.e., upstream of the dryer group A with respect to a direction of travel of a paper web through the paper machine, and a further dryer group (not shown) is connected downstream of the dryer group B with respect to a direction of travel of a paper web through the paper machine. However, such dryer groups are not further discussed herein. Other types of paper machine components or units can be disposed upstream and downstream of dryer groups A and B. For example, a press part may be disposed upstream of the dryer group A.
The two dryer groups A and B operate as follows: The dryer group A takes over a paper web (not shown here in detail) from an upstream paper machine unit by transfer of the web with the aid of the dryer wire 9 and the suction guide roll 5. As the paper web loops about the suction guide roll 5, the paper web is disposed outside of the dryer wire 9. Then, together with the dryer wire 9, the paper web is conveyed to the dryer cylinder 2, during the conveyance of which the web is sandwiched between a surface of the dryer cylinder 2 and the dryer wire 9. Thereafter, the paper web is further transported in succession to the suction guide roll 6, the dryer cylinder 3, the suction guide roll 7, the dryer cylinder 4, and the suction guide roll 8. In the region of the suction guide roll 8 which is a transfer region between the dryer groups A and B, the paper web is transferred from the dryer group A to the dryer group B by conveyance of the paper web from the dryer wire 9 to a surface of the dryer cylinder 12. In the transfer region between dryer groups A and B, the paper web is sandwiched for a short time between the dryer wire 9 and the surface of the dryer cylinder 12. The paper web then follows the surface of the dryer cylinder 12 and becomes sandwiched between the cylinder 12 and the dryer wire 10 of the dryer group B.
If the paper web tears, the rocker 50 is swiveled to a position shown by a dashed line in FIG. 1. During this swiveling, the portion of the dryer wire 9 which is between the suction roll 8 and the guide/tension roll 30 is moved away from the surface of the dryer cylinder 12. As a result, the path of the paper web is opened so that the paper web can fall down through an open gap into a machine cellar for recycling. The swiveling of the rocker 50 occurs about the axis 51 in a direction indicated by an arrow 60.
During the swiveling of the rocker 50 the total path of the dryer wire 9 is shortened. However, at the same time, the guide/tension roll 31 acts as a tension roll as it is swiveled in a direction indicated by an arrow 61. The swiveling movements of the rolls 8, 30, and 31 carried by the rocker 50 are necessarily coupled to one another, so that the tension of the dryer wire 9 remains the same at all times and displacement of the dryer wire 9 cannot occur.
FIG. 2 also shows two dryer groups disposed in succession. A guide roll 30' can be displaced in a direction indicated by an arrow 60' to provide an opening at a transfer region between two dryer wires 9' and 10'. A neighboring tension roll 31' is rigidly coupled to the guide roll 30' by a rod 70' so that when the guide roll 30' is displaced, the tension roll 31' is simultaneously displaced with positive locking. The slackening of the dryer wire 9' due to the displacement of the guide roll 30' is compensated for instantly by tightening of the wire 9' due to the controlled displacement of the tension roll 31'.
Modifications of embodiments according to the invention described herein are also possible. In the embodiment shown in FIG. 1, it is possible to support only the guide/tension roll 30 and the guide/tension roll 31 on the rocker 50, but not the suction guide roll 8. Furthermore, the guide/tension roll 30 and the roll 8 can be displaced together, while allowing the roll 31 to remain stationary. Also, various participating rolls, for example, the guide roll 31, can be supported rigidly or flexibly.
Finally, the invention can be applied independently of whether the transfer region is between two bottom felt groups, between a bottom and a top felt group or between a top felt group and a bottom felt group.
The foregoing detailed description is given for clearness of understanding only, and no unnecessary limitations should be understood therefrom, as modifications within the scope of the invention will be apparent to those skilled in the art.
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A paper machine dryer group has a plurality of rolls, including a guide roll and a tension roll, and a carrier belt traveling over the rolls and forming a continuous loop. The guide roll can be displaced to a location parallel to its axis as well as at an angle to the direction of movement of the carrier belt. The guide roll and the tension roll are coupled to each other in such a way that, when the guide roll is displaced, the tension roll is simultaneously displaced in such a direction and to such an extent that the carrier belt tension remains at least approximately constant.
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This application is a continuation of application Ser. No. 08/304,644 filed Sep. 12, 1994 now abandoned, which is a continuation of application Ser. No. 08/025,347 filed Mar. 2, 1993 now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a disk chucking device employed for a disk drive unit that chucks an information recording disk, drives the disk to rotate, and records or regenerates information. More particularly, this invention is concerned with a disk chucking device suitable for chucking a so-called 3.5"-diameter floppy disk.
2. Description of the Prior Art
In a disk drive unit for driving a disk-like information recording medium (hereafter, referred to as a disk), a variety of improvements and inventions have been proposed in efforts to improve recording density or to realize downsizing and weight cutting. In one of the proposals, for recording or regeneration information, a turntable is attached to a spindle, and then a disk is driven to rotate via a drive pin projecting from the disk loading surface of the turntable.
FIGS. 11 to 13 show an example of a major portion of this kind of disk drive unit known conventionally. FIG. 11 is a plan view of the major portion of the disk drive unit. FIGS. 12a and 12b are a plan view and a front view of a blade spring. FIGS. 13a, 13b, 13c, and 13d are explanatory diagrams showing the operating states of the blade spring.
In these drawings, a disk driving section of the disk drive unit consists mainly of a disk drive motor 1, a spindle 2 for the disk drive motor 1, a turntable 3 attached to the distal end of the spindle 2, and a drive pin 19 having a cylinder (roller) that is supported by a blade spring 17 attached to the bottom of the turntable 3, and inserted in a drive pin insertion hole 13 bored on the turntable 3, and whose outer circumferential portion is rotatable.
The turntable 3 has a center hole 12 in which the spindle 2 of the disk drive motor 1 is inserted, a drive pin inserting hole 13 in which the drive pin 19 is inserted, and an attachment hole 14 to which a member for fixing the blade spring 17, for example, an eyelet is fitted with pressure. An anti-friction plastic sheet is adhering to the central portion of the surface of the turntable 3. A chucking magnet 16 such as a rubber magnet is adhering to the front surface excluding the center hole 12, drive pin insertion hole 13, and plastic sheet. The blade spring 17 is a thin plate made of a material with excellent elasticity; such as, phosphor bronze, and shaped like an arc. A distal end 19a of the drive pin 19 fixed to the distal end of the blade spring 17 penetrates through the drive pin insertion hole 13 bored on the turntable 3 and projects from the top of the turntable 3.
FIG. 15 shows an example of a disk 23 having a metallic hub. The disk 23 has, as shown in FIG. 15, a magnetic recording layer on the surface thereof, and is encased in a rigid envelope 24a to form a disk cartridge 24. In the center of the disk 23, a metallic hub 25 of a metallic thin plate having magnetism is locked. A substantially square chucking hole 26, in which the distal end 2a of the spindle 2 is inserted, is bored in the center of the metallic hub 25. A substantially rectangular alignment hole 27, to which the distal end 19a of the drive pin 19 is fitted for engagement, is bored on the outer circumferential area of the metallic hub 25.
When the disk cartridge 24 is placed on the turntable 3, the chucking magnet 16 attracts the metallic hub 25. Then, the distal end 2a of the spindle 2 is inserted in the chucking hole 26. At this time, the drive pin 19 is pressed down in the opposite direction of a disk loading direction against spring force of the blade spring 17 by means of the metallic hub 25, and then pushed into the drive pin inserting hole 13 on the turntable 3. Then, as shown in FIG. 13a, the drive pin 19 is located under the metallic hub 25. Then, the turntable 3 rotates in an arrow-F direction in FIG. 13a (FIG. 13b). When the drive pin 19 agrees with the position of the alignment hole 27, as shown in FIG. 13c, the drive pin 19 is fitted in the alignment hole 27. When the turntable 3 further rotates, as shown in FIG. 13d, the drive pin 19 comes into contact with an inner margin 27a of the outer circumference of the alignment hole 27. The elastic force of the blade spring 17 causes the entire disk 23 (including the metallic hub 25) to move from the spindle 2 toward the drive pin 19 or radially outward. The spindle 2 is pushed away to that corner 26a of the chucking hole 26 located farthest from the alignment hole 27. Then, centering is carried out. Then, with the spindle 2 as a center, the metallic hub 25 and disk 23 rotate in the arrow-F direction. Consequently, recording or regeneration is achieved.
FIG. 14 includes explanatory diagrams showing structures of a drive pin 19 for a conventional disk chucking device. As shown in FIG. 14a, a normal structure is made of a metallic material or a resin. As shown in FIG. 14b, a drive pin 19 whose surface is made of a metallic material may be coated with a coating layer 19b made of a resin.
In the aforesaid prior art, the drive pin 19 attached to the distal end of the blade spring 17 is usually made of a rigid metal. When the drive pin 19 rubs against the bottom 25 of a center core of the metallic hub 25, sound is heard, or a trace of rubbing against the center core (hereafter, referred to as a metallic hub 25) is left. As for the drive pin 19 made of a resin, when chucked, the portion thereof fitted in the inner margin 27a of the alignment hole 27 is torn. This results in a short service life. As for a metallic drive pin 19 coated with a resin, the coating is peeled off gradually as working time increases. This results in poor durability. The use of a blade spring, caulking pin, roller, or the like results in a large number of parts and high manufacturing costs.
SUMMARY OF THE INVENTION
The present invention attempts to solve the foregoing problems of a prior art. An object of the invention is to provide a disk chucking device realizing reduction in the number of parts, enabling prevention of abrasion of a drive pin during alignment (chucking) by bringing the rigid portion of the drive pin into contact with a metallic hub and thus permitting reliable chucking, and improving durability by causing no traces even when the drive pin rubs against the bottom of the metallic hub.
To achieve the foregoing object, the present invention provides a disk chucking device comprising a drive spindle fitted in a center hole of an information recording disk, a turntable that is attached to the drive spindle and rotates as part of the drive spindle, and a support plate one of whose ends is supported by the turntable and the other one of whose ends is provided with a drive pin fitted to a drive pin fitting hole bored at a decentered position on the information recording disk. The drive pin is made of a less frictional material. A contact wall is formed in that portion of the drive pin engaging with that surface of the information recording disk having the drive pin fitting hole. The apex of the drive pin lies higher than the top of the contact wall.
In the foregoing means, the contact wall is formed as part of that side face of the drive pin engaging with the surface having the drive pin fitting hole. The drive pin is made of a less frictional material. The apex of the drive pin lies higher than the top of the contact wall. Therefore, during alignment, the rigid portion of the drive pin comes into contact with the metallic hub to permit reliable chucking. Even when the drive pin rubs against the bottom of the metallic hub, no traces are left.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a plan view of a disk chucking device of the first embodiment relating to the present invention;
FIGS. 2(a) and 2(b) are a plan and a front view of a rotary plate in the first embodiment relating to the present invention;
FIG. 3 is an explanatory diagram showing the relationship between the rotary plate and a disk hub in the first embodiment relating to the present invention;
FIGS. 4(a) and 4(b) are a plan and a front view diagrams of the rotary plate in the first embodiment relating to the present invention;
FIGS. 5(a) and 5(b) are a plan and a front view of a drive pin in the first embodiment relating to the present invention;
FIGS. 6(a), 6(b), 6(c), 6(d), 6(e) and 6(f) are plan views of chucking states in the first embodiment relating to the present invention;
FIGS. 7(a), 7(b) and 7(c) are section views taken along lines BB, CC and DD of FIGS. 6(a), 6(b) and 6(c), respectively, showing the operations in the states of FIG. 6;
FIGS. 8(a) and 8(b) are section views taken along lines EE and AA of FIG. 6(d) and FIG. (a), respectively, showing the operations in the states of FIG. 6;
FIG. 9 is an explanatory diagram showing a construction of the second embodiment relating to the present invention;
FIGS. 10(a) and 10(b) are section views showing structures of a drive pin in the second embodiment of the present invention;
FIG. 11 is a plan view of a major portion of a disk chucking device of a prior art;
FIGS. 12 (a) and 12 (b) are a plan and a front view of a blade spring for the disk chucking device of a prior art;
FIGS. 13(a), 13(b), 13(c) and 13(d) are plan views showing the operating states of the disk chucking device of a prior art;
FIGS. 14(a) and 14(b) are section views showing structures of a drive pin for the disk chucking device of a prior art; and
FIG. 15 is an explanatory diagram showing an example of a typical disk having a metallic hub.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Embodiments of the present invention will be described with reference to the drawings. Hereafter, components identical to or regarded as identical to those in the aforesaid prior art are assigned the same numerals. The duplicate description will be omitted.
FIGS. 1 to 8 are diagrams for explaining the first embodiment. FIG. 1 is a plan view of a disk chucking device relating to the present invention. FIGS. 2a and 2b a plan view and a front view of a support plate. FIG. 3 is an explanatory diagram showing the relationship between the support plate and a disk hub. FIGS. 4a and 4b are a plan view and a front view of the support plate. FIGS. 5a and 5b are a plan view and a front view of a drive pin. FIGS. 6a to 6f are explanatory diagrams showing the states of chucking operations schematically. FIGS. 7a, 7b, and 7c show B--B, C--C, and D--D cross sections of FIG. 6. FIGS. 8a and 8b show E--E and A--A cross sections of FIG. 6.
The first embodiment represents such a type that a drive pin does not sink under the bottom of a turntable. A support plate 30 is a rigid plate shaped substantially like a semi-arc as shown in FIGS. 2a and 2b. Alignment projections 33 for aligning a drive pin 32 are projecting from one end 31 of the support plate 30. The margin of the end 31 is folded up to form a contact wall 34. The contact wall 34 assumes part of a cylindrical shape along the outer circumference of the drive pin 32. The support plate 30 is bent, as shown in FIGS. 5a and 5b, from the side margin over the top thereof to form a locking claw 38. An attachment hole 39 is bored for attachment to a turntable 3.
The drive pin 32 is shaped like a cylinder and made of a less frictional material such as a synthetic resin. The top 35 of the drive pin 32 has, for example, a spherical shape and becomes highest at its center. The periphery 36 of the top 35 of the drive pin 32 is lower than the top 37 of the contact wall 34. The inclination of the top 37 of the contact wall 34 is designed to be larger than the inclination of a metallic hub 25 lying on the top 37 of the contact wall 34. Thereby, even when the metallic hub 25 rides on the top of the contact wall 34, the bottom 25a of the metallic hub 25 can move onto the top 35 of the drive pin 32 smoothly. The drive pin 32 has, as shown in FIGS. 4a and 4b, alignment holes 40 on the bottom of the flat plate thereof.
When the drive pin 32 is attached to a rotary plate 30, the flat plate of the drive pin 32 is inserted while pushing the locking claw 38 apart against the elastic force of the claw 38. The alignment projections 33 are fitted in the alignment holes 40 for alignment. Then, the flat plate of the drive pin 32 is clamped due to the elastic force of the locking claw 38. 41 denotes a guide projection of the locking claw 38 projecting from the top of the flat plate of the drive pin 32.
The other components, which have not been described in particular, are identical to those in the aforesaid prior art.
The operations of the first embodiment of a disk chucking device having the aforesaid construction will be described.
As described previously, soon after a disk cartridge 24 is loaded, a drive pin 32 may sometimes be in the state shown in FIGS. 6a, 7a, and 8b. Specifically, a top 37 of a contact wall 34 invades in a portion of a bottom 25a of a metallic hub 25.
In the above state, when a turntable 3 rotates in an arrow-F direction in FIG. 6a, even if the metallic hub 25 rides on the top 37 of the contact wall 34, the metallic hub 25 will not hit a periphery 36 of the top of the drive pin 32 as shown in FIGS. 6b and 7b, but the bottom 25a of the metallic hub 25 moves smoothly onto the top 35 of the drive pin 32 as shown in FIGS. 6c and 7c. Then, the metallic hub 25 is rotated while sliding on the drive pin 32 made of a less frictional material as shown in FIGS. 6d and 8a.
Then, the metallic hub 25 rotates while withstanding the frictional force occurring between the metallic hub 25 and the turntable 3 and between the metallic hub 25 and the drive pin 32 until the drive pin 32 comes to a position opposed to an alignment hole 27. Then, the drive pin 32 is fitted in the alignment hole 27 as shown in FIG. 6e, and brought into contact with the inner surface 27a of the outer circumference of the alignment hole 27. At this time, a head comes into contact with a disk 23, causing force in the opposite direction of the arrow-F direction. Thereby, force oriented in the radial direction of the metallic hub 25 develops in the contact wall 34. With the force, the metallic hub 25 is moved in the same direction. Consequently, a spindle 2 is pushed onto the corner 26a of a chucking hole 26 farthest from the alignment hole 27. Then, centering is carried out.
In the first embodiment having the aforesaid construction, a rotary plate 30 is formed with a plate. A contact wall 34 is formed as part of a drive pin 32 in the portion of the drive pin 32 engaging with a surface having a drive pin fitting hole. The drive pin 32 is made of a less frictional material. The apex of the top of the drive pin 32 lies higher than a top 37 of the contact wall 34. This realizes reduction in the number of parts. During alignment, the rigid portion of the drive pin 32 comes into contact with a metallic hub 25. This prevents abrasion of the drive pin, and permits reliable chucking. Even when the drive pin 32 rubs against a bottom 25a of the metallic hub 25, no trace occurs. This improves durability.
Furthermore, a periphery 36 of the top of the drive pin 32 lies lower than the top 37 of the contact wall 34. Therefore, even when the metallic hub 25 rides on the top 37 of the contact wall 34, the bottom 25a of the metallic hub 25 can move smoothly onto the top of the drive pin 32.
Referring to FIGS. 9 and 10, the second embodiment of the present invention will be described. FIG. 9 is an explanatory diagram showing a construction of the second embodiment. FIG. 10 includes explanatory diagrams showing structures of a drive pin in the second embodiment.
The second embodiment is of the same type as the aforesaid prior art. Specifically, as shown in FIGS. 9 and 10a, a blade spring 17 is attached to the bottom of a turntable 3. A drive pin 50 is supported by a pin 51 at one end of the blade spring 17 so that the drive pin 50 can rotate freely. The drive pin 50 projects through an insertion hole 13 of the turntable 3. The drive pin 50 is made of a less frictional material such as a resin. A contact wall 50 made of a metallic material is formed to shield the peripheral surface of the drive pin 50. Alternatively, the drive pin 50 may be made of a resin, and a contact wall 50b made of a metallic material may be formed to shield the peripheral surface and bottom of the drive pin 50. The top of the drive pin 50 is projecting higher than the top end of the metallic contact wall 50a or 50b.
The other components and operations of the second embodiment, which have not be described in particular, are identical to those in the aforesaid prior art.
In the second embodiment, similarly to the aforesaid prior art, chucking is carried out (a chucking state is shown in FIG. 9). Specifically, as shown in FIG. 9, a drive pin 50 of a blade spring 17 is fitted in an alignment hole 27, and a metallic contact wall 50a is brought into contact with an inner surface 27a of the alignment hole 27. Then, centering is carried out.
Even the second embodiment having the aforesaid construction provides the same advantages as the first embodiment.
As described previously, according to the present invention, the number of parts can be reduced. During alignment, a rigid portion of a drive pin comes into contact with a metallic hub. This prevents abrasion of the drive pin, and permits reliable chucking. Even when the drive pin rubs against the bottom of the metallic hub, no trace occurs. This improves durability.
|
A chucking device for receiving and rotating a magnetic disk, the magnetic disk having a centrally-located drive spindle receiving hole and an off-center alignment hole. The chucking device includes a turntable, a drive spindle centrally-located on the turntable, and a support plate including a drive pin and a contact wall. The contact wall is formed adjacent the drive pin and is used to rotate the magnetic disk by pressing against an inner wall of the alignment hole. The drive pin is made of a low friction material, such as synthetic resin, and extends above the contact wall such that when the magnetic disk is mounted on the disk chucking device, the drive pin slides easily against the hub until the drive pin and contact wall are received in the alignment hole.
| 6
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. patent application Ser. No. 13/414,090, filed on Mar. 7, 2012, which is a continuation of U.S. patent application Ser. No. 12/279,539, filed on Nov. 24, 2008, which application is a national phase entry under 35 U.S.C. §371 of International Application No. PCT/US06/42944 filed Nov. 3, 2006, which claims the benefit of U.S. Provisional Patent Application No. 60/733,988, filed Nov. 3, 2005. The disclosures of the aforesaid applications are hereby incorporated by reference herein.
FIELD OF THE INVENTION
[0002] Polymers with specialized properties for medical device coatings are described. These polymers are hydrolytically degradable and resorb within one year. These polymers are derived from monomer units which are relatively water soluble and it is this property that improves the polymers' resorption ability to within 1 year once hydrolytic degradation occurs. The polymers, nonetheless, still provide appropriately robust mechanical properties to function as medical device coatings. The polymers of the invention are based on modifications of the tyrosine-derived family of polyarylates.
BACKGROUND OF THE INVENTION
[0003] Diphenols, particularly those derived from tyrosine, are monomeric starting materials for biocompatible polycarbonates, polyiminocarbonates, polyarylates, polyurethanes, and the like. U.S. Pat. Nos. 5,099,060, 5,198,507, and 5,670,602 disclose amino acid-derived diphenol compounds useful in the preparation of polyarylates, polycarbonates and polyiminocarbonates. The polymers, for example those described in U.S. Pat. Nos. 4,980,449, 5,216,115, 5,658,995, 6,048,521, and 6,120,491, and U.S. patent application publication No. 2004/0254334, are useful as degradable polymers in general, and are particularly useful as tissue-compatible bioerodible materials for medical uses. The suitability of these polymers for this end use application is at least in part the result of their derivation from diphenols derived from the naturally-occurring amino acid L-tyrosine.
[0004] The polycarbonates in particular are strong, water-insoluble materials most suitable for use as structural implants. The L-tyrosine derived polyarylates described in U.S. Pat. No. 5,216,115, and the poly(alkylene oxide) block copolymers with these polyarylates disclosed in U.S. Pat. No. 5,658,995, feature protected carboxylic acid groups, and these polymers are limited in application because of their slow rate of degradation and significant hydrophobicity. The free acid forms of the polymers, described in U.S. Pat. No. 6,120,491 (“the '491 patent”), in which to varying degrees the ester protecting groups have been removed from the pendent carboxylic acid chains of the diphenols, are less hydrophobic and exhibit an increased degradation rate (i.e. backbone cleavage) compared to their counterparts with fully esterified carboxylic acid groups. Increasing the amount of pendant carboxylic acid diphenol contained within a particular polymer increases the hydrophilicity (water uptake) of the polymer; however, its relative complete resorption rate does not change significantly. This is because the mechanism of degradation—namely, backbone cleavage to successively smaller units containing diphenols with ester protected carboxylic acid groups-does not change the relative water solubility of the esterified monomeric units incorporated within the polymer chains, nor, in the case of the tyrosine-derived polyarylates, does it change the relative water solubility of the diacids with which they are condensed. Therefore, the introduction of an increasing fraction of free carboxylic acid side chains only increases the hydrophilicity of the polymer itself. It does not significantly impact the resorption rate of the ester diphenol fragments produced by polymer backbone degradation.
[0005] Hence, medical devices comprised of such materials will retain some significant portion of their mass for roughly the same time period as those polymers described in U.S. Pat. No. 5,099,060, which describes polymers with diphenol monomeric units that lack carboxylic acid side chains. Such polymers resorb completely only in time periods in excess of 1 year, and in many cases in closer to 2-2.5 years. The diphenol monomeric units of these polymers are significantly hydrophobic and have low water solubility.
[0006] The '491 patent describes polymers formed from a similar series of diphenol monomeric units but which contain repeating units of the same general diphenol monomers with both protected and unprotected carboxylic acid side chains. The '491 patent teaches that “the incorporation of pendent carboxylic acid groups within the polymer bulk has a dramatic and previously unrecognized accelerating effect on the rate of polymer backbone degradation and resorption both in vitro and in vivo.” However, the present inventors have surprisingly found that incorporating some fraction of diphenol monomers with pendant carboxylic acid groups into the polymer does not accelerate overall resorption, because the monomers with protected carboxylic acid groups remain too hydrophobic for resorption on desirable time scales. For example, a polymer incorporating 10% pendant carboxylic acid side chain will degrade (by backbone cleavage) at a faster rate than one containing no pendant carboxylic acid side chains, and some resorption will occur, but this resorption is due to the water solubility of the diphenol monomers containing the pendant carboxylic acid groups. Once this monomer is resorbed, the remaining polymer, albeit one of smaller chain length, contains the protected carboxylic acid side chain monomers which are hydrophobic and resorb at a very slow rate. Incorporating a high fraction of pendant carboxylic acid side chain monomer (e.g., 50% of the diphenol monomer content of the polymer) essentially creates a water-soluble polymer that solubilizes and undergoes degradation until the polymer chain fragments that are enriched in protected pendant carboxylic acid groups precipitate out of solution. The preferred protected monomers in the '491 patent are actually the most hydrophobic and therefore the slowest to resorb, i.e. the ethyl, butyl, hexyl, and octyl esters.
[0007] Complete, or nearly complete, polymer resorption (e.g., at least 90%, 95%, 96%. 97%. 98%, 99%, 99.5%, or 100%) is important in the use of “biodegradable” polymers in medical devices. Biodegradable and resorbable polymers are primarily used to deliver drugs for a finite period of time or to serve some other temporary purpose, such as to provide a biocompatible surface, enhanced tissue growth, or extra strength during implantation. Polymers that do not completely resorb leave remnants that can cause anything from minor inflammation and pain to excess scarring, and in the case of cardiovascular implants, such remnants can cause thrombosis and possibly patient death.
SUMMARY OF THE INVENTION
[0008] The invention provides polymers with specialized properties, making them particularly suitable for coatings on implanted medical devices, for forming films for use with medical devices, and other uses requiring the short- or defined-term presence of a polymer matrix. The polymers of the invention are hydrolytically degradable and are resorbed by the body within one year. These polymers are derived from monomer units which are relatively water-soluble and it is this property that improves the polymers' resorption time to within 1 year once hydrolytic degradation begins. The polymers nonetheless exhibit sufficiently robust mechanical properties to function as medical device coatings. The polymers of the invention are based on modifications of the tyrosine-derived family of polyarylates.
[0009] The need for polymers that resorb within one year (or such lesser times as may be desired), while retaining useful properties (e.g., at least 1 week of drug elution, biocompatibility, and spray coating capability), is met by the present invention. It has now been found that it is possible to effect better resorption by increasing the water solubility of one or more of the component parts of the diphenol or diacid monomer units of the polymer. Thus, the present invention makes it possible to modulate the rate of resorption without compromising the drug release rate or other physical properties optimized for the end use application, by choosing components having increased water solubility and/or or increased hydrolysis rates in vivo. Certain polymers of the invention can, for example, release a drug over at least a 5 day period.
[0010] The present invention also makes it possible to create resorbable polymers with pendant carboxylic acid groups, which modulates the hydrophilicity of the polymer as well as the time over which the polymer properties remain intact. This provides a wide variety of drug release capabilities, so that the polymer can be adapted for hydrophobic and hydrophilic drugs. This is a significant improvement over conventional medical polymers such as poly(lactic acid), poly(glycolic acid), polycaprolactone, and the phenolic polyarylates and polycarbonates exemplified in U.S. Pat. No. 6,120,491. This invention allows independent optimization of the useful properties of the polymers, and significantly improves upon the versatility and utility of the phenolic polymer systems known in the art, particularly phenolic polycarbonates, polyarylates, and poly(iminocarbonates), and poly(alkylene oxide) copolymers thereof.
[0011] The polymers of the present invention have many uses and may be formed into a variety of products, including but not limited to implantable medical devices with desired lifetimes of less than one year (e.g., adhesion barriers and surgical meshes to aid wound healing), incorporation into implantable medical devices, and combination with a quantity of a biologically or pharmaceutically active compound sufficient for effective site-specific or systemic drug delivery. See, for example, Gutowska et al., J. Biomater. Res., 29, 811-21 (1995) and Hoffman, J. Controlled Release, 6, 297-305 (1987). A biologically or pharmaceutically active compound may be physically admixed with, embedded in or dispersed in a polymer of the invention, or the polymer may be applied as an overcoating of another polymer-containing drug layer, where such overcoating delays or slows drug release. In other uses and products, the polymer is in the form of a sheet or a coating applied to an implantable medical device, such as a hernia repair mesh, a stent, or a barrier layer for the prevention of surgical adhesions (see, e.g., Urry et al., Mat. Res. Soc. Symp. Proc., 292, 253-64 (1993).
[0012] Another aspect of the present invention provides a method for site-specific or systemic drug delivery, by implanting in the body of a patient in need thereof an implantable drug delivery device containing a therapeutically effective amount of a biologically or pharmaceutically active compound, in a matrix of (or coated with) a polymer of the present invention. Yet another aspect of the present invention provides a method for preventing the formation of adhesions between injured or surgically repaired tissues, by inserting as a barrier between the injured tissues a sheet or coating comprising a polymer of the present invention.
BRIEF DESCRIPTION OF THE FIGURES
[0013] FIG. 1 shows the degradation over time of polymers of the invention.
[0014] FIG. 2 shows the degradation over time of polymers of the invention.
[0015] FIG. 3 shows the degradation over time of polymers of the invention.
[0016] FIG. 4 shows the degradation over time of polymers of the invention.
[0017] FIG. 5 shows the degradation over time of polymers of the invention.
[0018] FIG. 6 shows the degradation over time of polymers of the invention.
[0019] FIG. 7 shows the degradation over time of polymers of the invention.
[0020] FIG. 8 shows the degradation over time of polymers of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0021] As used herein, DTE refers to the diphenol monomer desaminotyrosyl-tyrosine ethyl ester; DTBn is the diphenol monomer desaminotyrosyl-tyrosine benzyl ester; DT is the diphenol monomer desaminotyrosyl-tyrosine with a free carboxylic acid. Other diphenol monomers can be named using a similar system. P22 is a polymer produced by condensation of DTE and succinic acid. P22-10, P22-15, P22-20, etc., represent polymers produced by condensation of a mixture of DTE and the indicated percentage of DT (i.e., 10, and 20% DT) with succinic acid. See U.S. patent application publication No. 2004/0254334 for further explanation and examples of the nomenclature of these phenolic polymers.
[0022] The invention provides diphenol monmer units having structure
[0000]
[0000] wherein m is 0, 1, or 2; n is 0 to 4, and Y is selected from the group consisting of C 1 -C 18 alkylamino, —NHCH 2 CO 2 R′, —NH(CH 2 ) q OR′, —NH(CH 2 CH 2 O) p R′, —NH(CH 2 CH 2 CH 2 O) p R′,
[0000]
[0000] where q is 0 to 4, p is 1 to 5000, and R′ is selected from the group consisting of H, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 8 -C 14 alkylaryl, benzyl, and substituted benzyl. As used herein, the terms alkyl and alkenyl refer to branched- or straight-chain alkyl and alkenyl groups. The term aryl refers to phenyl and naphthyl groups which may be substituted or unsubstituted with halogen, methoxy, alkyl, and the like. The term alkylaryl does not refer to aryl groups having alkyl substituents; it refers to alkyl groups having an aryl substituent. Substituted benzyl refers to benzyl groups substituted with one or more halogens, methoxy groups, nitro groups, alkyl groups, and the like. Substituted benzyl groups known in the art to be suitable for use as protecting groups for ethers and esters are included, including but not limited to 4-methoxybenzyl, 2-methoxybenzyl, 2,4-dimethoxybenzyl, and 2-nitrobenzyl groups.
[0023] The invention also provides diphenol monomer units having structure
[0000]
[0000] wherein n is 0 to 4; and Y is selected from the group consisting of C 1 -C 18 alkylamino, —NHCH 2 CO 2 R′, —NH(CH 2 ) q OR′—NH(CH 2 CH 2 O) p R′, —NH(CH 2 CH 2 CH 2 O) p R′,
[0000]
[0000] where q is 0 to 4, p is 1-5000 and R′ is selected from the group consisting of H, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 8 -C 14 alkylaryl, benzyl, and substituted benzyl. In preferred embodiments, Y is NHCH 2 CO 2 R′.
[0024] The invention also provides diphenol monomer units having structure
[0000]
[0000] wherein m is 0, 1, or 2; and R′ is selected from the group consisting of H, C 1 -C 18 alkyl, C 2 -C 18 alkenyl, C 8 -C 18 alkylaryl, benzyl, and substituted benzyl.
[0025] Through co-polymerization of the diphenol monomer units described above with phosgene, cyanogen bromide, or an appropriate diacid, by methods known in the art, the invention provides polymers comprising monomer units having formula
[0000]
[0000] wherein Y is OMe or OEt. In these polymers, m, n, and Y and R′ are as defined above, and A is selected from the group consisting of —CO—, —C(—NH)—, and —CO—X—CO—. In these polymers, X is selected from the group consisting of C 1 -C 18 alkylene, C 1 -C 18 alkenylene, divalent C 6 -C 10 arylene, divalent C 7 -C 18 alkylaryl, CH 2 OCH 2 , CH 2 O(CH 2 CH 2 O) s CH 2 , (CH 2 ) r CO 2 (CH 2 CH 2 CH 2 O) s CO(CH 2 ) r , and (CH 2 ) r CO 2 (CH 2 CH 2 O) s CO(CH 2 ) r , where r is 2 to 4 and s is 1 to 5000. In specific embodiments of the polymers of the invention, Y is preferably NHCH 2 CO 2 R′.
[0026] In certain embodiments, the polymers of the invention consist essentially of monomer units having formula
[0000]
[0000] where m, n, A and Y are as defined above.
[0027] In certain embodiments, the polymers of the invention as described above further comprising monomer units independently having formula
[0000]
[0000] wherein m, n, and A are as defined in claim 5 , and Y is OH or O-benzyl.
[0028] In preferred embodiments of these polymers, A is —CO—X—CO—, and between 0.1% and 99.9% of the X moieties are CH 2 ) r CO 2 (CH 2 CH 2 O) s CO(CH 2 ) r and/or (CH 2 ) r CO 2 (CH 2 CH 2 CH 2 O) s CO(CH 2 ) r . The range is preferably from about 1% to about 99%, more preferably from about 10% to about 80%. Most preferably, from about 20% to about 50% of the X moieties are (CH 2 ) r CO 2 (CH 2 CH 2 O) s CO(CH 2 ) r and/or (CH 2 ) r CO 2 (CH 2 CH 2 CH 2 O) s CO(CH 2 ) r .
[0029] In certain preferred embodiments, between about 1% and 50% of the monomer units have formula
[0000]
[0000] wherein Y is OH or O-benzyl. The range is more preferably from about 5% to about 40%, and most preferably from about 10% to about 30%.
[0030] Particularly preferred are polymers wherein A is —CO—X—CO— and X is —CH 2 —O—(CH 2 CH 2 O) s CH 2 , with s being 0 to 200. Also provided are polymers comprising monomer units having formula
[0000]
[0000] wherein Y is OMe or OEt, A is selected from the group consisting of —CO—, —C(—NH)—, and —CO—X—CO—, and X is selected from the group consisting of CH 2 CH 2 , CH 2 CH 2 CH 2 , and —CH 2 —O—(CH 2 CH 2 O) s CH 2 , and s is 0 to 200.
[0031] Polymers of the present invention may be formed by reaction of the diphenol monomer units of the invention with a diacid or with phosgene, thereby forming polyarylates and polycarbonates respectively. A schematic diagram of the reaction of the diphenol monomer DTE with a diacid is shown in Scheme 1 below.
[0000]
[0032] The compounds of the invention are those where the “starting” moieties designated as positions 1-4 below are replaced by one or more moieties that are more hydrophilic or more water-soluble, as illustrated in Tables 1 and 2 below.
[0000]
[0033] The polymers of the invention thus have at least one of any one of positions 1-4 changed, but can also have 2 positions, 3 positions or all four positions changed. Any permutation of changes to the 4 positions is contemplated, provided that at least one change is made and that at least one change to a moiety make it more soluble than its corresponding starting moiety. In the case of the ester position (position 3), the change may introduce a better leaving group than ethanol. Hence, in accordance with the invention, at least one moiety at one of the positions is more water soluble than its starting moiety; at position 3 the moiety may also be a better leaving group than ethanol, or otherwise be more sensitive to hydrolysis under the conditions of use. By way of example, amides can be more sensitive to hydrolysis in vivo than ethyl esters, due to the action of proteases.
[0034] The starting moieties are as follows: position 1, tyrosine (T); position 2, desaminotyrosine (D), position 3, ethyl ester (E); position 4, succinate (S or succinate). It is convenient to name the polymer families according to the four positions so that the “starting polymer” with no changes of moieties is DTES or DTE succinate (note this is distinct from DTE, when DTE refers to the diphenol monomeric unit). Either single letters or moiety names are used. Hence examples of polymer families include BTE glutarate, DTM glutarate, DTM succinate and the like. The single letters for each moiety as used herein are shown in Tables 1 and 2. In Table 1, the bold T is used as a shorthand to represent the remainder of the molecule.
[0035] The preferred polymer families of the invention are provided in Table 3 below and do not include all the possible permutations that occur from combining the all four positions. However, all such permutations are contemplated by the invention.
[0036] The polymers of the present invention preferably have from 0.1 to 99.9% diphenol monomer DT or from 0.1 to 99.9% PEG diacid to promote the degradation process. The use of either or both methods, i.e. incorporation of DT and/or a PEG diacid (see examples in table below), is within the scope of the invention, and can be used with any of the polymer families of the invention.
[0000]
TABLE 1
DTE
Chemical Name
Succinate
(Abbrev for polymer
Site
water
family)
Change
solubility
Ethyl ester (E)
Site 3: none
Methyl ester (M)
3
Propyl amide
3
Glycine amide methyl ester
3
2-methoxyethyl amide
3
3-methoxypropyl amide
3
Glycine amide benzyl ester
3
Glycine amide
3
Glucosamine amide
3
PEG amide (n = 1-5000)
3
PEG ester (n = 1-5000)
3
Tyrosine (T)
Site 1: none
0.45 mg/mL
Hydroxyphenyl glycine
1
3
[0000]
TABLE 2
Polymer
Site
Water
Solubility
Base Elements
Change
Solubility
Difference
Succinic acid
0
76
0
Glutaric acid
4
640
9
PEG diacid at .01-99% (succinate PEG, n = 1-500)
4
Water soluble
Greater than 8; depends on amount of PEG incorporated in backbone
Diglycolic acid
4
Water soluble
Greater than 10
bis(carboxymethyl) PEG (N = 250-600
4
Water soluble
Greater than 10
DAT
0
1.63
4-hydroxy benzoic acid
2
8
4
4-hydroxy phenylacetic acid
2
3-hydroxy benzoic acid
2
Salicylic acid
[0000]
TABLE 3
Polymer Family
(includes all free
acid versions
BTE glutarate
DTM glutarate
DT Propylamide glutarate
DT Glycinamide methyl ester glutarate
BTE succinate
BTM succinate
BTM succinate PEG
BTM succinate PEG
DTM succinate PEG
DT propyl amide succinate
DT glucosamine succinate
DT glucosamine glutarate
DT PEG amide succinate
DT PEG amide glutarate
[0037] Methods for preparing the diphenol monomers are known in the art, for example as disclosed in U.S. Pat. Nos. 5,587,507 and 5,670,602. Methods for preparing polymers with DT content are disclosed in U.S. application publication 2004/0254334.
[0038] The polymers of the present invention having pendent carboxylic acid groups may be prepared by the palladium-catalyzed hydrogenolysis of corresponding polymers having pendant benzyl carboxylate groups as describe in the '491 patent. Any other method that allows for the selective deprotection of a pendant carboxylate group is suitable for use in the preparation of the carboxylate-containing polymers of the present invention.
[0039] The polymers of the present invention can find application in areas where both solid materials and solvent-soluble materials are commonly employed. Such application include polymeric scaffolds in tissue engineering applications and medical implant applications, including the use of the polycarbonates and polyarylates of the present invention to form shaped articles such as vascular grafts and stents, drug eluting stents, bone plates, sutures, implantable sensors, barriers for surgical adhesion prevention, implantable drug delivery devices, scaffolds for tissue regeneration, and other therapeutic agent articles that decompose harmlessly within a known period of time.
[0040] Controlled drug delivery systems may be prepared, in which a biologically or pharmaceutically active agent is physically embedded or dispersed within a polymeric matrix or physically admixed with a polycarbonate or polyarylate of the present invention, or it could be covalently attached to the pendant carboxylic acid.
[0041] Examples of biologically or pharmaceutically active compounds suitable for use with the present invention include non-steroidal anti-inflammatories such as naproxen, ketoprofen, ibuprofen; anesthetics such as licodaine, bupivacaine, and mepivacaine; paclitaxel, 5-fluorouracil; antimicrobials such as triclosan, chlorhexidine, rifampin, minocycline; keflex; acyclovir, cephradine, malphalen, procaine, ephedrine, adriamycin, daunomycin, plumbagin, atropine, quinine, digoxin, quinidine, biologically active peptides, chlorin e6, cephradine, cephalothin, cis-hydroxy-L-proline, melphalan, penicillin V, aspirin, nicotinic acid, chemodeoxycholic acid, chlorambucil, and the like. The compounds are covalently bonded to the polycarbonate or polyarylate copolymer by methods well understood by those of ordinary skill in the art. Drug delivery compounds may also be formed by physically blending the biologically or pharmaceutically active compound to be delivered with the polymers of the present invention having pendent carboxylic acid groups, using conventional techniques well-known to those of ordinary skill in the art.
[0042] Detailed chemical procedures for the attachment of various drugs and ligands to polymer bound free carboxylic acid groups have been described in the literature. See, for example, Nathan et al., Bio. Cong. Chem., 4, 54-62 (1993).
[0043] Biologically active compounds, for purposes of the present invention, are additionally defined as including cell attachment mediators, biologically active ligands and the like.
[0044] Processability of the polymers is generally as described in the '491 patent.
[0045] It will be appreciated by those skilled in the art that various omissions, additions and modifications may be made to the invention described above without departing from the scope of the invention, and all such modifications and changes are intended to fall within the scope of the invention, as defined by the appended claims. All references, patents, patent applications or other documents cited are herein incorporated by reference in their entirety.
EXPERIMENTAL
Degradation Study Protocol
[0046] Molecular weight (MW) profile: For monitoring MW decrease as a function of time, polymer films, or meshes coated with polymer, with approximate dimensions 1×1×0.01 cm, were incubated with 0.01 M PBS or 0.01M PBS with Tween20 (50 to 100 mL) at 37° C. without shaking. At each time point, polymer samples were dissolved in 5 mL of DMF containing 0.1% TFA. The solutions were filtered through 0.45μ Teflon™ syringe-mountable tilters and transferred to analysis vials for analysis by gel permeation chromatography (GPC).
[0047] Mass loss profile: For mass loss analysis, films or meshes coated with polymer were incubated with 0.01 M PBS or 0.01M PBS with Tween20 (50 to 100 mL) at 37° C. The buffer in the vials was changed at periodic intervals and analyzed for soluble degrading components. At each time point, 1-2 mL buffer from three small vials was filtered through 0.45μ Teflon™ syringe-mountable filters and transferred to analysis vials for analysis by reversed phase HPLC. Alternately, the devices were washed, dried and weighed (final weight) and the mass loss determined by subtracting the final weight from the original weight.
Polymer Synthesis
[0048] DTE (17.85 g), diglycolic acid (6.7 g) and DPTS catalyst (5.88 g) were added to 75 mL methylene chloride. After stirring for 30 minutes, diisopropylcarbodiimide (20 g) was added and the mixture stirred for 24 hours. The polymer formed was isolated by precipitation into 2-propanol. The polymer was purified by three precipitations from methylene chloride/isopropanol to produce the polymer P(DTE diglycolate) in about 65% yield. MW=40 to 75000.
Results
[0049] FIG. 1 shows molecular weight (MW) retention as a function of time for various members of the DTE succinate family with DT content ranging from 10-25% of the diphenol content. Very little difference in the degradation times (backbone cleavage) is evident.
[0050] FIG. 2 shows the mass loss of various members of the DTE succinate family with DT ranging from 10-25% of the diphenol content. The mass loss slows as function of time because the DT is gone.
[0051] FIG. 3 shows the mass loss of 10% DT/DTE succinate at 37° C. and 50° C. Mass loss slows down (curve evens out) as all DT is expended from the polymer.
[0052] FIGS. 4-8 show the rate of degradation of various polymers of the invention, as measured by the decrease in molecular weight over time.
[0053] The table below shows the average molecular weight (MW) and composition of residual fragments of polymers within the DT-DTE succinate family of polymers at various times during in vitro incubation. The residual fragments are analyzed by liquid chromatography-mass spectrometry and relative quantities of peaks for each compound are reported. No indicates that the compound corresponding to that peak was not detectable. The relative total mass is found by the sum of the peak areas for a given compound. From this it is evident that the DT-containing fragments peaks 1 and 4 represent very little of the remaining mass. Peak 8 also contains DT but with twice the amount of DTE-succinate. DTE-suc is DTE-succinate.
[0054] Virtually no DT-containing fragments remain at the time points noted and time to total resorption for all of the polymers within the DTE succinate family will be equivalent, because the remaining insoluble fraction in each polymer is chemically equivalent.
[0000]
Sample
Peak 1
Peak 2
Peak 3
Peak 4
Peak 5
Peak 6
Peak 7
Peak 8
Peak 9
P22-10
DT
DTE
No
DTE-
No
DTE-
DTE-suc
DTE-
DTE-suc
MW = 3000
(1.67)
(0.29)
suc-DT
suc-DTE
DTE-suc
suc
DTE-suc
(6 months)
(0.68)
(6.1)
DT (2.8)
DTE-
DTE-suc
suc
DTE (9.5)
DTE
(10)
P22-12.5
No
DTE
No
DTE-
No
DTE-
DTE-suc
DTE-
DTE-suc
MW = 2000
(0.037)
(2.33)
suc-DT
suc-DTE
DTE-suc
suc
DTE-suc
(6 months)
(0.44)
(10)
DT (4.5)
DTE-
DTE-suc
suc
DTE (6.9)
DTE
(8.6)
P22-15
DT
DTE
No
DTE-
No
DTE-
DTE-suc
DTE-
DTE-suc
MW = 3000
(0.22)
(0.9)
suc-DT
suc-DTE
DTE-suc
suc
DTE-suc
(4 months)
(0.4)
(8.7)
DT (2.66)
DTE-
DTE-suc
suc
DTE (6.6)
DTE
(10)
P22-17.5
No
DTE
No
DTE-
No
DTE-
DTE-suc
DTE-
DTE-suc
MW = 3700
(0.41)
(0.1)
suc-DT
suc-DTE
DTE-suc
suc
DTE-suc
(3.5 months)
(0.39)
(4.58)
DT (2.1)
DTE-
DTE-suc
suc
DTE (10)
DTE
(3.2)
P22-20
DT
DTE
No
DTE-
No
DTE-
DTE-suc
DTE-
DTE-suc
MW = 3600
(0.07)
(0.2)
suc-DT
suc-DTE
DTE-suc
suc
DTE-suc
(5 months)
(0.28)
(6.2)
DT (1.6)
DTE-
DTE-suc
suc
DTE (7.7)
DTE
(10)
[0055] For P(DTE diglycolate) incubated at 50° C. for 10 days in PBS buffer, the degradation results were as follows:
[0000]
MW (avg.) of
MW of residual
residual solid
solid
Initial MW
at 5 days
at 10 days
Solid: 25,000 kD
Solid: 7,000 kD
No solid remaining
Buffer: none
Buffer DTE
Sample completely
resorbed
Buffer: DTE
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The invention provides biocompatible resorbable polymers, comprising monomer units having formula (I), formula (II), formula (III) or formula (IV). The polymers degrade over time when implanted in the body, and are useful as components of implantable medical devices.
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REFERENCE TO RELATED APPLICATION
[0001] This application is a divisional patent application of U.S. patent application Ser. No. 10/253,139, filed Sep. 24, 2002.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to water treatment systems and more particularly pertains to a new and simplified water treatment system for reducing the level of bacteria in a flow of water by creating an environment favorable for aerobic bacteria and unfavorable for anaerobic bacteria.
[0004] 2. Description of the Prior Art
[0005] The use of water treatment systems is known in the prior art. Many known water treatment systems mix constituent chemicals together (sometimes forming a gaseous substance) prior to mixing the resulting combination of the chemicals with the water at a single location, and typically in such systems three pumps are employed for pumping the constituent chemicals and combinations.
[0006] In these respects, the water treatment system according to the present invention substantially departs from the conventional concepts and designs of the prior art, and in so doing provides an apparatus and method primarily developed for the purpose of reducing the level of bacteria in a flow of water by creating an environment favorable for aerobic bacteria and unfavorable for anaerobic bacteria.
SUMMARY OF THE INVENTION
[0007] In the most general sense, the system of the invention is directed to creating in a flow of water an environment favorable for aerobic bacteria and unfavorable for anaerobic bacteria.
[0008] The present invention contemplates a system including a method for treating water and a suitable apparatus for carrying out the method of the invention, although other apparatus may also be suitable for carrying out the method.
[0009] Significantly, one aspect of the method includes lowering the pH level of the flow of water to a level, or range of levels, that is sufficient to produce a relatively acidic water environment, and adding sodium chlorite to the flow of water so that the sodium chlorite is activated to form, or converted into, chlorine dioxide (and other by products) for killing various undesirable bacterial elements that may be present in the water, such as, for example, E - coli, salmonella, chrytosporidium, etc. In at least one embodiment of the invention, the range of suitable pH levels is between approximately 5.5 and approximately 6.5.
[0010] Another aspect of the method contemplates adding or injecting sodium chlorite into the flow of water at a location relatively close to the location in the flow of water where the pH of the water is lowered into the desired range, and in some embodiments of the invention this addition of sodium chlorite is performed generally as close as possible to the location of pH lowering. In at least one embodiment of the invention, the location of sodium chlorite addition to the flow of water is less than approximately one foot (approximately 30 cm) from the location of pH lowering, which may comprise, for example, the point of injecting a product that lowers the pH of the flow of water.
[0011] Yet another aspect of the method of the invention contemplates creating an acidic water environment sufficient to cause conversion of much of the added sodium chlorite to chlorine dioxide (and other byproducts), but generally insufficient to cause conversion of all of the sodium chlorite to chlorine dioxide in the proximity of the location of addition of the sodium chlorite to the flow of water. Preferably, a portion of the sodium chlorite added to the flow of water remains unconverted at the point of use of the water, so that after ingestion of the water, a portion of the sodium chlorite is also ingested into the stomach or gut of the end user, and contributes to control of bacteria in the relatively acidic environment of the stomach of the end user of the water. In at least one embodiment of the invention, the residual level of chlorine dioxide in the flow of water at the point of use is in the range of approximately 0.2 PPM to approximately 0.8 PPM.
[0012] With regard to the apparatus aspects of the invention, one embodiment includes a conduit with an inlet end and an outlet end for carrying a flow of water moving in a direction of flow extending from the inlet end to the outlet end. Flow measuring means may be provided for detecting a rate of water flow through the conduit. A first fluid injection means may be provided for adjustably injecting a first fluid into the flow of water, with the first fluid injection means being in fluid communication with the flow of water through the conduit. A second fluid injection means may be provided for adjustably injecting a second fluid into the flow of water separately of the injection of the first fluid, with the second fluid injection means also being in fluid communication with the flow of water through the conduit.
[0013] There has thus been outlined, rather broadly, the more important features of the invention in order that the detailed description thereof that follows may be better understood, and in order that the present contribution to the art may be better appreciated. There are additional features of the invention that will be described hereinafter and which will form the subject matter of the claims appended hereto.
[0014] In this respect, before explaining at least one embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of construction and to the arrangements of the components set forth in the following description or illustrated in the drawings. The invention is capable of other embodiments and of being practiced and carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein are for the purpose of description and should not be regarded as limiting.
[0015] As such, those skilled in the art will appreciate that the conception, upon which this disclosure is based, may readily be utilized as a basis for the designing of other structures, methods and systems for carrying out the several purposes of the present invention. It is important, therefore, that the claims be regarded as including such equivalent constructions insofar as they do not depart from the spirit and scope of the present invention.
[0016] Advantages of the invention, along with the various features of novelty which characterize the invention, are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and the specific objects attained by its uses, reference should be made to the accompanying drawings and descriptive matter in which there are illustrated preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] The invention will be better understood and objects of the invention will become apparent when consideration is given to the following detailed description thereof. Such description makes reference to the annexed drawings wherein:
[0018] FIG. 1 is a schematic front view of a water treatment apparatus of the system according to the present invention.
[0019] FIG. 2 is a schematic flow diagram of the method the present invention.
[0020] FIG. 3 is a schematic diagrammatic view of the signal paths of the present invention.
[0021] FIG. 4 is a schematic diagrammatic view of the fluid paths of the present invention.
DESCRIPTION OF PREFERRED EMBODIMENTS
[0022] With reference now to the drawings, and in particular to FIGS. 1 through 4 thereof, a new water treatment system embodying the principles and concepts of the present invention and generally designated by the reference numeral 10 will be described.
[0023] As best illustrated in FIGS. 1 through 4 and described below, the water treatment system 10 generally includes a method of continuously treating a flow of water (or optionally another fluid), and a means or apparatus for treating the water according to aspects of the method of the invention.
[0024] The aspects of a suitable apparatus, or water treatment assembly 10 , for performing the method aspects of the invention will first be described. The water treatment assembly 10 may include a conduit 12 with an inlet end 14 and an outlet end 16 for carrying a flow of water moving in a direction of flow extending from the inlet end of the conduit to the outlet end of the conduit.
[0025] In one embodiment of the invention, a valve 18 is provided for controlling flow through the conduit. The valve 18 may be mounted on the conduit 12 at a location that is generally toward the inlet end 14 of the conduit. Illustratively, the valve 18 may comprise a ball valve, although other suitable valve types may be used. A check valve 20 may also be provided for resisting flow of water in a direction from the outlet end 16 toward the inlet end 14 of the conduit 12 . The check valve 20 may be mounted on the conduit 12 toward the inlet end 14 of the conduit 12 , and may be mounted between the valve 18 and the outlet end 16 of the conduit, but before the fluid injection means (described below) in the direction of the flow of water through the conduit, so that treated water is blocked from flowing out of the inlet end 14 back towards the supply of water.
[0026] The water treatment assembly 10 may also include means for measuring flow through the conduit 12 to detect a rate of water flow through the conduit. The flow measuring means may be located on the conduit 12 toward the inlet end 14 of the conduit, and may be located after the valve 18 and check valve 20 (if such are included in the water treatment assembly 10 ) but before the fluid injection means. The flow measuring means may comprise a flow meter 22 that is in communication with a flow sensor 23 mounted on the conduit 12 . One suitable flow meter is the AUTOTROL 491 SM flow meter available from Osmonics Corporation of Minnetonka, Minn.
[0027] The water treatment assembly 10 also includes a first fluid injection means for adjustably injecting a first fluid into the flow of water. The first fluid injection means may comprise a first fluid injection apparatus 24 that is in fluid communication with the flow of water in the conduit 12 . The first fluid injection apparatus 24 may be connected to the conduit 12 at a location after the flow meter 22 in the flow of water. The first fluid injection apparatus 24 may include a first injection fitting 26 mounted on the conduit 12 so that the first injection fitting is in fluid communication with the flow of water moving through the conduit. The first fluid injection apparatus 24 may also include a first injection pump 28 that is in fluid communication with the first injection fitting 26 for pumping the first fluid into the flow of water in the conduit 12 through the first injection fitting. An output of the first injection pump 28 may be suitably connected to the first injection fitting 26 , and an input of the first injection pump may be suitably connected to a supply 29 of the first fluid. The first injection pump 28 may be programmable to output or inject the first fluid into the flow of water at a predetermined rate per unit (for example, parts per million (PPM)) of water flow. The injection of the first fluid at the predetermined rate per unit of water flow should also be responsive to a signal provided to the pump 28 by the flow meter 22 that indicates the actual water flow rate.
[0028] The water treatment assembly 10 may also include a second fluid injection means for adjustably injecting a second fluid into the flow of water. The second fluid injection means may comprise a second fluid injection apparatus 30 that is in fluid communication with the flow of water in the conduit 12 . The second fluid injection apparatus 30 may be connected to the conduit 12 at a location after the flow meter 22 in the flow of water through the conduit, and should be located after the first injection means in the direction of the water flow. The second fluid injection apparatus 30 may include a second injection fitting 32 mounted on the conduit so that the second injection fitting is in fluid communication with the flow of water through the conduit. The second fluid injection apparatus 30 may also include a second injection pump 34 that is in fluid communication with the second injection fitting 32 for pumping the second fluid into the flow of water in the conduit 12 through the second injection fitting. An output of the second injection pump 34 may be suitably connected to the second injection fitting 32 , and an input of the second injection pump may be suitably connected to a supply 35 of the second fluid. The second injection pump 34 may also be programmable to output or inject the second fluid into the flow of water based on a flow rate signal provided to the pump 34 by the flow meter 22 .
[0029] In one illustrative embodiment of the invention, each of the injection pumps may be of the same general type, such as, for example, a solenoid-driven metering pump. One such type of pump is the PZ and PZi series of pumps that may be obtained from Tacmina Corporation of Osaka Japan.
[0030] The water treatment assembly 10 may also include means for continuously facilitating the mixing of the flow of water with the first fluid and the second fluid added to the flow of water. In one embodiment of the invention, the mixing means comprises a mixer 36 which includes a plurality of vanes that are located on an interior of the conduit 12 near the outlet end 16 of the conduit, although other suitable active or passive mixing means may be employed.
[0031] The water treatment assembly 10 may also include means for controlling the injection of the first fluid by the first fluid injecting apparatus 24 and injection of the second fluid by the second fluid injection apparatus 30 into the flow of water in the conduit 12 based upon the rate of flow of water as measured by the flow meter 22 . In one embodiment of the invention, the means for controlling injection may be incorporated into the flow meter 22 and the injection pumps 28 , 34 , and the connections between these elements. The flow meter 22 may provide an electrical signal to each of the injection pumps 28 , 34 that varies with the rate of the flow of water through the conduit 12 as measured or detected by the flow sensor 23 . Additionally, each of the injection pumps 28 , 34 may be set or calibrated to inject the respective fluid at a predetermined rate per unit water flow (to achieve a desired PPM) based on the rate of water flow through the conduit as measured by the flow meter. The predetermined rates for each of the first and second fluids may be entered or programmed into the respective first 28 and second 34 pumps based on the characteristics of the water detected by periodic testing of the water.
[0032] In the method aspect of the invention, a flow of water may be treated according to the inventive method using, for example, the water treatment assembly described above or other suitable apparatus. The water treatment assembly may be provided or situated in a suitable location for treating a substantially continuous, or even intermittent, flow of water through the conduit of the assembly. The inlet end of the conduit may be connected directly or indirectly to a supply of relatively untreated water, such as a well, and the water may be pumped from the supply to the conduit by a pump thus producing the flow of water. Various types of filtration of the water may optionally also be performed on the flow of water prior to the introduction of the water into the inlet end 14 of the conduit. The outlet end 16 may be connected directly or indirectly to the point of use of the water.
[0033] The method of the invention may include performing an initial set up for the water treatment assembly 10 by analyzing a sample of the water to be treated on an ongoing basis by the water treatment system. The initial set up step may include detecting a pH level of the water to be treated by the water treatment assembly. It is preferred that the detection of the pH level of the water is performed on an ongoing intermittent basis, such as, for example, at least twice a week, but more frequent testing may be necessary if the characteristics of the water is known to vary significantly over time.
[0034] As part of the initial set up, the untreated water may also be tested for other characteristics, such as elements and compounds. In one embodiment of the invention, the characteristics tested include iron, manganese, sulfur, calcium, nitrates, arsenic, and sodium. The untreated water may also be tested for the presence of organisms such as coliform bacteria. The presence of such items is typically determined, for example, in levels of parts per million (PPM). The water may also be tested after treatment for residual levels of various characteristics, and such testing may be carried out using, for example, the Chlorine Dioxide Tester available from Chemtrics of Charleston, Va. It should be realized that the rates of adding the first and second fluids may be determined by testing the untreated water and adjusting the rates of the addition of the first and second fluids, or by testing water that has been treated at initial rates and then adjusting the initial rate appropriately until testing of the treated water results in the desired characteristics.
[0035] The initial set up step may also include determining a rate for adding the first fluid to the flow of water based on the rate of water flow, and also determining a rate for adding the second fluid to the flow of water based on the rate of water flow. The rate of adding each of the first and second fluids is generally based on the pH level, mineral level, and bacteria level that are measured in the water to be treated.
[0036] The method of the invention includes measuring a rate of water flow through the conduit, and the flow measurement is preferably performed on a continuous basis as the system operates, so that fluctuations in the flow rate of water through the water treatment assembly do not result in too much or too little of the first and second fluids being added to the flow of water as the fluctuations occur. It should be realized that the measurement of the water flow rate may not necessarily be performed by a flow meter, and that other means may be employed to activate the injection pumps, such as, for example, the use of signals generated by a pump that is pumping the water from the supply to the water treatment assembly to establish a flow rate. The use of the flow meter is preferred for creating a compact, generally self-contained water treatment assembly that does not rely upon various external systems for operation.
[0037] The method of the invention may include injecting the first fluid into the flow of water at a rate according to the quantity of water moving through the conduit, to thereby increase the relative acidity of the water and bring the pH level of the water into a predetermined range. In one embodiment of the invention, the predetermined range of pH levels is between approximately 5.5 and approximately 6.5, inclusive. (It should be understood that small variations outside of this range may also provide the benefits of the invention.) The first fluid may comprise an acid substance for increasing the relative acidity of the flow of water when injected into the flow of water, and thereby lowering the pH level of the water in the flow to a desirable level within a range of pH levels. The rate at which the first fluid is added or injected into the flow of water not only depends upon the rate at which the flow of water is moving through the conduit, but also upon the character of the particular substance being used as the first fluid. Typically, the supplier of the substance or product being used to lower the pH into the desired range will indicate the amount or rate at which the substance must be added to the flow of water to adjust the pH level of the untreated water to the desired pH level after the addition of the substance. One suitable substance for lowering the pH of the water flow is carbonyl diamide sulfate which is included in a product available under the tradename “VEROX ACTIVATOR” from The Verox Group, LLC, 45 Henderson Road, Beverly, Mass. 01915 or from Eagle Systems of Calhoun, Ga. Other substances or products may also be suitable for lowering the pH of the flow of water into the desired range of pH levels.
[0038] For example, the VEROX Activator product may be added to the flow of water at a rate of approximately 1 PPM to approximately 5 PPM. Generally, if a relatively higher concentration of the minerals and organisms is detected in the untreated water, then the rate of adding the VEROX Activator is preferably closer to 5 PPM, and if relatively lower concentrations of minerals and organisms is detected, then the rate of adding the VEROX Activator is preferably closer to 1 PPM.
[0039] The method of the invention may also include injecting the second fluid into the flow of water after the injection of the first fluid into the flow of water at a rate that corresponds to the rate water flow through the conduit. In one embodiment of the invention, the addition of the second fluid to the flow of water occurs at a location that is relatively close to the location of the addition of the first fluid, and may be at a location that is less than approximately one foot (approximately 30 cm) from the location of adding the first fluid, although a distance of up to approximately 100 cm may be used. The most preferred second fluid comprises sodium chlorite. The most preferred method of the invention contemplates adding the sodium chlorite to the flow water at a rate that exceeds the amount sodium chlorite that can be completely converted into chlorine dioxide (and other byproducts) so that a residual amount of sodium chlorite remains in the water at the point of use. The rate of adding sodium chlorite to achieve the desired residual will vary with the characteristics of the water, including the pH level to which the water is lowered, and may have to be repeatedly adjusted until the desired residual amount results in the treated water. In one preferred embodiment of the invention, the residual amount of chlorine dioxide in the water at the point of use is in the range of approximately 0.2 PPM to approximately 0.8 PPM. It has been found that this residual level of chlorine dioxide in the stomach of the user of the water helps to control bacteria in the stomach, including E - coli, salmonella, chrytosporidium, etc.
[0040] Finally, the method of the invention may also include the step of disturbing the flow of water through the conduit in a manner that produces mixing of the flow of water with the first and second fluids in the conduit to facilitate the conversion of sodium chlorite to chlorine dioxide.
[0041] With respect to the above description then, it is to be realized that the optimum dimensional relationships for the parts of the invention, to include variations in size, materials, shape, form, function and manner of operation, assembly and use, are deemed readily apparent and obvious to one skilled in the art, and all equivalent relationships to those illustrated in the drawings and described in the specification are intended to be encompassed by the present invention.
[0042] Therefore, the foregoing is considered as illustrative only of the principles of the invention. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the invention to the exact construction and operation shown and described, and accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope of the invention.
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A water treatment system for reducing the level of bacteria in a flow of water by creating an environment favorable for aerobic bacteria and unfavorable for anaerobic bacteria is disclosed. The system may include a method including intaking a flow of water, lowering a pH level of the flow of water to a predetermined range of pH levels, and adding sodium chlorite to the flow of water after lowering the pH level to the predetermined range of pH levels for producing chlorine dioxide. The sodium chlorite is added in an amount sufficient to produce a residual amount of sodium chlorite that does not produce chlorine dioxide, and the flow of water is outputted to the point of use with a residual amount of chlorine dioxide. The system may include an apparatus for carrying out the method of the invention.
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[0001] This application claims benefit from provisional application U.S. Ser. No. 60/026,004, filed Sep. 12, 1996.
BACKGROUND OF THE INVENTION
[0002] This invention relates to the use of nucleosomes for the treatment and prevention of cancer.
[0003] In the course of pursuing cures for cancer, researchers have attempted to evoke an effective anti-tumor immune response in individuals suffering from various forms of the disease. For this approach to succeed, one must first identify tumor antigens that effectively stimulate the immune system. Specific antigens for certain tumors, such as melanomas, have been identified (Darrow et.al., J. Immunol. 142:3329-3335, 1989; Cox et al., Science 264:716-719, 1994). Furthermore, human carcinoma-associated antigens, which can be recognized by T cells, have been described (Kantor et al., J. Natl. Cancer Inst. 84 :1084-1091, 1992; Ioannides et al., J. Immunol. 151:3696-3703, 1993; Tsang et al., J. Natl. Cancer Inst. 87:982-990, 1995). However, the number of tumors that can be treated by vaccination with preparations of specific antigens is extremely limited. To date, a vaccine effective against many different types of malignant cells has not been successfully realized.
SUMMARY OF THE INVENTION
[0004] The invention described herein is based on the discovery that antinuclear autoantibodies (ANAs) specifically bind nucleosomes that are present on the surface of tumor cells. These antibodies are so named because they recognize an antigen that is normally found in the nuclei of cells (“antinuclear”) and they can be self-produced (“autoantibodies”), for example in the elderly or in humans (or other animals) that have an autoimmune disease.
[0005] A monoclonal ANA, designated 2C5, was generated by standard techniques from the fusion of splenocytes obtained from a healthy, aged Balb/c mouse. This antibody was shown to react with the surface of a broad spectrum of tumor cells including those derived from human lymphoid tumors (e.g., MOLT-4, HEL 92.1.7, Raji, and U-937 cells) and non-lymphoid tumors (e.g., SK-BR3 cells (from an adenocarcinoma of the breast) and PC3 cells (from an adenocarcinoma of the prostate). Furthermore, 2C5 was shown to suppress the formation of a lymphoma in vivo. Therefore, the induction of such antibodies in vivo provides a means for preventing or treating neoplastic cell growth.
[0006] Accordingly, the invention features a method of treating neoplastic cell growth in a mammal, such as a human, by administering nucleosomes that elicit the production of antinuclear autoantibodies sufficient to inhibit neoplastic cell growth. The nucleosomes may be purified from eukaryotic cells or reconstituted in vitro, as described herein, using histones and mammalian or bacterial DNA. The nucleosomes can be administered in a substantially pure form in a physiologically acceptable carrier, diluent, or excipient, with or without an adjuvant. Alternatively, the nucleosomes can be liposome-encapsulated, for example, by the method described herein. Furthermore, administration may commence before or after the appearance of a tumor.
[0007] Also within the scope of the invention is a nucleosome-based composition for eliciting the production of antinuclear autoantibodies in a mammal. The composition consists of nucleosomes (which can be isolated from a eukaryotic cell or reconstituted in vitro) and a pharmaceutically acceptable carrier, diluent, or excipient. The reconstituted nucleosomes can contain either eukaryotic or bacterial DNA, and can be encapsulated in liposomes, for example, for administration as a vaccine.
[0008] The neoplastic cell growth prevented by or treated with the composition disclosed herein may be a malignant or benign growth. Malignant cell growth can give rise to lymphomas such as Burkitt's lymphoma, pre-B lymphoma, or histiocytic lymphoma, adenocarcinomas, for example of the breast, prostate, or kidney, erythroleukemia, thymomas, osteogenic sarcomas, hepatomas, melanomas, brain tumors, glial cell tumors, ovarian or uterine tumors, pancreatic tumors, or tumors within the stomach or gastrointestinal tract.
[0009] Individuals considered at risk for developing cancer may benefit particularly from the invention, primarily because prophylactic treatment can be begun before there is any evidence of a tumor. Individuals at risk include those with a genetic predisposition to one or more cancers and those who have been inadvertently exposed to nuclear radiation or a carcinogenic substance.
[0010] By “nucleosome” is meant any complex of histones and DNA including complete, naturally occurring nucleosomes, artificially prepared “reconstituted” nucleosomes, and antigenic portions of these nucleosomes. Nucleosomes are present naturally in the nuclei of eukaryotic cells and can be reconstituted, as described below, in vitro. Naturally occurring nucleosomes appear in sectioned tissue, when viewed with an electron microscope, as beadlike bodies on a string of DNA.
[0011] The term “reconstituted,” as used herein in reference to nucleosomes, refers to the process in which nucleosomes are artificially prepared by, for example, the salt step dialysis method described below.
[0012] Enhancing the anti-tumor potential of the immune system by immunizing the host with nucleosomes is advantageous in that it is expected to generate polyclonal antibodies that will recognize several determinants of tumor cell surface-bound nucleosomes. Thus, anti-nucleosomal autoantibodies should mediate the effector anti-tumor function of the host immune system more effectively than administration of an exogenous monoclonal antibody.
[0013] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, suitable methods and materials are described below. All publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety. In case of conflict, the present specification, including definitions, will control. In addition, the materials, methods, and examples are illustrative only and not intended to be limiting.
[0014] Other features and advantages of the invention will be apparent from the following detailed description, and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] [0015]FIG. 1 is a line graph depicting the selective reactivity of the monoclonal ANA 2C5 with a nucleosome-containing preparation of nucleohistones in an enzyme-linked immunosorbant assay (ELISA). The samples tested are represented on the graph as follows: nucleohistones as ▪, single-stranded DNA as O, double-stranded DNA as Δ, a mixture of individual histones as □, and ribonucleoprotein as X.
[0016] [0016]FIG. 2 is a line graph depicting the reactivity of the monoclonal ANA 2C5 to reconstituted nucleosomes. The samples tested are represented on the graph as follows: nucleosomes reconstituted in vitro from a DNA-histone mixture using step salt dialysis as ▪, similarly treated DNA as Δ, similarly treated histones as □, and a nucleosome-free DNA-histone mixture as O.
[0017] [0017]FIG. 3 is a bar graph depicting the humoral response in C57BL/6 mice to injected nucleosomes. An ELISA was performed using plasma samples obtained 0, 5, and 12 days following injection. The wells were sensitized with 50 μg/well double-stranded DNA (Bar A), 10 μg/well total histone (Bar B), or 10 μg/well nucleohistone (Bar C), and the optical density was determined (as shown on the y axis).
[0018] [0018]FIG. 4 is a bar graph depicting the MHC non-restricted cytotoxicity of mouse splenocytes against S49 lymphoma cells after immunization with nucleochromatin.
DETAILED DESCRIPTION
[0019] The data presented below demonstrate that nucleosomes are the target for tumoricidal ANAs and that immunization with nucleosomes can provide both humoral and cellular anti-tumor responses that increase the anti-tumor potential of the immune system. Thus, nucleosomes can serve as the basis of an anti-cancer vaccine.
[0020] The invention is based on the discovery that an antinuclear autoantibody (ANA), 2C5, which has been shown to dramatically inhibit the development of an aggressive cancer in vivo (Torchilin et al., WO 96/00084, hereby incorporated by reference), specifically binds to nucleosomes that are present on the surface of all tumor cells examined (Torchilin et al. supra; Iakoubov et al., Immunol. Lett. 47:147-149, 1995) but not on the surface of normal, non-malignant cells. This specificity is demonstrated by Western blot analysis and by an enzyme-linked immunosorbant assay (ELISA). The reactivity of 2C5 against various potential antigenic targets is reported in Table 1 and the results of an ELISA in which a panel of different nuclear antigens was tested, is shown in FIG. 1.
[0021] Two additional ANAs, referred to as 1G3 and 4D11, were also obtained from aged, healthy Balb/c mice, and similarly have been shown to bind the surface of both human and rodent tumor cells, but not normal cells. These data are shown below in Table 2.
[0022] To conduct the initial reactivity assay, ELISA plates (Corning, New York, N.Y.) were covered with potential targets including a nucleosome-containing preparation of nucleohistone, single-stranded DNA, double-stranded DNA, a mixture of individual histones, or ribonucleoprotein (10 μg/well in phosphate buffered saline (PBS), pH 7.2) for two hours. The plates were then washed and incubated for 30 minutes with a 10% solution of heat-inactivated bovine calf serum in PBS containing 0.1% Tween 20 (PBST). This procedure effectively prevents non-specific binding. Dilutions of 2C5 or of a control isotype-matched myeloma antibody UPC10 (in the same solution; Cappel, Durham, N.C.), were added in duplicate and incubated at room temperature for 60 minutes. The bound antibody was revealed by adding peroxidase-labeled goat anti-mouse antibodies followed by substrate; visualization of absorbed goat antibodies was performed using a solution of 0.05% orthophenylenediamine hydrochloride and 0.01% hydrogen peroxide as the substrate. The reaction was stopped by adding 2.5 M sulfuric acid (50 μl/well), and the optical density was read using a microplate ELISA reader (Fisher Scientific, Pittsburgh, Pa.). In each set of experiments, a limiting value, which was taken as the mean plus 3 times the standard error of the mean (SEM) was established to permit differentiation between positive (antigen-containing) and negative serum samples. As the serum titer, the maximum dilution is taken at which the optical density of positive sample is at least 3 times higher than that of the negative sample.
[0023] The data regarding the specificity of 2C5, which was collected from the ELISA described above and from standard Western blot analysis, is shown in Table 1. The absence of reactivity with a corresponding band in the Western blot and/or reactivity within 3 standard deviations from negative control in the ELISA is indicated in Table 1 by (−). A sample was scored as positive (+++) if the signal generated was more than 10 standard deviations from the negative control in the ELISA.
TABLE 1 Nuclear Autoantigens Other Potential Antiqens nucleohistone +++ myosin − ssDNA − β galactosidase − dsDNA − phosphorylase b − histones glutamic dehydrogenase − (individual and mixture) − lactate dehydrogenase − H1 peptide 144-159 − carbonic anhydrase − H1 peptide 204-218 − trypsin inhibitor − ribonucleoprotein − lysozyme − La/SS-B − aprotinin − Ro/SS-A − insulin − Sm − heparin − Jo-1 − dextran sulfate − scl-70 − heparin sulfate −
[0024] The monoclonal ANA 2C5 was also shown to possess nucleosome-restricted specificity when tested against reconstituted nucleosomes. Nucleosomes were reconstituted in vitro as described by Rhodes et al. ( Methods Enzymol. 170:575-585, 1989). Briefly, a mixture of individual histones (50 μg/ml of each histone (H1, H2A, H2B, H3, and H4); Boehringer Mannheim, Indianapolis, Ind.) were dissolved in distilled water with 100 μg/ml purified commercial bovine thymus or bacterial DNA (Sigma Chemical Co., St. Louis, Mo.). The solution was dialyzed against 2 M NaCl for 3 hours at 4° C., followed by stepwise dialysis to 0.15 M NaCl (decrements of 0.5 M NaCl over a period of 24 hours at 4° C.). All solutions contained 1 mM EDTA and 0.1 mM phenylmethylsulfonyl fluoride.
[0025] The ability of 2C5 to bind reconstituted nucleosomes was then tested. Varying concentrations of 2C5 (from approximately 0.005 to 5.0 μg/ml) were added to nucleosomes reconstituted in vitro from a DNA-histone mixture using step salt dialysis (as described above (▪)), and to similarly treated DNA (Δ), similarly treated histones (□), and a nucleosome-free DNA-histone mixture (O). A colored reaction product can be generated by tagging 2C5, for example with horseradish peroxidase, or by subsequently adding a tagged secondary antibody to the reaction. The result, as analyzed by reading the optical density (at A 450 ) is depicted in the line graph of FIG. 2. The ability of the 2C5 antibody to specifically bind reconstituted nucleosomes is evident by the steady increase in the optical density of the sample containing reconstituted nucleosomes with increasing concentrations of 2C5.
[0026] The ability of the ANAs 2C5, 1G3, and 4D11 to specifically bind a wide variety of human and rodent tumor cells has been demonstrated. These three ANAs were tested for their ability to bind human and rodent normal cells and human and rodent carcinomas, melanomas, sarcomas, leukemias, and lymphomas. Each of the three ANAs bound the human and rodent tumor cells, but not the normal cells. These data are shown in Table 2, where the reaction intensity is presented as a difference between flow cytometric peaks of monoclonal antibodies and a non-specific, control antibody, UPC10. The sample was scored as (+++) if the intensity was more than 3 logs from that obtained with UPC10, as (++) if the intensity was between 1.5 and 3 logs of that obtained with UPC10, (+) if the intensity was between 0.5 and 1.5 logs of that obtained with UPC10, and (−) if the intensity was less than 0.2 logs from that obtained with UPC10. Some samples were not determined (n/d).
TABLE 2 CELLS 2C5 1G3 4D11 Carcinomas: human breast ductal BT-474 +++ n/d ++ colon HT-29 ++ n/d n/d colon LS-174T ++ ++ n/d breast SK-BR-3 +++ n/d ++ adenocarcinoma breast ductal MDA-MB-134 ++ n/d n/d carcinoma prostate carcinoma DU145 +++ ++ n/d prostate PC3 +++ n/d n/d adenocarcinoma rodent lung LL/2 ++ ++ n/d squamous cell KLN205 ++ n/d n/d caracinoma Melanomas: human SK-MEL-5 + n/d n/d rodents B16 ++ n/d n/d Clone M-3 + n/d n/d Sarcomas: human osteogenic sarcoma U-20S +++ +++ n/d rodent osteogenic sarcoma UMR +++ n/d +++ Leukemias: human promyeloblastic HL60 + n/d n/d erythroleukemia HEL 92.1.7 ++ n/d n/d rodent L1210 + n/d n/d P383 ++ n/d n/d J774 ++ n/d n/d Lymphomas: human T lymphoma MOLT4 ++ ++ n/d Burkitt lymphoma Raji + n/d + Burkitt lymphoma Daudi + n/d n/d histocytic lymphoma U-937 + n/d n/d plasmocytoma RPMI 8226 ++ n/d n/d rodent T lymphoma YAC-1 +++ n/d n/d T lymphoma S49 ++ n/d + pre-B lymphoma 7OZ/3 ++ n/d n/d B lymphoma A20 +++ ++ n/d B lymphoma CH1 +++ n/d ++ myeloma P3X63-Ag.8.653 + ++ n/d plasmocytoma MOPC 315 ++ n/d n/d thymoma EL4 in culture ++ + ++ thymoma EL4 from tumor ++ n/d n/d Normal cells: human PBML from fresh blood − − n/d PBML in 24 hr cell − n/d − culture rodent splenocytes, Balb/c, − n/d − fresh lung cells, Balb/c, − − n/d fresh liver cells, Balb/c, − − − fresh
[0027] To determine whether the anti-tumor potential of the immune system can be increased in non-autoimmune adult mice, nucleosomes were prepared and used to immunize these animals as follows.
[0028] Preparation of Nucleosomes
[0029] Two types of nucleosomes, one containing mammalian DNA and mammalian histones, and the other containing bacterial DNA and mammalian histones, can be reconstituted in vitro using the standard procedure of step salt dialysis described above (see also Rhodes et al., Methods Enzymol. 170:575-585, 1989). Bacterial DNA itself can exhibit an adjuvant function due to the presence of hypomethylated CpG dinucleotides, which are much less characteristic of mammalian DNA (Krieg et al., Nature 374:546-549, 1995; for review, see Krieg, J. Clin. Immunol. 15:284-292, 1995). Thus, the mammalian immune response against immunogens containing bacterial DNA may be greater than-the response to mammalian DNA.
[0030] For subsequent immunization, both preparations can be further combined with an adjuvant, such as Freund's adjuvant, or incorporated into phosphatidyl choline (PC) or PC/cholesterol liposomes as described below.
[0031] Nucleosomes can be administered directly or first entrapped within liposomes, which are artificial phospholipid nanovesicles. Liposomes can be made, for example, of pure egg lecithin, or of a mixture of lecithin and cholesterol in a 7:3 molar ratio, by e.g., the reverse phase evaporation method of Szoka et al. ( Proc. Natl. Acad. Sci. USA 74:4191, 1978)). After the lipids are dried under argon and vacuum, the resulting film is dissolved in ether. For example, a film containing 16 mg of lecithin, with or without an appropriate quantity of cholesterol, is dissolved in 640 μl of ether, and supplemented with 100 to 500 μg of prepared nucleosomes (at 1 μg/μl) in phosphate buffered saline, pH 7.5. The mixture is then vortexed for 1 minute and treated in an ultrasound disintegrator (e.g., a Lab-Line Ultratip Labsonic System) at 40 W for 3-5 minutes at 4° C., and the ether is removed using a rotor evaporator.
[0032] Alternatively, nucleosomes can be entrapped within liposomes by dehydration-rehydration of vesicles according to Senior et al., Biochem. Biophys. Acta. 1003:58-62, 1989), or by prolonged co-sonication as described by Trubetskoy et al., FEBS Lett. 299:79-82, 1990). In the former procedure, 150 μl of pyrogen-free deionized water is added to the lipid film (prepared by solvent evaporation from a solution of one or more lipids in chloroform), and the film is resuspended in phosphate buffered saline, pH 7.5. Nucleosomes are incorporated by vigorous vortexing at a nucleosome:lipid weight ratio of 1:10. The final mixture is sonicated three times for one minute each at 0° C., under an argon flow, and then freeze-dried. The dry residue is reconstituted with 1 ml of pyrogen-free saline. In the latter procedure, the lipid film is resuspended in the presence of the same quantity of saline and nucleosomes by sonication for 35 to 40 minutes at 0° C., under argon flow.
[0033] The efficiency of the nucleosomal incorporation into liposomes can be determined by labeling the nucleosomes with fluorescein isothiocyanate (FITC, Sigma Chemical Co., St. Louis, Mo.) and subsequently separating the liposome-entrapped from the non-entrapped nucleosomes by Ficoll density gradient centrifugation. To accomplish this, 250 μl of a liposome-FITC-labeled nucleosome preparation is mixed vigorously with 60% Ficoll-400 in PBS (1:1 ratio, v:v), transferred to a plastic tube, and carefully layered from the top with 3 ml of a 40% Ficoll solution (in PBS) and 250 μl of PBS, without mixing the phases. The tube is then centrifuged at 35,000 rpm, for example in a Beckman ultracentrifuge, for 1 hour at −17° C. Liposomes with incorporated nucleosomes will partition into the upper layer, as will be evident from fluorescence intensity readings obtained before and after addition of a detergent, such as Triton X-100, to aliquots consisting of 10 successive fractions of 375 μl each.
[0034] The fluorescence of liposome-entrapped and non-entrapped nucleosomes can be determined, for example, using a Hitachi spectrofluorimeter, according to the manufacturer's instructions. The liposome-associated fluorescence intensity will also reflect the efficiency of nucleosome incorporation. If necessary, the composition of the liposomes can be varied to provide maximum nucleosome incorporation (see, e.g., Lesserman, Liposomes as Transporters of Oligonucleotides In “Liposomes as Tools in Basic Research and Industry,” pp. 215-223, J. R. Philippot and F. Schuber, Eds., CRC Press, 1995).
[0035] Entrapping nucleosomes within liposomes, which are then administered as described herein, offers additional advantages in that lipsomes are versatile and effective immunoadjuvants (Gregoriadis, Immunol. Today, p. 89-97, 1990; van Rooijen, Liposomes as Carrier and Immunoadjuvant of Vaccine Antigens, In “Bacterial Vaccines,” pp. 255-279, Alan R. Liss, Inc., 1990). They are considered versatile because their properties can be altered by altering their chemical and physical composition, and they have been proven effective; the immune response induced by an influenza antigen administered within liposomes was several fold greater than when administered with other adjuvants (Mbawnike et al., Vaccine 8:347-352, 1990). Furthermore, liposomes are biodegradable, non-immunogenic, less toxic and less irritating than conventional adjuvants, and they stimulate both humoral and cellular immune responses (Alving, J. Immunol. Meth. 140:1-13, 1991; Fries et al., Proc. Natl. Acad. Sci. USA 89:358-362, 1992).
[0036] Immunization
[0037] Rodents, such as C57BL/6 or Balb/c mice, can be immunized with different nucleosomal preparations, for example those combined with adjuvant or encapsulated in liposomes, according to the protocol disclosed by Mohan et al. ( J. Exp. Med. 177:1367-1381, 1993). The mice are injected intraperitoneally three times, at 2 week intervals, with nucleosomes or, as a control, with PBS. When Freund's adjuvant is used, the first injection consists of nucleosomes (10 μg in 50 μl PBS/mouse) or PBS (50 μl/mouse) mixed 1:1 with complete Freund's adjuvant (Gibco Laboratories, Gaithersburg, Md.), and the two subsequent injections are administered in incomplete Freund's adjuvant. When liposome-encapsulated nucleosomes are administered, all three injections can consist of the same antigen preparation, i.e., the quantity of nucleosomes and the volume of the injection are identical to that administered with Freund's adjuvant. When administering liposome-encapsulated nucleosomes, the negative control can be liposomes that do not contain nucleosomes.
[0038] Analysis of the Humoral Immune Response
[0039] The humoral component of the immune response can be tested, for example, 7 and 12 days following the first immunization, and 5 and 9 days after the second and third immunizations. The production of nucleosome-reactive and tumor cell surface-reactive antibodies of the IgM and IgG isotypes in blood samples of individual immunized mice is examined, as is the production of these antibodies in non-immunized mice or those immunized with either adjuvant alone or liposomes alone. The pattern of nucleosome-reactive antibodies is characterized in each case using different ELISA-based systems that allow different types of nucleosome-reactive antibodies to be quantified, particularly antibodies with DNA-, histone-, and nucleosome-restricted specificities.
[0040] Blood samples from immunized mice can be screened for the presence of ANAs as follows. Approximately 5 μl of blood plasma obtained from individual, immunized mice (obtained, e.g., as described above, 7 and 12 days following the first immunization, and 5 and 9 days after the second and third immunizations) are serially diluted in 10% calf bovine sera (in PBS). The diluted samples are then tested for nuclear reactivity, as evidenced by immunofluorescent staining of commercially available Hep-2 cells (Immunoconcepts, Sacramento, Calif.). Samples from non-immunized mice can be used as negative controls, and the 2C5 antibody can be used as a positive control. The Hep-2 cells are washed 5 times with PBS, and incubated in 10% calf bovine sera (in PBS; HyClone, Logan, Utah) with either the variously diluted plasma samples or mAb 2C5 for 15 minutes. The cells are then washed twice with PBS, incubated with working dilutions of FITC-labeled F(ab) 2 fragments of goat anti-mouse IgG (whole molecule; in PBS) with 1% bovine calf sera, and washed again with PBS. The humoral immune response of immunized animals can be assessed by comparing the intensity of Hep-2 staining produced by plasma samples from these animals with the staining produced by 2C5.
[0041] Aliquots of the same diluted plasma samples (from mice immunized with various nucleosomal preparations and from non-immunized mice) that were used to stain living cells can be used to stain fixed Hep-2 cells. Before beginning this analysis, cell viability should be determined, for example by the Trypan Blue exclusion test, and should be at least 95%. The cells are washed twice with Hank's Buffered Saline Solution (HBSS), incubated for 30 minutes with plasma from immunized mice, plasma from non-immunized mice, or the monoclonal antibody 2C5 (as a positive control, at 5 μg/ml in medium containing 10% bovine calf sera), and washed twice with HBSS. The cells are then stained for 30 minutes with FITC-labeled F(ab) 2 fragments of goat anti-mouse antibody diluted 1:100 in medium containing 1% bovine calf serum. After staining, the cells are washed twice with HBSS, and fixed with 4% paraformaldehyde in PBS. All incubations are performed at 20° C. The cells may be analyzed using FACScan (Becton Dickinson, Mountain View, Calif.) and live-gated using forward and 90° scatter to exclude debris and dead cells.
[0042] The early immune response to injection of nucleosomes was analyzed by ELISA, as follows. ELISA plates were sensitized with 50 μg/well of double-stranded DNA (Bar A in FIG. 3), 10 μg/well of total histone (Bar B in FIG. 3), or 10 μg/well of nucleohistone (Bar C in FIG. 3), washed in PBS with 0.1% Tween 20 (PBST) and incubated for 30 minutes with a 10% solution of heat-inactivated fetal calf serum in PBST to prevent non-specific binding. Plasma samples from immunized mice were diluted 1:100 in PBST and added in triplicate. After 1 hour of incubation at room temperature, the bound material was revealed by adding peroxidase-conjugated goat anti-mouse IgG for 1 hour (Cappel, Durham, NC; 1:1000 in PBST) followed by a solution of 2,2′-asino-bis(3-ethylbenz-thuazoline-6-sulfonic) acid in 0.05 M citrate buffer (pH 4.0). Hydrogen peroxide (0.01%) was used as the substrate to obtain a color reaction. The optical density of each sample was measured. As shown in FIG. 3, nucleohistones elicited the most effective immune response, with nucleosome-reactive antibodies appearing in the blood within 5 days of the initial immunization. As described herein, these antibodies specifically bind nucleosomes expressed on the surface of tumor cells but not on the surface of normal cells.
[0043] Analysis of the Cellular Immune Response
[0044] The effectiveness of the cellular immune response was also studied. The cellular component of the immune response, which is either MHC-restricted or MHC-non-restricted, can be tested by examining cellular cytotoxicity in in vitro assays in which splenocytes from immunized and control mice are used as effector cells, and 51-Cr-labeled EL4 T lymphoma cells and S49 T lymphoma cells are used as syngeneic or allogeneic targets. The tumor cells useful for studies of the cellular immune response include those from the EL4 lymphoma cell line, which originated in C57BL/6 mice treated with dimethyl benzanthracene. Inoculation with a small number of these cells leads to progressive tumor formation and subsequent death of all animals. Such aggressive tumorigenicity makes these tumor cells attractive as an experimental model. The S49 cells, which were used in the assay depicted in FIG. 4, are from a mouse lymphoma cell line that was established from a lymphoma induced in a Balb/c mouse by injection of phage and oil. These cells do not bear surface immunoglobulins.
[0045] Both EL4 T lymphoma and S49 cells are available from the American Type Culture Collection (A.T.C.C.; Rockville, Md.) under Accession Numbers TIB-39 and TIB-28, respectively.
[0046] MHC-non-restricted cytotoxicity of mouse splenocytes against S49 T lymphoma cells was demonstrated following immunization with nucleosomes, as follows. C57BL/6 mice were immunized intraperitoneally with nucleochromatin (100 μg/mouse) in complete Freund's adjuvant. Splenocytes were isolated on day 5, boosted in vitro (5% CO 2 . 37° C.) with 50 μg/ml of nucleochromatin for 24 hours and, after washing, added in triplicate to the wells of a round-bottomed 96-well plate containing 51-Cr-labeled S49 T lymphoma cells (E:T=20:1). After 8 hours of incubation, the released radioactivity was quantified in a γ-counter and the degree of cytotoxicity was determined as the % lysis, according to the formula:
% lysis = 100 × observed cpm - background cpm total cpm - background cpm
[0047] Significantly higher cytotoxicity of splenocytes from immunized mice (see column 3 of FIG. 4) versus mice injected with Freund's adjuvant alone (see column 1 and 2 of FIG. 4) was observed. The cytoxic effect could be partially inhibited when nucleosomes were present in the incubation medium throughout the experiment (columns 2 and 4 of FIG. 4).
[0048] Identification of the Cellular Subsets Responsible for Cytoxicity
[0049] To determine the mechanism and type of cellular immune response, the particular population of splenocytes must be determined. Therefore, the cytotoxicity of splenocytes from immunized mice should be tested after the depletion of different cellular subsets using complement-dependent lysis mediated by pan-T, pan-B, anti-CD4, anti-CD8, or anti-NK monoclonal antibodies (Boyle et al., J. Immunol. Meth. 15:135-146, 1977).
[0050] Analysis of the Effect of Nucleosome-based Immunization on Protection from Tumor Formation
[0051] Nucleosomal-based vaccines can be readily assessed for their effectiveness in cancer therapy. For this purpose, syngeneic tumor cells are administered to nucleosome-immunized C57BL/6 mice according to standard techniques. For example, 2×10 4 EL4 lymphoma cells are injected intraperitoneally or 2×10 6 B16.F10 melanoma cells are injected intravenously. The tumor-preventative effect of the immunization can be tested: (a) at the peak of the humoral IgG. antinucleosome response, (b) at the peak of the immunization-induced cellular cytotoxicity against tumor targets, and/or (c) when both components, humoral and cellular, are equally well presented. These data can be used to select an optimum protocol for immunization with nucleosomes.
[0052] B16.F10 melanoma cells are a derivative of B16 melanoma cells that have a highly metatastic potential for the lung and are available from the A.T.C.C. (Accession No. CRL-6322).
[0053] Analysis of the Effect of 2C5 Administration on the Development of a Human Tumor
[0054] To determine the effect of administration of the ANA 2C5 on human tumor cells, BT20 human breast carcinoma cells were implanted into nude mice subcutaneously and the animals were treated with four intravenous injections of 2C5 (75 μg/injection) every second day, starting on the day the tumor cells were administered. A group of control mice received similarly scheduled injections of the isotype-matched control antibody, UPC10. After 40 days, 75 percent of the treated mice were tumor-free, whereas every control mouse had developed a tumor. The average size of the tumor in the 25 percent of 2C5-treated mice that developed tumors, was only 10 to 15% as large as the tumors developed by mice that were not treated with 2C5.
[0055] Vaccination with Nucleosomes Protects Against Tumorigenesis
[0056] The effect of vaccinating mice (C57BL/6) with nucleosomes was tested using the following immunization protocol and two syngenic tumor models: EL4 T lymphoma and Lewis carcinoma. Mice were immunized with a nucleohistone preparation that contains mononucleosomes and oligonucleosomes (Sigma Chemical Co.) by intraperitoneal or subcutaneous injection, and then injected with tumor cells, as described below.
[0057] Two adjuvant protocols were used for the immunization. According to the first, nucleosomes were injected in incomplete Freunds adjuvant. According to the second, a mixture of nucleosomes and oligonucleotides containing nucleotide sequence from bacterial DNA was used (5 μg/mouse/injection). The oligonucleotides possessed strong adjuvant activity.
[0058] The mice were divided into two groups: an experimental group, in which mice were immunized with 100 μg of nucleosomes on day 0 and on day 9, and a control group that received a sham immunization consisting of PBS. Tumor cells were administered to the mice 9 days after the second immunization with nucleosomes, as follows. One group of experimental mice received an injection of EL4 T lymphoma cells (50,000 cells/mouse), and another group of experimental mice received an injection of Lewis carcinoma cells (250,000 cells/mouse). To avoid producing and observing simply a local effect, the nucleosomes and tumor cells were injected into different sites. That is, mice immunized by i.p. injection of nucleosomes received Lewis carcinoma cells by subcutaneous injection. Similarly, mice immunized by subcutaneous injection of nucleosomes received EL4 T lymphoma cells by i.p. injection.
[0059] Regardless of the route or site of administration, the development of tumors was strongly inhibited. On day 15, the average weight of the tumors that developed following administration of Lewis carcinoma cells in nucleosome-treated mice was less than one third the weight of tumors in untreated mice (i.e., PBS sham-immunized) mice. Tumors in untreated mice weighed 0.34±0.49 g, while tumors in mice treated with nucleosomes and incomplete Freunds adjuvant weighed 0.08±0.07 g, and tumors in mice treated with nucleosomes and oligonucleotides weighed 0.11±0.08 g. The development of EL4 T lymphoma was also strongly inhibited in immunized mice. In this instance, tumors in untreated mice weighed 3.3±0.49 g, but tumors in mice treated with nucleosomes and oligonucleotides weighed only 1.3±0.21 g.
[0060] Analysis of the Effect of Nucleosome-based Immunization on the Development of Established Tumors
[0061] Immunization with nucleosomes should also be effective when a tumor is already present in the host. To analyze this aspect of the invention, immunizations are performed when macroscopic tumor lesions have developed (for example, in mice on the 7th day after i.p. injection of EL4 T lymphoma cells or the 20th day after i.v. injection of B16 melanoma cells). The type of immunizing agent is chosen according to the humoral immune response and the subset of cells shown to be responsible for cytotoxicity.
[0062] Use
[0063] Skilled artisans will understand that any nuclear material that contains nucleosomes will elicit the production of antinuclear autoantibodies that specifically bind nucleosomes. This nuclear material includes, For example, nucleohistones, which are complex nucleoproteins that include the nucleosome and additional proteinaceous nuclear material, such as the DNA-binding proteins that function as transcription factors. Nuclear extract, nucleochromatin, or subnucleosomes, which are nucleosomes that have a structure that differs from that of naturally-occurring nucleosomes, can also elicit the generation of ANAs, and thus are considered within the scope of the invention.
[0064] In addition to the intraperitoneal route of administration described above, nucleosome-based vaccines can be administered intravenously, intramuscularly, transmucosally, or subcutaneously. These modes of administration can also be combined. For example, the first administration can be transmucosal and the subsequent administration can be intraperitoneal.
[0065] Vaccines can be administered in any pharmaceutically acceptable carrier or diluent, including water, normal saline, phosphate buffered saline, or a solution of bicarbonate such as 0.1 M NaHCO 3 . The carrier or diluent is selected on the basis of the mode and route of administration, and standard pharmaceutical practice. Additional suitable pharmaceutical carriers and diluents, as well as pharmaceutical necessities for their use in pharmaceutical formulations, are described, for example, in Remington's Pharmaceutical Sciences, a standard reference text in the field of pharmacology.
[0066] The amount of vaccine administered will depend on the particular vaccine antigen, whether an adjuvant is co-administered, the mode and frequency of administration, and the desired effect. Each of these considerations are understood by skilled artisans. In general, the vaccine antigen of the invention (the nucleosome) is administered in amounts ranging between, for example, 1 μg and 100 mg. If adjuvants are administered with the vaccines, amounts ranging from between, for example, 1 ng and 1 mg of antigen can be used. The dosage can also be calculated empirically, for example,. based on animal studies and, expressed in terms of a patient's weight, can range from 0.2 to 200 μg/kg.
[0067] Skilled artisans will recognize that the vaccine described herein can be administered in conjunction with other methods of treatment. For example, the vaccine can be administered before, during, or after administration of chemotherapeutic agents, radiation therapy, or surgical ablation of a malignant tumor or benign growth of cells.
OTHER EMBODIMENTS
[0068] A number of adjuvants, in addition to those described above, are known to skilled artisans and may be used to perform the immunization described herein. For example, cholera toxin (CT), the heat-labile enterotoxin of Escherichia coli (LT), or fragments or derivatives thereof having adjuvant activity, can be used for transmucosal administration. Alternatively, adjuvants such as RIBI (ImmunoChem, Hamilton, Vt.) or aluminum hydroxide can be used for parenteral administration.
[0069] Fusion proteins containing nucleosomes fused to an adjuvant (e.g., CT, LT, or a fragment or derivative thereof having adjuvant activity), are considered within the scope of the invention, and can be prepared using standard methods (see, e.g., Ausubel et al. “Current Protocols in Molecular Biology, Vol. I,” Green Publishing Associates, Inc., and John Wiley & Sons, Inc., NY, 1989). In addition, the vaccines of the invention can be covalently coupled or cross-linked to adjuvants. Methods of covalently coupling or chemically cross-linking adjuvants to antigens are described in, for example, Cryz et al. ( Vaccine 13:67-71, 1994), Liang et al. ( J. Immunol. 141:1495-1501, 1988), and Czerkinsky et al. (Infection and Immunity 57:1072-1077, 1989).
[0070] As stated above, the nucleosomes can be administered as a physiologically acceptable formulation containing an excipient. Examples of excipients which may be included with the formulation are buffers such as citrate buffer, phosphate buffer, acetate buffer, and bicarbonate buffer, amino acids, urea, alcohols, ascorbic acid, proteins, such as serum albumin and gelatin, EDTA, sodium chloride, polyvinylpyrollidone, mannitol, sorbitol, glycerol, propylene glycol, and polyethylene glycol (e.g., PEG-4000, PEG-6000).
[0071] It is to be understood that while the invention has been described in conjunction with the detailed description thereof, that the foregoing description is intended to illustrate and not limit the scope of the invention, which is defined by the scope of the appended claims. Other aspects, advantages, and modifications are within the scope of the following claims.
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A method of inhibiting neoplastic cell growth in a mammal by administering to the mammal nucleosomes that elicit the production of antinuclear autoantibodies sufficient to inhibit neoplastic cell growth.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application Ser. No. 61/254,236 filed on Oct. 23, 2009, which is hereby incorporated by reference in its entirety.
FIELD OF THE INVENTION
[0002] The present invention relates to novel 2-oxo-2H-chromene-3-carboxamide derivatives, processes for preparing them, pharmaceutical compositions containing them and their use as pharmaceuticals as modulators of sphingosine-1-phosphate receptors. The invention relates specifically to the use of these compounds and their pharmaceutical compositions to treat disorders associated with sphingosine-1-phosphate 1 (S1P1) receptor modulation.
BACKGROUND OF THE INVENTION
[0003] Sphingosine-1 phosphate is stored in relatively high concentrations in human platelets, which lack the enzymes responsible for its catabolism, and it is released into the blood stream upon activation of physiological stimuli, such as growth factors, cytokines, and receptor agonists and antigens. It may also have a critical role in platelet aggregation and thrombosis and could aggravate cardiovascular diseases. On the other hand the relatively high concentration of the metabolite in high-density lipoproteins (HDL) may have beneficial implications for atherogenesis. For example, there are recent suggestions that sphingosine-1-phosphate, together with other lysolipids such as sphingosylphosphorylcholine and lysosulfatide, are responsible for the beneficial clinical effects of HDL by stimulating the production of the potent antiatherogenic signaling molecule nitric oxide by the vascular endothelium. In addition, like lysophosphatidic acid, it is a marker for certain types of cancer, and there is evidence that its role in cell division or proliferation may have an influence on the development of cancers. These are currently topics that are attracting great interest amongst medical researchers, and the potential for therapeutic intervention in sphingosine-1-phosphate metabolism is under active investigation.
[0004] International patent application WO2008/092930 A1 discloses Chromene S1P1 receptor antagonists.
[0005] International patent application WO2007/115820 A1 discloses Chromen-2-one derivatives.
[0006] United States Patent Application Publication US2006/0148834 A1 discloses coumarin derivatives, their carboxamides, pharmaceutical compositions containing them and their uses.
SUMMARY OF THE INVENTION
[0007] We have now discovered a group of novel compounds which are potent and selective sphingosine-1-phosphate modulators. As such, the compounds described herein are useful in treating a wide variety of disorders associated with modulation of sphingosine-1-phosphate receptors. The term “modulator” as used herein, includes but is not limited to: receptor agonist, antagonist, inverse agonist, inverse antagonist, partial agonist, partial antagonist.
[0008] This document describes compounds of Formula I, which have sphingosine-1-phosphate receptor biological activity. The compounds in accordance with the present invention are thus of use in medicine, for example in the treatment of humans with diseases and conditions that are alleviated by S1P modulation, and in particular use as S1P1 agonists or antagonists (functional antagonists).
[0009] In one aspect the invention provides a compound having Formula I or a pharmaceutically acceptable salt thereof or stereoisomeric forms thereof, and the geometrical isomers, enantiomers, diastereoisomers, tautomers, zwitterions and pharmaceutically acceptable salts thereof:
[0000]
[0000] wherein:
[0010] R 1 is hydrogen, halogen or C 1-6 alkyl;
[0011] R 2 is CR 3 or N;
[0012] R 3 is hydrogen, halogen, O(C 1-6 alkyl), S(C 1-6 alkyl), cyano, aldehyde, heterocycle, C 1-6 alkyl or hydroxyl;
[0013] R 4 is CR 5 or N;
[0014] R 5 is hydrogen, halogen, hydroxyl or non-substituted C 1-6 alkyl;
[0015] R 6 is CR 7 or N;
[0016] R 7 is —NHR 12 , —S(O) 2 R 14 , —C(O)NHR 16 , —OR 17 , hydrogen, halogen, phosphonic acid, boronic acid, —CH 2 —OH, —CH 2 —S(O) 2 CH 3 , —(CH 2 ) a —NH—(CH 2 ) b —O c —P(O)(OH) 2 , —(CH 2 ) d —C(NH 2 )(CH 2 OH)(CH 2 —O—P(O)(OH) 2 ), —(CH 2 ) e —C(NH 2 )(CH 3 )(CH 2 —O—P(O)(OH) 2 ); or —(CH 2 ) f —NH—(CH 2 ) g —SO 3 H;
[0017] a is 1 or 2;
[0018] b is 2 or 3;
[0019] c is 0 or 1;
[0020] d is 0 or 1;
[0021] e is 0 or 1;
[0022] f is 0 or 1;
[0023] g is 2 or 3;
[0024] R 8 is CR 9 or N;
[0025] R 9 is hydrogen, halogen, non-substituted C 1-6 alkyl or hydroxyl;
[0026] R 10 is CR 11 or N;
[0027] R 11 is hydrogen, halogen or C 1-6 alkyl;
[0028] R 12 is hydrogen, C 1-6 alkyl, —C(O)R 13 , —S(O) 2 (C 1-3 alkyl) or heterocycle;
[0029] R 13 is amino or C 1-6 alkyl;
[0030] R 14 is C 1-4 alkyl, NHR 15 or hydroxyl;
[0031] R 15 is hydrogen or C 1-6 alkyl;
[0032] R 16 is hydrogen or C 1-6 alkyl;
[0033] R 17 is hydrogen, C 1-6 alkyl or —S(O) 2 (C 1-3 alkyl);
[0034] R 18 is C 2-4 alkyl or —OC 2-4 alkyl;
[0035] R 19 is hydrogen, halogen or C 1-6 alkyl;
[0036] R 20 is hydrogen, halogen or C 1-6 alkyl; and
[0037] R 21 is —OC 1-4 alkyl.
[0038] The term “alkyl”, as used herein, refers to saturated, monovalent or divalent hydrocarbon moieties having linear or branched moieties or combinations thereof and containing 1-8 carbon atoms, preferably 1-6 carbon atoms and more preferable 1-4 carbon atoms. One methylene (—CH 2 —) group, of the alkyl can be replaced by oxygen, sulfur, sulfoxide, nitrogen, carbonyl, carboxyl, sulfonyl, or by a divalent (C 3-6 cycloalkyl). Alkyl moieties can optionally be substituted by halogen, hydroxyl, cycloalkyl, amino, non-aromatic heterocycles, carboxylic acid, phosphonic acid groups, sulphonic acid groups, phosphoric acid. Usually, in the present case, alkyl groups are methyl, ethyl, iso-propyl, 1-methylsulfanyl, trifluoromethyl, methylsulfanyl, isopropyldifluoro, n-propyl, propylsulphonic acid, 1,1,1,2,2 pentafluoroethyl, 3(ethylamino)cyclobutylphosphonic acid. Preferred alkyl groups are methyl, ethyl, n-propyl, iso-propyl, trifluoromethyl.
[0039] The term “cycloalkyl”, as used herein, refers to a monovalent or divalent group of 3 to 8 carbon atoms, preferably 3-6 carbon atoms derived from a saturated cyclic hydrocarbon. Cycloalkyl can be optionally substituted by C 1-3 alkyl groups or halogen. Usually, in the present case, cycloalkyl groups are cyclohexyl, methylcyclopropyl, cyclobutyl.
[0040] The term “halogen”, as used herein, refers to an atom of chlorine, bromine, fluorine, iodine. Usually, in the present case, halogens are chlorine, fluorine, bromine.
[0041] The term “heterocycle” as used herein, refers to a 3 to 10 membered ring, containing at least one heteroatom selected form O or N or S or combinations of at least two thereof interrupting the carbocyclic ring structure. The heterocyclic ring can be saturated or non-saturated. The heterocyclic ring can be interrupted by a C═O, the S heteroatom can be oxidized. Heterocyclic ring moieties can optionally be substituted by hydroxyl, C 1-3 alkyl or halogen. Usually heterocyclic groups in the present case are piperidyl, pyrryl, furyl.
[0042] The term “aryl” as used herein, is defined as including an organic moiety derived from an aromatic hydrocarbon consisting of a ring containing 6 to 10 carbon atoms by removal of one hydrogen, which can optionally be substituted by 1 to 3 halogen atoms or by 1 to 2 C 1-3 alkyl groups. Usually aryl is phenyl.
[0043] The term “hydroxyl” as used herein, represents a group of formula “—OH”.
[0044] The term “carbonyl” as used herein, represents a group of formula “—C═O”.
[0045] The term “carboxyl” as used herein, represents a group of formula “—C(O)O—”.
[0046] The term “cyano” as used herein, represents a group of formula “—CN”.
[0047] The term “aldehyde” as used herein, represents a group of formula “—C(O)H”.
[0048] The term “sulfonyl” as used herein, represents a group of formula “—SO 2 ”.
[0049] The term “sulfate” as used herein, represents a group of formula “—O—S(O) 2 —O—”.
[0050] The term “carboxylic acid” as used herein, represents a group of formula “—C(O)OH”.
[0051] The term “sulfoxide” as used herein, represents a group of formula “—S═O”.
[0052] The term “phosphonic acid” as used herein, represents a group of formula “—P(O)(OH) 2 ”.
[0053] The term “phosphoric acid” as used herein, represents a group of formula “—(O)P(O)(OH) 2 ”.
[0054] The term “boronic acid”, as used herein, represents a group of formula “—B(OH) 2 ”.
[0055] The term “sulphonic acid” as used herein, represents a group of formula “—S(O) 2 OH”.
[0056] The term “modulator” as used herein, represents receptor agonist, antagonist, inverse agonist, inverse antagonist, partial agonist, partial antagonist.
[0057] Generally R 1 is hydrogen, halogen, C 1-6 alkyl. Usually R 1 is hydrogen.
[0058] Generally R 2 is CR 3 or N. Usually R 2 is CR 3 .
[0059] Generally R 3 is hydrogen, halogen, O(C 1-6 alkyl), S(C 1-6 alkyl), cyano, aldehyde, heterocycle, C 1-6 alkyl or hydroxyl. Usually R 3 is hydrogen, CF 3 , Br, Cl, OMe, Me, OCHF 2 , OCF 3 , SMe, furyl, —C(O)H, Ethyl, cyano or n-Propyl.
[0060] Generally R 4 is CR 5 or N.
[0061] Generally R 5 is hydrogen, halogen, non-substituted C 1-6 alkyl or hydroxyl. Usually R 5 is hydrogen, fluoro or methyl.
[0062] Generally R 6 is CR 7 or N.
[0063] Generally R 7 is —NHR 12 , —S(O) 2 R 14 , —C(O)NHR 16 , —OR 17 , hydrogen, halogen, phosponic acid, boronic acid, —CH 2 —OH, —CH 2 —S(O) 2 CH 3 , —(CH 2 ) a —NH—(CH 2 ) b —O c —P(O)(OH) 2 , —(CH 2 ) d —C(NH 2 )(CH 2 OH)(CH 2 —O—P(O)(OH) 2 ), —(CH 2 ) e —C(NH 2 )(CH 3 )(CH 2 —O—P(O)(OH) 2 ) or (CH 2 ) f —NH—(CH 2 ) g —SO 3 H.
[0064] Usually R 7 is —NH—S(O) 2 CH 3 , hydrogen, —S(O) 2 NH 2 , hydroxyl, C(O)NH 2 , CH 2 OH, CH 2 —S(O) 2 CH 3 , phosponic acid or boronic acid.
[0065] Generally a is 1 or 2.
[0066] Generally b is 2 or 3.
[0067] Generally c is 0 or 1.
[0068] Generally d is 0 or 1.
[0069] Generally e is 0 or 1.
[0070] Generally f is 0 or 1.
[0071] Generally g is 2 or 3.
[0072] Generally R 8 is CR 9 or N.
[0073] Generally R 9 is hydrogen, halogen, non-substituted C 1-6 alkyl or phosponic acid, boronic acid. Usually R 9 is hydrogen, fluoro or methyl.
[0074] Generally R 10 is CR 11 or N.
[0075] Generally R 11 is hydrogen, halogen or C 1-6 alkyl. Usually R 11 is hydrogen, chloro or methyl.
[0076] Generally R 12 is hydrogen, C 1-6 alkyl, —C(O)R 13 , —S(O) 2 (C 1-3 alkyl), heterocycle. Usually R 12 is hydrogen, S(O) 2 (methyl), —C(O)CH(NH 2 )CH 2 —COOH, C(O)CH 3 , pyroyl or piperidinyl.
[0077] Generally R 13 is amino, C 1-6 alkyl. Usually R 13 is amino, methyl, —CH(NH 2 )CH 2 COOH.
[0078] Generally R 14 is C 1-4 alkyl, —NHR 15 or hydroxyl. Usually R 14 is amino, —NH(CH 2 ) 2 COOH.
[0079] Generally R 15 is hydrogen, C 1-6 alkyl. Usually R 15 is H, methyl, —CH 2 -heterocycle, —(CH 2 ) 2 —COOH or —CH 2 —P(O)(OH) 2 .
[0080] Generally R 16 is hydrogen or C 1-6 alkyl. Usually R 16 is hydrogen,
[0081] Generally R 17 is hydrogen, C 1-6 alkyl or —S(O) 2 (C 1-3 alky). Usually R 17 is hydrogen, —S(O) 2 CH 3 .
[0082] Generally R 18 is C 2-4 alkyl or —OC 2-4 alkyl. Usually R 18 is methyl, n-propyl, O-ethyl or O-isopropyl.
[0083] Generally R 19 is hydrogen, halogen or C 1-6 alkyl. Usually R 19 is hydrogen.
[0084] Generally R 20 is hydrogen, halogen or C 1-6 alkyl. Usually R 20 is hydrogen.
[0085] Generally R 21 is —OC 1-4 alkyl. Usually R 21 is O-methyl or O-ethyl.
[0086] In one embodiment of the invention
[0087] R 1 is hydrogen; and
[0088] R 2 is CR 3 ; and
[0089] R 3 is halogen, O(C 1-6 alkyl), S(C 1-6 alkyl), cyano, aldehyde, heterocycle, C 1-6 alkyl; and
[0090] R 4 is CR 5 or N; and
[0091] R 5 is hydrogen or halogen; and
[0092] R 6 is CR 7 or N; and
[0093] R 7 is —NHR 12 , —S(O) 2 R 14 , —OR 17 , hydrogen, phosphonic acid, boronic acid, —CH 2 —OH, —CH 2 —S(O) 2 CH 3 ; and
[0094] R 8 is CR 9 or N; and
[0095] R 9 is hydrogen, halogen or non-substituted C 1-6 alkyl; and
[0096] R 10 is CR 11 ; and
[0097] R 11 is hydrogen, halogen or C 1-6 alkyl; and
[0098] R 12 is —S(O) 2 (C 1-3 alkyl), C(O)R 13 or heterocycle; and
[0099] R 13 is C 1-6 alkyl; and
[0100] R 14 is NHR 15 ; and
[0101] R 15 is hydrogen or C 1-6 alkyl; and
[0102] R 16 is C 1-6 alkyl; and
[0103] R 17 is hydrogen, or —S(O) 2 (C 1-3 alkyl); and
[0104] R 18 is C 2-4 alkyl or —OC 2-4 alkyl; and
[0105] R 19 is hydrogen; and
[0106] R 20 is hydrogen; and
[0107] R 21 is —OC 1-4 alkyl.
[0108] In another embodiment of the invention
[0109] R 1 is hydrogen; and
[0110] R 2 is CR 3 ; and
[0111] R 3 is halogen, O(C 1-6 alkyl), C 1-6 alkyl; and
[0112] R 4 is CR 5 or N; and
[0113] R 5 is hydrogen; and
[0114] R 6 is CR 7 or N; and
[0115] R 7 is —NHR 12 , —S(O) 2 R 14 , —OR 17 , hydrogen, phosphonic acid or boronic acid; and
[0116] R 8 is CR 9 ; and
[0117] R 9 is hydrogen; and
[0118] R 10 is CR 11 ; and
[0119] R 11 is hydrogen or C 1-6 alkyl; and
[0120] R 12 is —S(O) 2 (C 1-3 alkyl) or C(O)R 13 ; and
[0121] R 13 is C 1-6 alkyl; and
[0122] R 14 is NHR 15 ; and
[0123] R 15 is hydrogen; and
[0124] R 17 is hydrogen; and
[0125] R 18 is C 2-4 alkyl or —OC 2-4 alkyl; and
[0126] R 19 is hydrogen; and
[0127] R 20 is hydrogen; and
[0128] R 21 is —OC 1-4 alkyl.
[0129] Compounds of the invention are:
[0130] N-[4-(hydroxymethyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0131] N-[4-(aminosulfonyl)-2-methylphenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0132] N-[4-(aminosulfonyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0133] N-[4-(aminosulfonyl)-2-bromophenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0134] N-[4-(aminosulfonyl)-2-chlorophenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0135] N-(4-amino-2-methylphenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0136] 7-methoxy-N-{2-methyl-4-[(methylsulfonyl)amino]phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0137] N-{4-[(ethylsulfonyl)amino]-2-methylphenyl}-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0138] N-[4-(acetylamino)-2-methylphenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0139] 7-methoxy-N-{2-methoxy-4-[(methylsulfonyl)amino]phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0140] 3-{[(4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)sulfonyl]amino}propanoic acid;
[0141] N-(2-chlorophenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0142] 7-methoxy-2-oxo-N-[4-(piperidin-3-ylamino)phenyl]-8-propyl-2H-chromene-3-carboxamide;
[0143] 7-methoxy-2-oxo-8-propyl-N-[4-(pyrrolidin-3-ylamino)phenyl]-2H-chromene-3-carboxamide;
[0144] 7-methoxy-2-oxo-N-{4-[(piperidin-2-ylmethyl)amino]phenyl}-8-propyl-2H-chromene-3-carboxamide;
[0145] 7-methoxy-2-oxo-N-{4-[(piperidin-3-ylmethyl)amino]phenyl}-8-propyl-2H-chromene-3-carboxamide;
[0146] 7-methoxy-N-(2-methylphenyl)-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0147] N-(2-cyanophenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0148] 7-methoxy-N-{4-[(methylsulfonyl)amino]-2-(trifluoromethyl)phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0149] 7-methoxy-N-{2-methyl-4-[(methylamino)sulfonyl]phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0150] 7-methoxy-N-[2-(methylthio)phenyl]-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0151] 7-methoxy-2-oxo-8-propyl-N-[2-(trifluoromethoxy)phenyl]-2H-chromene-3-carboxamide;
[0152] N-[2-(2-furyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0153] N-(3-fluoro-2-methylphenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0154] N-(2-fluorophenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0155] N-(2-chloropyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0156] N-(2-ethylphenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0157] 7-methoxy-N-(2-methoxyphenyl)-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0158] 7-methoxy-2-oxo-8-propyl-N-[2-(trifluoromethyl)phenyl]-2H-chromene-3-carboxamide;
[0159] N-(2-bromophenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0160] N-(4-hydroxy-2-methylphenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0161] 4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl methanesulfonate;
[0162] N-[2-(difluoromethoxy)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0163] N-(3-bromopyridin-4-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0164] N-(3-chloropyridin-4-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0165] 7-methoxy-N-(2-methoxypyridin-3-yl)-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0166] N-(2-chloro-5-methylpyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0167] N-(2-bromopyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0168] 7-methoxy-2-oxo-8-propyl-N-(2-propylphenyl)-2H-chromene-3-carboxamide;
[0169] N-(6-amino-2-methylpyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0170] N-[4-(acetylamino)-2-(trifluoromethyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0171] N-(2-ethylpyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0172] 7-methoxy-N-{2-methyl-6-[(methylsulfonyl)amino]pyridin-3-yl}-2-oxo-8-propyl- 2H-chromene-3-carboxamide;
[0173] 7-methoxy-2-oxo-8-propyl-N-pyridin-4-yl-2H-chromene-3-carboxamide;
[0174] 7-methoxy-N-(3-methylpyridin-4-yl)-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0175] 7-methoxy-2-oxo-8-propyl-N-[3-(trifluoromethyl)pyridin-4-yl]-2H-chromene-3-carboxamide;
[0176] 7-methoxy-2-oxo-8-propyl-N-pyridin-3-yl-2H-chromene-3-carboxamide;
[0177] N-[4-hydroxy-2-(trifluoromethyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0178] 7-methoxy-2-oxo-8-propyl-N-[2-(trifluoromethyl)pyridin-3-yl]-2H-chromene-3-carboxamide;
[0179] 7-methoxy-N-(3-methylpyridin-2-yl)-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0180] 7-methoxy-N-(2-methylpyridin-3-yl)-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0181] N-(2-formylpyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0182] N-(3-chloropyridazin-4-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0183] (3-chloro-4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}phenyl)boronic acid;
[0184] N-(2-chloro-5-fluoropyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0185] (4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)phosphonic acid;
[0186] N-[4-(aminosulfonyl)-2-(trifluoromethyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0187] (3S)-3-amino-4-[(4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)amino]-4-oxobutanoic acid;
[0188] 8-isopropoxy-7-methoxy-2-oxo-N-[2-(trifluoromethyl)pyridin-3-yl]-2H-chromene-3-carboxamide;
[0189] 8-isopropoxy-7-methoxy-N-(2-methylpyridin-3-yl)-2-oxo-2H-chromene-3-carboxamide;
[0190] 8-ethoxy-7-methoxy-N-(2-methylpyridin-3-yl)-2-oxo-2H-chromene-3-carboxamide;
[0191] 8-ethoxy-7-methoxy-2-oxo-N-[2-(trifluoromethyl)pyridin-3-yl]-2H-chromene-3-carboxamide;
[0192] 8-ethoxy-7-methoxy-2-oxo-N-[2-(trifluoromethyl)phenyl]-2H-chromene-3-carboxamide;
[0193] 8-isopropoxy-7-methoxy-2-oxo-N-[2-(trifluoromethyl)phenyl]-2H-chromene-3-carboxamide;
[0194] 7-methoxy-N-{2-methyl-4-[(methylsulfonyl)methyl]phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0195] N-{2-chloro-4-[(methylsulfonyl)amino]phenyl}-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0196] (4R)-4-amino-5-[(4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)amino]-5-oxopentanoic acid;
[0197] N-[4-(aminosulfonyl)-2-methylphenyl]-7,8-diethoxy-2-oxo-2H-chromene-3-carboxamide;
[0198] N-[4-(aminosulfonyl)-2-methylphenyl]-8-ethoxy-7-methoxy-2-oxo-2H-chromene-3-carboxamide;
[0199] N-[4-(aminosulfonyl)-2-methylphenyl]-8-isopropoxy-7-methoxy-2-oxo-2H-chromene-3-carboxamide;
[0200] 7,8-diethoxy-N-{4-[(methylsulfonyl)amino]-2-(trifluoromethyl)phenyl}-2-oxo-2H-chromene-3-carboxamide;
[0201] N-[4-(aminosulfonyl)-2-methylphenyl]-8-ethyl-7-methoxy-2-oxo-2H-chromene-3-carboxamide.
[0202] Preferred compounds of the invention are:
[0203] 7-methoxy-2-oxo-8-propyl-N-[2-(trifluoromethyl)phenyl]-2H-chromene-3-carboxamide;
[0204] N-(3-bromopyridin-4-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0205] N-(2-bromophenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0206] 7-methoxy-2-oxo-8-propyl-N-[3-(trifluoromethyl)pyridin-4-yl]-2H-chromene-3-carboxamide;
[0207] N-(3-chloropyridin-4-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0208] 8-ethoxy-7-methoxy-2-oxo-N-[2-(trifluoromethyl)pyridin-3-yl]-2H-chromene-3-carboxamide;
[0209] N-(2-ethylphenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0210] (4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)phosphonic acid;
[0211] (3-chloro-4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}phenyl)boronic acid;
[0212] 7-methoxy-2-oxo-8-propyl-N-[2-(trifluoromethoxy)phenyl]-2H-chromene-3-carboxamide;
[0213] N-[2-(difluoromethoxy)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0214] N-[4-(aminosulfonyl)-2-methylphenyl]-8-isopropoxy-7-methoxy-2-oxo-2H-chromene-3-carboxamide;
[0215] N-[4-(aminosulfonyl)-2-methylphenyl]-8-ethoxy-7-methoxy-2-oxo-2H-chromene-3-carboxamide;
[0216] N-[4-(aminosulfonyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0217] N-[4-(acetylamino)-2-methylphenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0218] 7-methoxy-2-oxo-8-propyl-N-[2-(trifluoromethyl)pyridin-3-yl]-2H-chromene-3-carboxamide;
[0219] N-(2-bromopyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0220] N-(2-ethylpyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0221] 7-methoxy-N-(2-methylpyridin-3-yl)-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0222] 7-methoxy-N-{4-[(methylsulfonyl)amino]-2-(trifluoromethyl)phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0223] 7,8-diethoxy-N-{4-[(methylsulfonyl)amino]-2-(trifluoromethyl)phenyl}-2-oxo-2H-chromene-3-carboxamide;
[0224] N-[4-(aminosulfonyl)-2-bromophenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0225] N-[4-(aminosulfonyl)-2-chlorophenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0226] 7-methoxy-N-{2-methyl-4-[(methylsulfonyl)amino]phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0227] 7-methoxy-N-{2-methyl-6-[(methylsulfonyl)amino]pyridin-3-yl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0228] 7-methoxy-N-{2-methoxy-4-[(methylsulfonyl)amino]phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0229] N-[4-(aminosulfonyl)-2-methylphenyl]-7,8-diethoxy-2-oxo-2H-chromene-3-carboxamide;
[0230] 7-methoxy-N-(2-methoxypyridin-3-yl)-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0231] N-{4-[(ethylsulfonyl)amino]-2-methylphenyl}-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0232] N-[4-(acetylamino)-2-(trifluoromethyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0233] N-(4-hydroxy-2-methylphenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0234] (3S)-3-amino-4-[(4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)amino]-4-oxobutanoic acid;
[0235] N-(2-chloropyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0236] (4R)-4-amino-5-[(4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)amino]-5-oxopentanoic acid;
[0237] N-[4-(aminosulfonyl)-2-methylphenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0238] N-[4-hydroxy-2-(trifluoromethyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide.
[0239] Most preferred compounds of the invention are:
[0240] 7-methoxy-2-oxo-8-propyl-N-[2-(trifluoromethyl)pyridin-3-yl]-2H-chromene-3-carboxamide;
[0241] N-(2-bromopyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0242] N-(2-ethylpyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0243] 7-methoxy-N-(2-methylpyridin-3-yl)-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0244] 7-methoxy-N-{4-[(methylsulfonyl)amino]-2-(trifluoromethyl)phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0245] 7,8-diethoxy-N-{4-[(methylsulfonyl)amino]-2-(trifluoromethyl)phenyl}-2-oxo-2H-chromene-3-carboxamide;
[0246] N-[4-(aminosulfonyl)-2-bromophenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0247] N-[4-(aminosulfonyl)-2-chlorophenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0248] 7-methoxy-N-{2-methyl-4-[(methylsulfonyl)amino]phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0249] 7-methoxy-N-{2-methyl-6-[(methylsulfonyl)amino]pyridin-3-yl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0250] 7-methoxy-N-{2-methoxy-4-[(methylsulfonyl)amino]phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0251] N-[4-(aminosulfonyl)-2-methylphenyl]-7,8-diethoxy-2-oxo-2H-chromene-3-carboxamide;
[0252] 7-methoxy-N-(2-methoxypyridin-3-yl)-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0253] N-{4-[(ethylsulfonyl)amino]-2-methylphenyl}-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0254] N-[4-(acetylamino)-2-(trifluoromethyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0255] N-(4-hydroxy-2-methylphenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0256] (3S)-3-amino-4-[(4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)amino]-4-oxobutanoic acid;
[0257] N-(2-chloropyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0258] (4R)-4-amino-5-[(4-{[(7-methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)amino]-5-oxopentanoic acid;
[0259] N-[4-(aminosulfonyl)-2-methylphenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide;
[0260] N-[4-hydroxy-2-(trifluoromethyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide.
[0261] Some compounds of Formula I and some of their intermediates have at least one stereogenic center in their structure. This stereogenic center may be present in an R or S configuration, said R and S notation is used in correspondence with the rules described in Pure Appli. Chem. (1976), 45, 11-13.
[0262] The term “pharmaceutically acceptable salts” refers to salts or complexes that retain the desired biological activity of the above identified compounds and exhibit minimal or no undesired toxicological effects. The “pharmaceutically acceptable salts” according to the invention include therapeutically active, non-toxic base or acid salt forms, which the compounds of Formula I are able to form.
[0263] The acid addition salt form of a compound of Formula I that occurs in its free form as a base can be obtained by treating the free base with an appropriate acid such as an inorganic, for example, a hydrohalic such as hydrochloric acid, hydrobromic acid, sulfuric acid, phosphoric acid, nitric acid and the like; or an organic acid such as for example, acetic, hydroxyacetic, propanoic, lactic, pyruvic, malonic, fumaric acid, maleic acid, oxalic acid, tartaric acid, succinic acid, malic acid, ascorbic acid, benzoic acid, tannic acid, pamoic acid, citric, methylsulfonic, ethanesulfonic, benzenesulfonic, formic and the like (Handbook of Pharmaceutical Salts, P. Heinrich Stahal & Camille G. Wermuth (Eds), Verlag Helvetica Chemica Acta-Zürich, 2002, 329-345).
[0264] Compounds of Formula I and their salts can be in the form of a solvate, which is included within the scope of the present invention. Such solvates include for example hydrates, alcoholates and the like.
[0265] With respect to the present invention reference to a compound or compounds, is intended to encompass that compound in each of its possible isomeric forms and mixtures thereof unless the particular isomeric form is referred to specifically.
[0266] Compounds according to the present invention may exist in different polymorphic forms. Although not explicitly indicated in the above formula, such forms are intended to be included within the scope of the present invention.
[0267] The compounds of the invention are indicated for use in treating or preventing conditions in which there is likely to be a component involving the sphingosine-1-phosphate receptors.
[0268] In another embodiment, there are provided pharmaceutical compositions including at least one compound of the invention in a pharmaceutically acceptable carrier.
[0269] In a further embodiment of the invention, there are provided methods for treating disorders associated with modulation of sphingosine-1-phosphate receptors. Such methods can be performed, for example, by administering to a subject in need thereof a pharmaceutical composition containing a therapeutically effective amount of at least one compound of the invention.
[0270] These compounds are useful for the treatment of mammals, including humans, with a range of conditions and diseases that are alleviated by S1P1 modulation: not limited to the treatment of diabetic retinopathy, other retinal degenerative conditions, dry eye, angiogenesis and wounds.
[0271] Therapeutic utilities of S1P1 agonists are ocular disease, such as but not limited to: wet and dry age-related macular degeneration, diabetic retinopathy, retinopathy of prematurity, retinal edema, geographic atrophy, glaucomatous optic neuropathy, chorioretinopathy, hypertensive retinopathy, ocular ischemic syndrome, prevention of inflammation-induced fibrosis in the back of the eye, various ocular inflammatory diseases including uveitis, scleritis, keratitis, and retinal vasculitis; or systemic vascular barrier related diseases such as but not limited to: various inflammatory diseases, including acute lung injury, its prevention, sepsis, tumor metastasis, atherosclerosis, pulmonary edemas, and ventilation-induced lung injury; or autoimmune diseases and immunosuppression such as but not limited to: rheumatoid arthritis, Crohn's disease, Graves' disease, inflammatory bowel disease, multiple sclerosis, Myasthenia gravis, Psoriasis, ulcerative colitis, autoimmune uveitis, renal ischemia/perfusion injury, contact hypersensitivity, atopic dermititis, and organ transplantation; or allergies and other inflammatory diseases such as but not limited to: urticaria, bronchial asthma, and other airway inflammations including pulmonary emphysema and chronic obstructive pulmonary diseases; or cardiac protection such as but not limited to: ischemia reperfusion injury and atherosclerosis; or wound healing such as but not limited to: scar-free healing of wounds from cosmetic skin surgery, ocular surgery, GI surgery, general surgery, oral injuries, various mechanical, heat and burn injuries, prevention and treatment of photoaging and skin ageing, and prevention of radiation-induced injuries; or bone formation such as but not limited to: treatment of osteoporosis and various bone fractures including hip and ankles; or anti-nociceptive activity such as but not limited to: visceral pain, pain associated with diabetic neuropathy, rheumatoid arthritis, chronic knee and joint pain, tendonitis, osteoarthritis, neuropathic pains.
[0272] In still another embodiment of the invention, there are provided methods for treating disorders associated with modulation of sphingosine-1-phosphate receptors. Such methods can be performed, for example, by administering to a subject in need thereof a therapeutically effective amount of at least one compound of the invention, or any combination thereof, or pharmaceutically acceptable salts, hydrates, solvates, crystal forms and individual isomers, enantiomers, and diastereomers thereof.
[0273] The present invention concerns the use of a compound of Formula I or a pharmaceutically acceptable salt thereof, for the manufacture of a medicament for the treatment of ocular disease, wet and dry age-related macular degeneration, diabetic retinopathy, retinopathy of prematurity, retinal edema, geographic atrophy, glaucomatous optic neuropathy, chorioretinopathy, hypertensive retinopathy, ocular ischemic syndrome, prevention of inflammation-induced fibrosis in the back of the eye, various ocular inflammatory diseases including uveitis, scleritis, keratitis, and retinal vasculitis; or systemic vascular barrier related diseases, various inflammatory diseases, including acute lung injury, its prevention, sepsis, tumor metastasis, atherosclerosis, pulmonary edemas, and ventilation-induced lung injury; or autoimmune diseases and immunosuppression, rheumatoid arthritis, Crohn's disease, Graves' disease, inflammatory bowel disease, multiple sclerosis, Myasthenia gravis, Psoriasis, ulcerative colitis, autoimmune uveitis, renal ischemia/perfusion injury, contact hypersensitivity, atopic dermititis, and organ transplantation; or allergies and other inflammatory diseases, urticaria, bronchial asthma, and other airway inflammations including pulmonary emphysema and chronic obstructive pulmonary diseases; or cardiac protection, ischemia reperfusion injury and atherosclerosis; or wound healing, scar-free healing of wounds from cosmetic skin surgery, ocular surgery, GI surgery, general surgery, oral injuries, various mechanical, heat and burn injuries, prevention and treatment of photoaging and skin ageing, and prevention of radiation-induced injuries; or bone formation, treatment of osteoporosis and various bone fractures including hip and ankles; or anti-nociceptive activity, visceral pain, pain associated with diabetic neuropathy, rheumatoid arthritis, chronic knee and joint pain, tendonitis, osteoarthritis, neuropathic pains.
[0274] The actual amount of the compound to be administered in any given case will be determined by a physician taking into account the relevant circumstances, such as the severity of the condition, the age and weight of the patient, the patient's general physical condition, the cause of the condition, and the route of administration.
[0275] The patient will be administered the compound orally in any acceptable form, such as a tablet, liquid, capsule, powder and the like, or other routes may be desirable or necessary, particularly if the patient suffers from nausea. Such other routes may include, without exception, transdermal, parenteral, subcutaneous, intranasal, via an implant stent, intrathecal, intravitreal, topical to the eye, back to the eye, intramuscular, intravenous, and intrarectal modes of delivery. Additionally, the formulations may be designed to delay release of the active compound over a given period of time, or to carefully control the amount of drug released at a given time during the course of therapy.
[0276] In another embodiment of the invention, there are provided pharmaceutical compositions including at least one compound of the invention in a pharmaceutically acceptable carrier therefor. The phrase “pharmaceutically acceptable” means the carrier, diluent or excipient must be compatible with the other ingredients of the formulation and not deleterious to the recipient thereof.
[0277] Pharmaceutical compositions of the present invention can be used in the form of a solid, a solution, an emulsion, a dispersion, a micelle, a liposome, and the like, wherein the resulting composition contains one or more compounds of the present invention, as an active ingredient, in admixture with an organic or inorganic carrier or excipient suitable for enteral or parenteral applications. Invention compounds may be combined, for example, with the usual non-toxic, pharmaceutically acceptable carriers for tablets, pellets, capsules, suppositories, solutions, emulsions, suspensions, and any other form suitable for use. The carriers which can be used include glucose, lactose, gum acacia, gelatin, mannitol, starch paste, magnesium trisilicate, talc, corn starch, keratin, colloidal silica, potato starch, urea, medium chain length triglycerides, dextrans, and other carriers suitable for use in manufacturing preparations, in solid, semisolid, or liquid form. In addition auxiliary, stabilizing, thickening and coloring agents and perfumes may be used. Invention compounds are included in the pharmaceutical composition in an amount sufficient to produce the desired effect upon the process or disease condition.
[0278] Pharmaceutical compositions containing invention compounds may be in a form suitable for oral use, for example, as tablets, troches, lozenges, aqueous or oily suspensions, dispersible powders or granules, emulsions, hard or soft capsules, or syrups or elixirs. Compositions intended for oral use may be prepared according to any method known to the art for the manufacture of pharmaceutical compositions and such compositions may contain one or more agents selected from the group consisting of a sweetening agent such as sucrose, lactose, or saccharin, flavoring agents such as peppermint, oil of wintergreen or cherry, coloring agents and preserving agents in order to provide pharmaceutically elegant and palatable preparations. Tablets containing invention compounds in admixture with non-toxic pharmaceutically acceptable excipients may also be manufactured by known methods. The excipients used may be, for example, (1) inert diluents such as calcium carbonate, lactose, calcium phosphate or sodium phosphate; (2) granulating and disintegrating agents such as corn starch, potato starch or alginic acid; (3) binding agents such as gum tragacanth, corn starch, gelatin or acacia, and (4) lubricating agents such as magnesium stearate, stearic acid or talc. The tablets may be uncoated or they may be coated by known techniques to delay disintegration and absorption in the gastrointestinal tract and thereby provide a sustained action over a longer period. For example, a time delay material such as glyceryl monostearate or glyceryl distearate may be employed.
[0279] In some cases, formulations for oral use may be in the form of hard gelatin capsules wherein the invention compounds are mixed with an inert solid diluent, for example, calcium carbonate, calcium phosphate or kaolin. They may also be in the form of soft gelatin capsules wherein the invention compounds are mixed with water or an oil medium, for example, peanut oil, liquid paraffin, or olive oil.
[0280] The pharmaceutical compositions may be in the form of a sterile injectable suspension. This suspension may be formulated according to known methods using suitable dispersing or wetting agents and suspending agents. The sterile injectable preparation may also be a sterile injectable solution or suspension in a non-toxic parenterally-acceptable diluent or solvent, for example, as a solution in 1,3-butanediol. Sterile, fixed oils are conventionally employed as a solvent or suspending medium. For this purpose any bland fixed oil may be employed including synthetic mono- or diglycerides, fatty acids (including oleic acid), naturally occurring vegetable oils like sesame oil, coconut oil, peanut oil, cottonseed oil, etc., or synthetic fatty vehicles like ethyl oleate or the like. Buffers, preservatives, antioxidants, and the like can be incorporated as required.
[0281] Invention compounds may also be administered in the form of suppositories for rectal administration of the drug. These compositions may be prepared by mixing the invention compounds with a suitable non-irritating excipient, such as cocoa butter, synthetic glyceride esters of polyethylene glycols, which are solid at ordinary temperatures, but liquify and/or dissolve in the rectal cavity to release the drug.
[0282] Since individual subjects may present a wide variation in severity of symptoms and each drug has its unique therapeutic characteristics, the precise mode of administration and dosage employed for each subject is left to the discretion of the practitioner.
[0283] The compounds and pharmaceutical compositions described herein are useful as medicaments in mammals, including humans, for treatment of diseases and or alleviations of conditions which are responsive to treatment by agonists or functional antagonists of sphingosine-1-phosphate receptors. Thus, in further embodiments of the invention, there are provided methods for treating a disorder associated with modulation of sphingosine-1-phosphate receptors. Such methods can be performed, for example, by administering to a subject in need thereof a pharmaceutical composition containing a therapeutically effective amount of at least one invention compound. As used herein, the term “therapeutically effective amount” means the amount of the pharmaceutical composition that will elicit the biological or medical response of a subject in need thereof that is being sought by the researcher, veterinarian, medical doctor or other clinician. In some embodiments, the subject in need thereof is a mammal. In some embodiments, the mammal is human.
[0284] The present invention concerns also processes for preparing the compounds of Formula I.
[0285] The compounds of formula I according to the invention can be prepared analogously to conventional methods as understood by the person skilled in the art of synthetic organic chemistry.
[0286] The synthetic scheme set forth below, illustrates how compounds according to the invention can be made. Those skilled in the art will be able to routinely modify and/or adapt the following scheme to synthesize any compounds of the invention covered by Formula I.
[0287] General schemes for synthesizing coumarin derivatives:
[0000]
[0288] Substituted 2H-chromene-3-carboxylic acids intermediates, prepared from known procedures, and the desired aniline in N,N-dimethylformamide were treated with o-(7-azabenzotriazole-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate and diisopropylethyl amine. The reaction was stirred at room temperature for 16 hours. The solution was quenched with water and the product extracted with ethylacetate. The organic layers were combined and dried over sodium sulfate. The organic layer was filtered and evaporated under vacuum to afford the crude amide. Purification via medium pressure liquid chromatography (gradient MeOH/DCM) afforded the desired compound the corresponding compound of Formula I.
[0000]
[0289] To the substituted-2H-chromene-3-carboxylic acids intermediates, prepared from known procedures, in dichloromethane are added diisopropyl ethyl amine and a 50% solution of propylphosphonic anhydride in ethyl acetate. The mixture was stirred for 30 minutes at room temperature. The desired aniline is added to the reaction mixture which is stirred at room temperature overnight. The reaction mixture is then poured onto ice water and dichloromethane is added. The organic layer is separated and washed with brine dried with sodium sulfate, filtered and concentrated to dryness. The residue was triturated with dichloromethane/Hexanes and then the solid was passed through a medium pressure liquid chromatography to give the corresponding compound of Formula I.
DETAILED DESCRIPTION OF THE INVENTION
[0290] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention claimed. As used herein, the use of the singular includes the plural unless specifically stated otherwise.
[0291] It will be readily apparent to those skilled in the art that some of the compounds of the invention may contain one or more asymmetric centers, such that the compounds may exist in enantiomeric as well as in diastereomeric forms. Unless it is specifically noted otherwise, the scope of the present invention includes all enantiomers, diastereomers and racemic mixtures. Some of the compounds of the invention may form salts with pharmaceutically acceptable acids or bases, and such pharmaceutically acceptable salts of the compounds described herein are also within the scope of the invention.
[0292] The present invention includes all pharmaceutically acceptable isotopically enriched compounds. Any compound of the invention may contain one or more isotopic atoms enriched or different than the natural ratio such as deuterium 2 H (or D) in place of protium 1 H (or H) or use of 13 C enriched material in place of 12 C and the like. Similar substitutions can be employed for N, O and S. The use of isotopes may assist in analytical as well as therapeutic aspects of the invention. For example, use of deuterium may increase the in vivo half-life by altering the metabolism (rate) of the compounds of the invention. These compounds can be prepared in accord with the preparations described by use of isotopically enriched reagents.
[0293] The following examples are for illustrative purposes only and are not intended, nor should they be construed as limiting the invention in any manner. Those skilled in the art will appreciate that variations and modifications of the following examples can be made without exceeding the spirit or scope of the invention.
[0294] As will be evident to those skilled in the art, individual isomeric forms can be obtained by separation of mixtures thereof in conventional manner. For example, in the case of diasteroisomeric isomers, chromatographic separation may be employed.
[0295] The IUPAC names of the compounds mentioned in the examples were generated with ACD version 8.
[0296] Unless specified otherwise in the examples, characterization of the compounds is performed according to the following methods:
[0297] NMR spectra are recorded on 300 or 600 MHz Varian and acquired at room temperature. Chemical shifts are given in ppm referenced either to internal trimethylsilyl or to the residual solvent signal.
[0298] All the reagents, solvents, catalysts for which the synthesis is not described are purchased from chemical vendors such as Sigma Aldrich, Fluka, Bio-Blocks, Ryan Scientific, Syn Chem, Chem-Impex, Aces Pharma, however some known intermediates, for which the CAS registry number [CAS #] are mentioned, were prepared in-house following known procedures.
[0299] Usually the compounds of the invention were purified by flash column chromatography using a gradient solvent system of methanol/dichloromethane unless otherwise reported.
[0300] The following abbreviations are used in the examples:
[0301] NH 3 ammonia
[0302] BOC tert-butyloxy carbonyl
[0303] CH 3 CN acetonitrile
[0304] PPPA propylphosphonic anhydride
[0305] PSI pound per square inch
[0306] ClSO 2 OH chlorosulfonic acid
[0307] DIPEA diisopropylethyl amine
[0308] DCM dichloromethane
[0309] DMF N,N-dimethylformamide
[0310] HATU o-(7-azabenzotriazole-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate
[0311] NaOH sodium hydroxide
[0312] MeOH methanol
[0313] CD 3 OD deuterated methanol
[0314] NH 3 ammonia
[0315] HCl hydrochloric acid
[0316] NaIO 4 sodium periodate
[0317] Na 2 SO 4 sodium sulfate
[0318] ON overnight
[0319] R.T. room temperature
[0320] MgSO 4 magnesium sulfate
[0321] EtOAc ethyl acetate
[0322] CDCl 3 deuterated chloroform
[0323] DMSO-d 6 deuterated dimethyl sulfoxide
[0324] MPLC medium pressure liquid chromatography
[0325] TFA trifluoroacetic acid
[0326] THF tetrahydrofuran
[0327] PdCl 2 (PPh 3 ) 2 bis(triphenylphosphine)palladium(II) chloride
[0328] LiCl lithium chloride
[0329] Pd(PPh 3 ) 4 tetrakis(triphenylphosphine) palladium
[0330] CH 3 CN acetonitrile
[0331] TEA triethylamine
[0332] EDTA ethylenediaminetetraacetic acid
[0333] BCl 3 boron trichloride
[0334] NaHCO 3 sodium bicarbonate
[0335] TBME tert-butyl methylether
[0336] CH 3 CHO acetaldehyde
[0337] Hantzsch ester diethyl 1,4-dihydro-2,6-dimethyl-3,5-pyridinedicarboxylate
[0338] The following synthetic schemes illustrate how compounds according to the invention can be made. Those skilled in the art will be routinely able to modify and/or adapt the following schemes to synthesize any compound of the invention covered by Formula I.
[0339] Some compounds of this invention can generally be prepared in one step from commercially available literature starting materials.
EXAMPLE 1
Compound 1
N-(3-Fluoro-2-methylphenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide
[0340] 7-Methoxy-2-oxo-8-propyl-2H-chromene-3-carboxylic acid (CAS 952504-50-6) (Intermediate 1) (0.20 g, 0.76 mmol) and 3-fluoro-2-methyl-phenylamine [CAS 443-86-7] (0.09 mL, 0.84 mmol) in DMF (20 mL) were treated with HATU (0.42 g, 1.1 mmol) and diisopropylethyl amine (0.38 mL, 2.3 mmol). The reaction was stirred at r.t. for 16 hours. The solution was quenched with water and the product extracted with EtOAc. The organic layers were combined and dried over Na 2 SO 4 . The organic layer was filtered and evaporated under vacuum to afford the crude title compound. Purification via MPLC (gradient MeOH/DCM) afforded 0.14 g (50%) of Compound 1.
[0341] 1 H NMR (600 MHz, CDCl 3 -d 3 ) δ 10.92 (s, 1H), 8.95 (s, 1H), 8.11 (d, J=8.2 Hz, 1H), 7.58 (d, J=8.7 Hz, 1H), 7.25-7.17 (m, 1H), 6.98 (d, J=8.8 Hz, 1H), 6.87 (t, J=8.7 Hz, 1H), 3.98 (s, 3H), 2.93-2.78 (m, 2H), 2.34 (d, J=1.3 Hz, 3H), 1.67-1.60 (m, 2H), 1.00 (t, J=7.3 Hz, 3H).
EXAMPLE 2
Intermediate 2
8 -Ethyl-7-methoxy-2-oxo-2H-chromene-3-carboxylic acid
[0342] Step 1: 1,3-Cyclohexanedione (10 g, 89.2 mmol), 40% aqueous CH 3 CHO (49.4 g, 445.9 mmol) were dissolved in methanol (40 mL) followed by addition of Hantzsch ester (22.7 g, 89.2 mmol) and pyridine (2.1 g, 18.74 mmol) under nitrogen. The resulting light yellow mixture was stirred at room temperature overnight, then concentrated to give crude product that was re-slurried in a mixture of CH 2 Cl 2 (40 mL) and hexanes (60 mL) to furnish 2-ethyl-1,3-cyclohexanedione (8.6 g, 69%).
[0343] Step 2: 2-Ethyl-1,3-cyclohexanedione (15 g, 107 mmol), mesitylene (240 mL), and 5% Pd/C (7.8 g) were placed in a flask. The reaction mixture was stirred at 160° C. for two days. Filtration gave a crude product, which was purified by chromatography (EtOAc/Hexane) to give 2-ethyl-3-hydroxy phenol (2.2 g, 15%).
[0344] Step 3: DMF (46 mL) was placed in a flask followed by addition of POCl 3 (30.2 g, 194.34 mmol) dropwise at 0° C. The mixture was stirred at −5° C. for 30 min followed by addition of a solution of 2-ethyl-3-hydroxy phenol (8.95 g, 64.78 mmol) in DMF (40 mL). After 3.5 hours, the reaction mixture was poured into 2M aq. NaOH, and extracted with EtOAc (2×200 mL). The remained aqueous solution was neutralized with 5M aq. HCl. to pH ˜5, extracted with EtOAc (2×200 mL), and the EtOAc phase was dried over Na 2 SO 4 , concentrated, purified by chromatography (EtOAc/Hexane) to give a desired product (11 g, 62%).
[0345] Step 4: Sodium hydride (60%, 2.8 g) was added portionwise to a solution of 2-ethyl-3,4-dihydroxybenzaldehyde (5.8 g, 34.93 mmol) in DMSO (80 mL) at −10° C. under nitrogen, and the resulting mixture was stirred at −10° C. for 1.5 hours followed by addition of iodomethane (4.96 g, 34.93 mmol) dropwise. The solution was warmed to room temperature, and stirred overnight. The reaction solution was poured into ice/water, extracted with TBME. The combined organic phase was dried over anhydrous Na 2 SO 4 , and concentrated to give a crude product that was purified by chromatography to give 2-hydroxy-4-methoxy-3-ethyl-benzaldehyde (3.75 g, 55%).
[0346] Step 5: To a solution of 2-hydroxy-4-methoxy-3-ethyl-benzaldehyde (3.1 g, 17.2 mmol) in ethanol (93 mL) is added diethyl malonate (2.8 g, 17.2 mmol) and piperidine (1.5 g, 17.2 mmol). The reaction mixture was stirred at room temperature overnight. The reaction mixture was then cooled to 0° C. with ice/water bath and the formed precipitate was filtered and washed with ethanol to give 7-methoxy-2-oxo-8-ethyl-2H-chromene-3-carboxylic acid ethyl ester (3.1 g, 65%).
[0347] Step 6: To a solution of 7-methoxy-2-oxo-8-ethyl-2H-chromene-3-carboxylic acid ethyl ester (3.1 g, 11.2 mmol) in THF (62 mL) was added at 0° C. a 1M solution of NaOH (25 mL). The reaction mixture was stirred at room temperature overnight. The mixture was cooled to 0° C. with ice/water bath and pH was adjusted to ˜1 by adding 1M HCl solution. The formed precipitate was filtered and washed with water, dried to give the title Intermediate 2 (2.55 g, 99%).
[0348] 1 H NMR (300 MHz, DMSO-d 6 ) δ 12.95 (br s, 1H), 8.69 (s, 1H), 7.77 (d, J=8.8 Hz, 1H), 7.13 (d, J=8.8 Hz, 1H), 3.93 (s, 3H), 2.71 (q, J=7.3 Hz, 2H), 1.08 (t, J=7.3 Hz, 3H).
EXAMPLE 3
Intermediate 3
7 , 8 -Diethoxy-2-oxo-2H-chromene-3-carboxylic acid
[0349] Step 1: Sodium hydride (60%, 64 g) was added portionwise to a solution of 2,3,4-trihydroxybenzaldehyde (61.6 g, 400 mmol) at −10° C. under nitrogen, and the resulting mixture was stirred at −10° C. for 1.5 hours followed by addition of iodoethane (206 g, 1.32 mol) dropwise. The solution was warmed to room temperature, and stirred overnight. The reaction solution was poured into ice/water (3.5 kg), extracted with TBME (500 mL×5). The combined organic phase was washed with sat. NaHCO 3 (400 mL×3) and water (400 mL×2), dried over anhydrous Na 2 SO 4 , and concentrated to give a crude product (50 g) that was used directly for the next step without further purification.
[0350] Step 2: A solution of crude 2,3,4-triethoxybenzaldehyde (50 g) from step 1 was dissolved in CH 2 Cl 2 followed by slow addition of 1M BCl 3 in CH 2 Cl 2 (188 mL) while controlling the temperature at about 25° C. The resulting mixture was stirred at room temperature for 2 hours and then carefully poured into sat. aq. NaHCO 3 . The solution was adjusted to pH ˜1 by addition of concentrated HCl. The organic phase was separated, and the aqueous phase was extracted with TBME. The combined organic phase was dried over anhydrous Na 2 SO 4 , concentrated to give a crude product that was purified by chromatography to furnish the desired product (9.8 g, 21%).
[0351] Step 3: The material from Step 2 (11.2 g, 53.3 mmol) and diethyl malonate (8.54 g, 53.3 mmol) were dissolved in anhydrous ethanol (310 mL) under nitrogen. The mixture was cooled with ice/water followed by addition of piperidine (4.54 g, 53.3 mmol), and stirred at room temperature for 2 hours. The reaction solution was stored at −20° C. for 3 hours. Filtration gave a crude solid that was washed with cooled ethanol, and then dissolved in CH 2 Cl 2 , dried over anhydrous Na 2 SO 4 , concentrated to give a crude product that was purified by chromatography (EtOAc/Hexane) to obtain a desired product (14.0 g, 85.9%).
[0352] Step 4: The material from Step 3 (14.0 g, 45.7 mmol) was dissolved in THF (280 mL), cooled with ice/water followed by addition of 1M aq. NaOH (220 mL), and stirred at room temperature overnight. The organic phase was separated, and the aqueous phase was extracted with TBME (100 mL×3). The aqueous phase was adjusted to pH ˜1 by 1M aq. HCl, and then added CH 2 Cl 2 . The CH 2 Cl 2 phase was separated and the aqueous phase was extracted with CH 2 Cl 2 . The combined CH 2 Cl 2 was dried over anhydrous Na 2 SO 4 , and concentrated to give a light yellow solid as the title compound (12 g, 94.5%).
[0353] 1 H NMR (300 MHz, DMSO-d 6 ) δ 12.98 (s, 1H), 8.66 (s, 1H), 7.61 (d, J=9.0 Hz, 1H), 7.15 (d, J=8.8 Hz, 1H), 4.20 (q, J=7.0 Hz, 2H), 4.07 (q, J=7.0 Hz, 2H), 1.37 (t, J=6.9 Hz, 3H), 1.28 (t, J=7.0 Hz, 3H).
EXAMPLE 4
Intermediate 4
8-Isopropoxy-7-methoxy-2-oxo-2H-chromene-3-carboxylic acid
[0354] Step 1: A solution of 2,3,4-trimethoxybenzaldehyde (9.81 g, 50 mmol) was dissolved in CH 2 Cl 2 (250 mL) followed by addition of BCl 3 solution (1M, in CH 2 Cl 2 , 50 mL) dropwise. The mixture was stirred at room temperature for 2 hours, and then added another equivalent of BCl 3 solution (1M in CH 2 Cl 2 , 50 mL). The reaction mixture was stirred at RT overnight, and poured into 10% NaHCO 3 . The aqueous layer was acidified by 2M H 2 SO 4 to pH ˜1, extracted with EtOAc, dried over Na 2 SO 4 , concentrated to give a grey product (7.4 g, 88%).
[0355] Step 2: The compound from the previous step (20 g, 118.94 mmol) was added to a solution of sodium hydride (60%, 11 g) in dry DMSO (300 mL). The mixture was stirred for 40 min, added potassium iodide (20.0 g, 120.5 mmol) and stirred another 10 minutes followed by addition of 2-bromopropane (15.0 g, 122 mmol). The mixture was stirred overnight, diluted with EtOAc. The organic phase was dried over Na 2 SO 4 and concentrated to give a crude product that was purified by chromatography (EtOAc/Hexane) to give a desired product (5.4 g, 21%).
[0356] Step 3: The compound from the previous step (10.8 g, 51.37 mmol) and diethyl malonate (8.9 g, 55.57 mmol) were dissolved in anhydrous ethanol (300 mL) under nitrogen. The mixture was cooled with ice/water followed by addition of piperidine (4.7 g, 55.20 mmol), and stirred at room temperature for 2 hours. The reaction solution was stored at −20° C. for 3 hours. Filtration gave a crude solid that was washed with cooled ethanol, dried to obtain a desired product (10.4 g, 65%).
[0357] Step 4: The material from the previous step (8.3 g, 27.1 mmol) was dissolved in THF (100 mL), cooled with ice/water followed by addition of 1M aq. NaOH (50 mL), and stirred at room temperature overnight. The organic phase was separated, and the aqueous phase was extracted with TBME (50 mL×2). The remained aqueous phase was adjusted to pH ˜1 by 1M aq. HCl, and then cooled to 0° C. Filtration and drying gave a light yellow title intermediate (7 g, 25.16 mmol, 93.2%).
[0358] 1 H NMR (300 MHz, DMSO-d 6 ) δ 12.98 (br s, 1H), 8.68 (s, 1H), 7.63 (d, J=8.8 Hz, 1H), 7.17 (d, J=8.8 Hz, 1H), 4.50-4.34 (m, 1H), 3.91 (s, 3H), 1.24 (d, J=6.2 Hz, 6H).
EXAMPLE 5
Intermediate 5
8-Ethoxy-7-methoxy-2-oxo-2H-chromene-3-carboxylic acid
[0359] Step 1: A solution of 2,3,4-trimethoxybenzaldehyde (9.81 g, 50 mmol) was dissolved in CH 2 Cl 2 (250 mL) followed by addition of BCl 3 solution (1M, in CH 2 Cl 2 , 50 mL) dropwise. The mixture was stirred at room temperature for 2 hours, and then added another equivalent of BCl 3 solution (1M in CH 2 Cl 2 , 50 mL). The reaction mixture was stirred at room temperature overnight, and poured into 10% NaHCO 3 . The aqueous layer was acidified by 2M H 2 SO 4 to pH ˜1, extracted with EtOAc, dried over Na 2 SO 4 , concentrated to give a grey product (7.4 g, 88%).
[0360] Step 2: The product from the previous step (10.0 g, 59.47 mmol) was added to a solution of sodium hydride (4.8 g, 60%, 120 mmol) in dry DMSO (200 mL). The mixture was stirred for 20 min and iodoethane (9.4 g, 60.27 mmol) was added then stirred overnight. The reaction was quenched with water, adjusted by con. HCl to pH ˜6, extracted with EtOAc. The organic phase was washed with H 2 O and sat. aq. NaCl, dried, and concentrated to give a brown oil product (12 g, 55%).
[0361] Step 3: The product from the previous step (10.8 g, 55 mmol) and diethyl malonate (8.9 g, 55.6 mmol) were dissolved in anhydrous ethanol (300 mL) under nitrogen. The mixture was cooled with ice/water followed by addition of piperidine (4.7 g, 55.2 mmol), and stirred at room temperature for 2 hours. The reaction solution was stored at −20° C. for 3 hours. Filtration gave a crude solid that was washed with cooled ethanol, dried to obtain a desired product (10.4 g, 35.6 mmol, 65%).
[0362] Step 4: The product from the previous step (15.0 g, 51.32 mmol) was dissolved in THF (300 mL), cooled with ice/water followed by addition of 1M aq. NaOH (150 mL), and stirred at room temperature overnight. The organic phase was separated, and the aqueous phase was extracted with TBME (100 mL×3). The remained aqueous phase was adjusted to pH ˜1 by 1M aq. HCl, and cooled to 0° C. Filtration and drying gave a light yellow title compound (13.2 g, 49.96 mmol, 97.5%).
[0363] 1 H NMR (300 MHz, DMSO-d 6 ) δ 13.00 (br s, 1H), 8.68 (s, 1H), 7.64 (d, J=8.8 Hz, 1H), 7.17 (d, J=9.1 Hz, 1H), 4.06 (q, J=7.0 Hz, 2H), 3.92 (s, 3H), 1.28 (t, J=7.0 Hz, 3H).
[0364] Compounds 2-16, 18-20, 22-24, 26-40, 43-45, 47, 48, 51, 54, 56, 57, 58, 59, 60, 61, 64, 65, 62, 63, 69, 70, 71 and 72 were prepared from Intermediate 1 (unless otherwise specified) and the corresponding amine, in a similar manner to the method described in Example 1 for Compound 1. The reagents used and the results are described below in Table 1.
[0000]
TABLE 1
Compound number
IUPAC name
Reagent(s) used
1 H NMR δ (ppm) for Compound
2
N-(2-
2-fluoro-
(600 MHz; CDCl 3 ) δ 11.18 (br s,
fluorophenyl)-
phenylamine
1H), 8.92 (s, 1H), 8.50 (td, J = 1.5,
7-methoxy-2-
[CAS 348-54-9]
8.0 Hz, 1H), 7.57 (d, J = 8.7 Hz,
oxo-8-propyl-
1H), 7.20-7.13 (m, 2H),
2H-chromene-
7.12-7.08 (m, 1H), 6.97 (d, J = 8.8 Hz,
3-carboxamide
1H), 3.98 (s, 3H), 2.87 (dd, J = 7.0,
8.4 Hz, 2H), 1.63 (sxt, J = 7.5 Hz,
2H), 1.00 (t, J = 7.3 Hz,
3H).
3
N-(2-
2-chloro-pyridin-3-
(600 MHz, CDCl 3 ) δ 11.53 (br s,
chloropyridin-
ylamine
1H), 9.00-8.88 (m, 1H), 8.16 (br
3-yl)-7-
[CAS 6298-19-7]
s, 1H), 7.82 (br. s., 1H), 7.59 (d, J = 8.6 Hz,
methoxy-2-oxo-
1H), 7.38-7.24 (m, 1H),
8-propyl-2H-
7.06 (br. s., 3H), 6.99 (d, J = 8.5 Hz,
chromene-3-
1H), 3.99 (s, 2 H), 2.87 (t, J = 7.6 Hz,
carboxamide
1H), 1.74-1.50 (m, 1H),
1.00 (t, J = 7.3 Hz, 3H).
4
7-methoxy-2-
2-trifluoromethyl-
(600 MHz, CDCl 3 ) δ 11.25 (s,
oxo-8-propyl-N-
phenylamine
1H), 8.93 (s, 1H), 8.41 (d, J = 8.4 Hz,
[2-
[CAS 88-17-5]
1H), 7.68 (d, J = 7.8 Hz, 1H),
(trifluoromethyl)phenyl]-
7.60 (t, J = 7.9 Hz, 1H), 7.57 (d, J = 8.7 Hz,
2H-
1H), 7.27 (t, J = 7.6 Hz,
chromene-3-
1H), 6.97 (d, J = 8.7 Hz, 1H),
carboxamide
3.98 (s, 3H), 2.86 (dd, J = 6.9,
8.5 Hz, 2H), 1.62 (sxt, J = 7.5 Hz,
2H), 1.00 (t, J = 7.3 Hz, 3H).
5
N-(2-
2-bromo-
(600 MHz, CDCl 3 ) δ 11.32 (s,
bromophenyl)-
phenylamine
1H), 8.94 (s, 1H), 8.57 (dd, J = 1.5,
7-methoxy-2-
[CAS 615-36-1]
8.4 Hz, 1H), 7.61 (dd, J = 1.4,
oxo-8-propyl-
8.0 Hz, 1H), 7.58 (d, J = 8.7 Hz,
2H-chromene-
1H), 7.38-7.34 (m, 1H),
3-carboxamide
7.02 (td, J = 1.5, 7.7 Hz, 1H), 6.97 (d,
J = 8.7 Hz, 1H), 3.98 (s, 3H),
2.86 (dd, J = 6.9, 8.5 Hz, 2H),
1.68-1.59 (m, 2H), 1.00 (t, J = 7.3 Hz,
3H).
6
N-(3-
3-bromo-pyridin-4-
(600 MHz, CDCl 3 ) δ 11.65 (br s,
bromopyridin-
ylamine
1H), 8.94 (s, 1H), 8.73 (br s, 1H),
4-yl)-7-
[CAS 13534-98-0]
8.61 (br s, 1H), 8.49 (br s, 1H),
methoxy-2-oxo-
7.61 (d, J = 8.7 Hz, 1H), 7.00 (d,
8-propyl-2H-
J = 8.8 Hz, 1H), 4.00 (s, 3H),
chromene-3-
2.87 (t, J = 7.6 Hz, 2H),
carboxamide
1.69-1.56 (m, 2H), 1.00 (t, J = 7.3 Hz, 3H).
7
7-methoxy-2-
pyridin-4-ylamine
(600 MHz, CDCl 3 ) δ 11.08 (s,
oxo-8-propyl-N-
[CAS 504-24-5]
1H), 8.92 (s, 1H), 8.56 (d, J = 5.1 Hz,
pyridin-4-yl-2H-
2H), 7.67 (d, J = 6.3 Hz, 2H),
chromene-3-
7.59 (d, J = 8.7 Hz, 1H), 6.99 (d,
carboxamide
J = 8.8 Hz, 1H), 3.98 (s, 3H),
2.91-2.83 (m, 2H), 1.63 (sxt, J = 7.5 Hz,
2H), 1.00 (t, J = 7.3 Hz,
3H).
8
7-methoxy-N-
3-methyl-pyridin-4-
(600 MHz, CDCl 3 ) δ 11.17 (s,
(3-
ylamine
1H), 8.96 (s, 1H), 8.47-8.45 (m,
methylpyridin-
[CAS 1990-90-5]
1H), 8.43 (d, J = 5.4 Hz, 2H),
4-yl)-2-oxo-8-
8.43 (d, J = 5.4 Hz, 2H), 7.61 (d,
propyl-2H-
J = 8.7 Hz, 1H), 7.00 (d, J = 8.7 Hz,
chromene-3-
1H), 3.99 (s, 3H), 2.87 (dd, J = 6.9,
carboxamide
8.5 Hz, 2H), 2.42 (s, 3H),
1.63 (sxt, J = 7.5 Hz, 2H), 1.00 (t,
J = 7.3 Hz, 3H).
9
7-methoxy-2-
3-trifluoromethyl-
(600 MHz, CDCl 3 ) δ 11.68 (s,
oxo-8-propyl-N-
pyridin-4-ylamine
1H), 8.93 (s, 1H), 8.85 (br s, 1H),
[3-
[CAS 387824-61-5]
8.74 (d, J = 5.0 Hz, 1H), 8.68 (d,
(trifluoromethyl)pyridin-
J = 5.6 Hz, 1H), 7.60 (d, J = 8.7 Hz,
4-yl]-
1H), 7.00 (d, J = 8.8 Hz, 1H),
2H-chromene-
4.00 (s, 3H), 2.88-2.84 (m, 2H),
3-carboxamide
1.66-1.58 (m, 2H), 0.99 (t, J = 7.3 Hz,
3H).
10
7-methoxy-2-
pyridin-3-ylamine
(600 MHz, CDCl 3 ) δ 10.99 (s,
oxo-8-propyl-N-
[CAS 462-08-8]
1H), 8.94 (s, 1H), 8.87 (br s, 1H),
pyridin-3-yl-2H-
8.41 (br. s., 1H), 8.28 (ddd, J = 1.3,
chromene-3-
2.3, 8.3 Hz, 1H), 7.59 (d, J = 8.7 Hz,
carboxamide
1H), 7.34 (dd, J = 4.9, 8.1 Hz,
1H), 6.99 (d, J = 8.7 Hz, 1H),
3.99 (s, 3H), 2.91-2.85 (m, 2H),
1.68-1.59 (m, 2H), 1.00 (t, J = 7.3 Hz,
3H).
11
7-methoxy-2-
2-trifluoromethyl-
(600 MHz, CDCl 3 ) δ 11.45 (s,
oxo-8-propyl-N-
pyridin-3-ylamine
1H), 8.93 (s, 1H), 8.90 (d, J = 8.4 Hz,
[2-
[CAS 106877-32-1]
1H), 8.48 (dd, J = 1.2, 4.6 Hz,
(trifluoromethyl)pyridin-
1H), 7.59 (d, J = 8.7 Hz, 1H),
3-yl]-
7.55 (dd, J = 4.6, 8.4 Hz, 1H),
2H-chromene-
6.99 (d, J = 8.7 Hz, 1H), 3.99 (s,
3-carboxamide
3H), 2.89-2.85 (m, 2H),
1.67-1.59 (m, 2H), 1.00 (t, J = 7.3 Hz, 3H).
12
7-methoxy-N-
3-methyl-pyridin-2-
(600 MHz, CDCl 3 ) δ 10.94 (br s,
(3-
ylamine
1H), 8.97 (s, 1H), 8.42 (d, J = 11.3 Hz,
methylpyridin-
[CAS 1603-40-3]
1H), 7.59 (d, J = 8.7 Hz,
2-yl)-2-oxo-8-
2H), 7.11 (br s, 1H), 6.98 (d, J = 8.8 Hz,
propyl-2H-
1H), 3.98 (s, 3H),
chromene-3-
2.89-2.85 (m, 2H), 2.39 (s, 3H),
carboxamide
1.67-1.59 (m, 2H), 1.00 (t, J = 7.4 Hz,
3H).
13
N-(3-
3-chloro-pyridazin-4-
(600 MHz, CDCl 3 ) δ 11.85 (s,
chloropyridazin-
ylamine
1H), 9.02 (d, J = 5.6 Hz, 1H),
4-yl)-7-
[CAS 55928-83-1]
8.92 (s, 1H), 8.71 (d, J = 5.6 Hz,
methoxy-2-oxo-
1H), 7.62 (d, J = 8.7 Hz, 1H),
8-propyl-2H-
7.01 (d, J = 8.7 Hz, 1H), ),
chromene-3-
4.00 (s, 3H), 2.91-2.83 (m, 2H),
carboxamide
1.66-1.60 (m, 2H), 1.00 (t, J = 7.4 Hz,
3H).
14
N-(2-chloro-5-
2-chloro-5-fluoro-
(600 MHz, CDCl 3 ) δ 11.63 (s,
fluoropyridin-3-
pyridin-3-ylamine
1H), 8.92 (s, 1H), 8.85 (dd, J = 2.8,
yl)-7-methoxy-
[CAS 884495-37-8]
10.1 Hz, 1H), 8.04 (d, J = 2.8 Hz,
2-oxo-8-propyl-
1H), 7.60 (d, J = 8.7 Hz, 1H),
2H-chromene-
7.00 (d, J = 8.7 Hz, 1H), 3.99 (s,
3-carboxamide
3H), 2.89-2.84 (m, 2H), 1.63 (dq,
J = 7.5, 15.1 Hz, 2H), 1.00 (t, J = 7.3 Hz,
3H).
15
7-methoxy-N-
2-methyl-pyridin-3-
(600 MHz, CDCl 3 ) δ 11.00 (s,
(2-
ylamine
1H), 8.94 (s, 1H), 8.69-8.62 (m,
methylpyridin-
[CAS 3430-10-2]
1H), 8.30 (dd, J = 1.5, 4.8 Hz,
3-yl)-2-oxo-8-
1H), 7.59 (d, J = 8.7 Hz, 1H),
propyl-2H-
7.21 (dd, J = 4.8, 8.1 Hz, 1H),
chromene-3-
6.99 (d, J = 8.7 Hz, 1H), 3.99 (s,
carboxamide
3H), 2.87 (dd, J = 6.9, 8.4 Hz,
2H), 2.70 (s, 3H), 1.72-1.56 (m,
2H), 1.00 (t, J = 7.3 Hz, 3H).
16
N-(2-
2-bromopyridin-3-
(300 MHz, CDCl 3 ) δ 11.44 (s, 1H),
bromopyridin-
amine
8.91 (s, 1H), 8.87 (dd, J = 1.5, 8.4 Hz,
3-yl)-7-
[CAS 39856-58-1]
1H), 8.13 (dd, J = 1.2, 4.2 Hz,
methoxy-2-oxo-
1H), 7.58 (d, J = 9.0 Hz, 1H),
8-propyl-2H-
7.30 (dd, J = 4.8, 8.1 Hz, 1H),
chromene-3-
6.98 (d, J = 8.7 Hz, 1H), 3.98 (s,
carboxamide
3H), 2.85 (t, J = 7.8 Hz, 2H),
1.68-1.56 (m, 2H), 0.99 (t, J = 7.5 Hz,
3H).
18
N-(3-
3-chloropyridin-4-
(300 MHz, DMSO-d 6 ) δ 11.54 (s,
chloropyridin-
amine
1H), 9.03 (s, 1H), 8.64 (s, 1H),
4-yl)-7-
[CAS 19798-77-7]
8.51-8.46 (m, 2H), 7.96 (d, J = 8.7 Hz,
methoxy-2-oxo-
1H), 7.23 (d, J = 9.0 Hz,
8-propyl-2H-
1H), 3.95 (s, 3H), 2.72 (t, J = 7.8 Hz,
chromene-3-
2H), 1.58-1.50 (m, 2H),
carboxamide
0.92 (t, J = 7.5 Hz, 3H).
19
N-(2-
2-ethylaniline [CAS
(300 MHz, CDCl 3 ) δ10.88 (s, 1H),
ethylphenyl)-7-
578-54-1]
8.95 (s, 1H), 8.29 (d, J = 8.1 Hz,
methoxy-2-oxo-
1H), 7.57 (d, J = 9.0 Hz, 1H),
8-propyl-2H-
7.29-7.24 (m, 2H), 7.12 (t, J = 7.5 Hz,
chromene-3-
1H), 6.97 (d, J = 8.4 Hz, 1H),
carboxamide
3.97 (s, 3H), 2.89-2.76 (m, 4H),
1.69-1.56 (m, 2H), 1.32 (t, J = 7.8 Hz,
3H), 0.99 (t, J = 7.2 Hz, 3H).
20
N-(2-
2-chloroaniline
(300 MHz, CDCl 3 ) δ 11.42 (s,
chlorophenyl)-
[CAS 95-51-2]
1H), 8.93 (s, 1H), 8.60 (d, J = 7.8 Hz,
7-methoxy-2-
1H), 7.57 (d, J = 8.7 Hz, 1H),
oxo-8-propyl-
7.43 (d, J = 7.5 Hz, 1H), 7.31 (t, J = 7.8 Hz,
2H-chromene-
1H), 7.08 (t, J = 8.1 Hz,
3-carboxamide
1H), 6.97 (d, J = 8.7 Hz, 1H),
3.97 (s, 3H), 2.86 (t, J = 7.5 Hz,
2H), 1.66-1.54 (m, 2H), 0.99 (t, J = 7.8 Hz,
3H).
22
N-(2-
2-aminobenzonitrile
(300 MHz, DMSO-d 6 ) δ 11.31 (s,
cyanophenyl)-
[CAS 1885-29-6]
1H), 9.00 (s, 1H), 8.41 (d, J = 8.1 Hz,
7-methoxy-2-
1H), 7.94 (d, J = 9.0 Hz, 1H),
oxo-8-propyl-
7.85 (dd, J = 1.5, 8.1 Hz, 1H),
2H-chromene-
7.76-7.71 (m, 1H) 7.32 (t, J = 7.8 Hz,
3-carboxamide
1H), 7.22 (d, J = 9.0 Hz, 1H),
3.95 (s, 3H), 2.74 (t, J = 8.1 Hz,
2H), 1.59-1.49 (m, 2H), 0.92 (t, J = 7.5 Hz,
3H).
23
N-(2-chloro-5-
2-chloro-5-
(300 MHz, CDCl 3 ) δ 11.45 (s,
methylpyridin-
methylaniline
1H), 8.90 (s, 1H), 8.77 (s, 1H),
3-yl)-7-
[CAS 95-81-8]
7.98 (s, 1H), 7.58 (d, J = 8.7 Hz,
methoxy-2-oxo-
1H), 6.98 (d, J = 9.0 Hz, 1H),
8-propyl-2H-
3.98 (s, 3H), 2.86 (t, J = 7.8 Hz,
chromene-3-
2H), 2.37 (s, 3H), 1.66-1.57 (m,
carboxamide
2H), 0.99 (t, J = 7.2 Hz, 3H).
24
7-methoxy-2-
2-propylaniline
(600 MHz, CDCl 3 ) δ 10.85 (s,
oxo-8-propyl-N-
[CAS 1821-39-2]
1H), 8.95 (s, 1H), 8.28 (dd, J = 1.2,
(2-
8.4 Hz, 1H), 7.57 (d, J = 9.0 Hz,
propylphenyl)-
1H), 7.27-7.24 (m, 1H),
2H-chromene-
7.22 (dd, J = 1.2, 7.8 Hz, 1H),
3-carboxamide
7.12-7.09 (m, 1H), 6.96 (d, J = 9.0 Hz,
1H), 3.97 (s, 3H), 2.88-2.85 (m,
2H), 2.74 (t, J = 7.2 Hz, 2H),
1.74-1.68 (m, 2H), 1.66-1.60 (m,
2H), 1.04-0.98 (m, 6H).
26
7-methoxy-N-
o-toluidine
(300 MHz, DMSO-d 6 ) δ 10.68 (s,
(2-
[CAS 95-53-4]
1H), 8.98 (s, 1H), 8.19 (d, J = 8.2 Hz,
methylphenyl)-
1H), 7.93 (d, J = 8.5 Hz, 1H),
2-oxo-8-propyl-
7.32-7.18 (m, 3H), 7.07 (d, J = 8.5 Hz,
2H-chromene-
1H), 3.95 (s, 3H), 2.75 (t,
3-carboxamide
J = 6.9 Hz, 2H), 2.33 (s, 3H),
1.62-1.48 (m, 2H), 0.92 (t, J = 7.3 Hz,
3H).
27
8-isopropoxy-
Intermediate 4
(300 MHz, CDCl 3 ) δ11.37 (s, 1H),
7-methoxy-2-
(used in place of
8.92 (s, 1H), 8.86 (d, J = 8.2 Hz,
oxo-N-[2-
Intermediate 1) and
1H), 8.47 (dd, J = 1.0, 4.5 Hz,
(trifluoromethyl)pyridin-
2-Trifluoromethyl-
1H), 7.55 (dd, J = 4.5, 8.5 Hz,
3-yl]-
pyridin-3-ylamine
1H), 7.45 (d, J = 8.6 Hz, 1H),
2H-chromene-
[CAS 106877-32-1]
7.01 (d, J = 8.8 Hz, 1H),
3-carboxamide
4.71-4.54 (m, 1H), 4.00 (s, 3H),
1.39 (d, J = 6.2 Hz, 6H).
28
8-isopropoxy-
Intermediate 4
(300 MHz, CDCl 3 ) δ 10.93 (s,
7-methoxy-N-
(used in place of
1H), 8.94 (s, 1 H), 8.63 (dd, J = 1.5,
(2-
Intermediate 1) and
8.2 Hz, 1H), 8.30 (dd, J = 1.5,
methylpyridin-
2-Methyl-pyridin-3-
4.7 Hz, 1H), 7.46 (d, J = 8.8 Hz,
3-yl)-2-oxo-2H-
ylamine
1H), 7.21 (dd, J = 4.8, 8.2 Hz,
chromene-3-
[CAS 340-10-2]
1H), 7.02 (d, J = 8.8 Hz, 1H),
carboxamide
4.61 (dt, J = 6.2, 12.4 Hz, 1H),
4.00 (s, 3H), 2.69 (s, 3H), 1.41 (d,
6H).
29
8-ethoxy-7-
Intermediate 5
(600 MHz, CDCl 3 ) δ 10.93 (br s,
methoxy-N-(2-
(used in place of
1H), 8.96-8.93 (m, 1H), 8.63 (d, J = 8.0 Hz,
methylpyridin-
Intermediate 1) and
1H), 8.31 (d, J = 3.5 Hz,
3-yl)-2-oxo-2H-
2-Methyl-pyridin-3-
1H), 7.47 (d, J = 8.7 Hz, 1H),
chromene-3-
ylamine
7.21 (dd, J = 4.8, 8.0 Hz, 1H),
carboxamide
[CAS 3430-10-2]
7.03 (d, J = 8.7 Hz, 1H),
4.30-4.22 (m, 2H), 4.02 (s, 3H),
2.69 (s, 3H), 1.48 (t, J = 7.0 Hz, 3H).
30
8-ethoxy-7-
Intermediate 5
(300 MHz, CDCl 3 ) δ 11.37 (s,
methoxy-2-oxo-
(used in place of
1H), 8.93 (s, 1H), 8.87 (d, J = 8.4 Hz,
N-[2-
Intermediate 1)
1H), 8.58-8.41 (m, 1H),
(trifluoromethyl)pyridin-
2-Trifluoromethyl-
7.56 (dd, J = 4.6, 8.4 Hz, 1H), 7.46 (d,
3-yl]-
pyridin-3-ylamine
J = 8.8 Hz, 1H), 7.02 (d, J = 8.8 Hz,
2H-chromene-
[106877-32-1]
1H), 4.26 (q, J = 7.1 Hz, 2H),
3-carboxamide
4.02 (s, 3H), 1.47 (t, J = 7.0 Hz,
3H).
31
8-ethoxy-7-
Intermediate 5
(600 MHz, CDCl 3 ) δ 11.17 (br s,
methoxy-2-oxo-
(used in place of
1H), 8.93 (s, 1H), 8.37 (d, J = 8.2 Hz,
N-[2-
Intermediate 1) and
1H), 7.68 (d, J = 7.6 Hz, 1H),
(trifluoromethyl)phenyl]-
2-Trifluoromethyl-
7.60 (t, J = 7.8 Hz, 1H), 7.45 (d, J = 8.8 Hz,
2H-
phenylamine
1H), 7.28 (t, J = 7.5 Hz,
chromene-3-
[CAS 95-53-4]
1H), 7.01 (d, J = 8.8 Hz, 1H),
carboxamide
4.26 (q, J = 7.0 Hz, 2H), 4.01 (s,
3H), 1.47 (t, 3H).
32
8-isopropoxy-
Intermediate 4
(600 MHz, CDCl 3 ) δ 11.18 (br s,
7-methoxy-2-
(used in place of
1H), 8.93 (s, 1H), 8.38 (d, J = 8.2 Hz,
oxo-N-[2-
Intermediate 1) and
1H), 7.68 (d, J = 7.8 Hz, 1H),
(trifluoromethyl)phenyl]-
2-trifluoromethoxy-
7.60 (t, J = 7.8 Hz, 1H), 7.44 (d, J = 8.8 Hz,
2H-
phenylamine
1H), 7.28 (t, J = 7.5 Hz,
chromene-3-
[CAS 88-17-5]
1H), 7.01 (d, 1H) 4.63 (dt, J = 12.3,
carboxamide
6.2 Hz, 1H), 4.00 (s, 3 H),
1.42-1.36 (m, 7H).
33
7-methoxy-N-
2-methoxy-
(600 MHz, CDCl 3 ) δ 11.35 (s,
(2-
phenylamine
1H), 8.91 (s, 1H), 8.58 (dd, J = 1.4,
methoxyphenyl)-
[CAS 90-04-0]
8.0 Hz, 1H), 7.56 (d, J = 8.7 Hz,
2-oxo-8-
1H), 7.13-7.07 (m, 1H),
propyl-2H-
7.04-6.98 (m, 1H), 6.98-6.92 (m, 2H),
chromene-3-
3.97 (d, J = 10.3 Hz, 6H),
carboxamide
2.89-2.81 (m, 2H), 1.62 (sxt, J = 7.5 Hz,
2H), 0.99 (t, J = 7.3 Hz, 3H).
34
7-methoxy-N-
2-methylsulfanyl-
(600 MHz, CDCl 3 ) δ 11.48 (s,
[2-
phenylamine [CAS
1H), 8.94 (s, 1H), 8.52 (dd, J = 1.2,
(methylthio)phenyl]-
2987-53-3]
8.2 Hz, 1H), 7.57 (d, J = 8.7 Hz,
2-oxo-8-
1H), 7.53 (dd, J = 1.5, 7.8 Hz,
propyl-2H-
1H), 7.36-7.31 (m, 1H), 7.12 (td,
chromene-3-
J = 1.3, 7.6 Hz, 1H), 6.97 (d, J = 8.7 Hz,
carboxamide
1H), 3.97 (s, 3H),
2.86 (dd, J = 6.9, 8.5 Hz, 2H), 2.47 (s,
3H), 1.66-1.60 (m, 2H), 0.99 (t, J = 7.3 Hz,
3H).
35
N-[2-(2-
2-furan-2-yl-
(600 MHz, CDCl 3 ) δ 11.21 (s,
furyl)phenyl]-7-
phenylamine
1H), 8.93 (s, 1H), 8.36 (d, J = 7.6 Hz,
methoxy-2-oxo-
[CAS 55578-79-5]
1H), 7.65-7.62 (m, 2H),
8-propyl-2H-
7.55 (d, J = 8.7 Hz, 1H), 7.40-7.35 (m,
chromene-3-
1H), 7.22 (td, J = 1.2, 7.6 Hz,
carboxamide
1H), 6.95 (d, J = 8.7 Hz, 1H),
6.73 (d, J = 3.4 Hz, 1H), 6.57 (dd,
J = 1.8, 3.3 Hz, 1H), 3.97 (s, 3H),
2.86 (dd, J = 6.9, 8.5 Hz, 2H),
1.62 (sxt, J = 7.5 Hz, 2H), 0.99 (t,
J = 7.3, 3 H).
36
N-[4-
(4-aminophenyl)methanol
(300 MHz, DMSO-d 6 ) δ 10.90 (s,
(hydroxymethyl)phenyl]-
[CAS 623-04-1]
1H), 8.93 (s, 1H), 7.74 (d, J = 8.5 Hz,
7-
2H), 7.57 (d, J = 8.8 Hz, 1H),
methoxy-2-oxo-
7.38 (d, J = 8.5 Hz, 2H), 6.97 (d,
8-propyl-2H-
J = 7.9 Hz, 1H), 4.69 (s, 2H),
chromene-3-
3.97 (s, 3H), 2.86 (t, J = 7.8 Hz,
carboxamide
2H), 1.70-1.57 (m, 2H), 0.99 (t, J = 7.2 Hz,
3H).
37
7-methoxy-N-
N-(4-amino-3-
(300 MHz, CDCl 3 δ 11.28 (s, 1H),
{4-
(trifluoromethyl)phenyl)methanesulfonamide
8.94 (s, 1H), 8.37 (d, J = 8.7 Hz,
[(methylsulfonyl)amino]-
[CAS
1H), 7.60-7.54 (m, 2H),
2-
926228-44-6]
7.48-7.45 (m, 1H), 6.98 (d, J = 9.0 Hz, 1H),
(trifluoromethyl)phenyl}-
6.68 (s, 1H), 3.98 (s, 3H), 3.05 (s,
2-oxo-
3H), 2.85 (t, J = 7.5 Hz, 2H),
8-propyl-2H-
1.65-1.58 (m, 2H), 0.99 (t, J = 7.5 Hz,
chromene-3-
3H).
carboxamide
38
N-[4-
4-amino-3-
(300 MHz, DMSO-d 6 ) δ 11.41 (s,
(aminosulfonyl)-
bromobenzenesulfonamide
1H), 9.03 (s, 1H), 8.70-8.66 (m,
2-
[CAS
1H), 8.10-8.08 (m, 1H), 7.96 (d, J = 8.4 Hz,
bromophenyl]-
53297-69-1]
1H), 7.88-7.84 (m, 1H),
7-methoxy-2-
7.44 (s, 2H), 7.24 (d, J = 7.8 Hz,
oxo-8-propyl-
1H), 3.96 (s, 3H), 2.80-2.65 (m,
2H-chromene-
2H), 1.60-1.50 (m, 2H), 0.92 (t, J = 6.9 Hz,
3-carboxamide
3H).
39
N-[4-
4-amino-3-
(300 MHz, DMSO-d 6 ) δ 11.51 (s,
(aminosulfonyl)-
chlorobenzenesulfonamide
1H), 9.02 (s, 1H), 8.71 (d, J = 4.2 Hz,
2-
[CAS 53297-68-0]
1H), 7.96-7.94 (m, 2H),
chlorophenyl]-
7.81 (dd, J = 0.6, 4.2 Hz, 1H), 7.43 (s,
7-methoxy-2-
2H), 7.23 (d, J = 4.8 Hz, 1H),
oxo-8-propyl-
3.95 (s, 3H), 2.73 (t, J = 3.9 Hz,
2H-chromene-
2H), 1.56-1.52 (m, 2H), 0.91 (t, J = 3.6 Hz,
3-carboxamide
3H).
40
N-[4-
4-aminobenzene
(300 MHz, DMSO-d 6 ) δ 10.89 (s,
(aminosulfonyl)phenyl]-
sulfonamide
1H), 8.88 (s, 1H), 7.95-7.78 (m,
7-
[CAS 63-74-1]
5H), 7.32 (s, 2H), 7.23 (d, J = 8.8 Hz,
methoxy-2-oxo-
1H), 3.96 (s, 3H),
8-propyl-2H-
2.80-2.70 (m, 2H), 1.61-1.51 (m, 2H),
chromene-3-
0.93 (t, J = 7.4 Hz, 3H).
carboxamide
43
7-methoxy-N-
2-methoxypyridin-3-
(600 MHz, CDCl 3 ) δ 11.28 (s,
(2-
amine
1H), 8.87 (s, 1H), 8.76 (dd, J = 1.8,
methoxypyridin-
[CAS 20265-38-7]
7.8 Hz, 1H), 7.89 (dd, J = 1.8,
3-yl)-2-oxo-8-
5.4 Hz, 1H), 7.54 (d, J = 9.0 Hz,
propyl-2H-
1H), 6.95-6.91 (m, 2H),
chromene-3-
4.10 (s, 3H), 3.96 (s, 3H),
carboxamide
2.86-2.84 (m, 2H), 1.64-1.58 (m, 2H),
0.98 (t, J = 7.8 Hz, 3H).
44
7-methoxy-N-
N-(5-amino-6-
(300 MHz, DMSO-d 6 ) δ 11.10 (s,
{2-methoxy-4-
methoxypyridin-2-yl)methanesulfonamide
1H), 9.64 (br s, 1H), 8.95 (s, 1H),
[(methylsulfonyl)amino]phenyl}-
[CAS 57165-06-7]
8.37 (d, J = 8.7 Hz, 1H), 7.91 (d,
2-oxo-8-
J = 8.7 Hz, 1H), 7.21 (d, J = 8.7 Hz,
propyl-2H-
1H) 6.93 (d, J = 2.4 Hz, 1H),
chromene-3-
6.81 (dd, J = 2.4, 8.7 Hz, 1H),
carboxamide
3.94 (s, 3H), 3.87 (s, 3H), 2.96 (s,
3H), 2.73 (t, J = 6.9 Hz, 2H),
1.58-1.50 (m, 2H), 0.92 (t, J = 7.5 Hz,
3H).
45
N-(4-hydroxy-2-
4-amino-3-
(300 MHz, DMSO-d 6 ) δ 10.38 (s,
methylphenyl)-
methylphenol
1H), 9.25 (s, 1H), 8.92 (s, 1H),
7-methoxy-2-
[CAS 2835-99-6]
7.90 (d, J = 8.7 Hz, 1H), 7.82 (d,
oxo-8-propyl-
J = 8.4 Hz, 1H), 7.20 (d, J = 8.4 Hz,
2H-chromene-
1H), 6.65-6.59 (m, 2H),
3-carboxamide
3.94 (s, 3H), 2.74 (t, J = 8.1 Hz, 2H),
2.22 (s, 3H), 1.58-1.50 (m, 2H),
0.92 (t, J = 7.8 Hz, 3H).
47
N-[4-
N-(4-amino-3-
(300 MHz, CDCl 3 ) δ 11.18 (s,
(acetylamino)-
(trifluoromethyl)phenyl)acetamide
1H), 8.91 (s, 1H), 8.31 (d, J = 9.3 Hz,
2-
[CAS
1H), 7.88 (s, 1H), 7.69 (d, J = 8.7 Hz,
(trifluoromethyl)phenyl]-
1579-89-1]
1H), 7.56 (d, J = 8.7 Hz,
7-
1H), 7.32 (s, 1H), 6.97 (d, J = 8.4 Hz,
methoxy-2-oxo-
1H), 3.97 (s, 3H),
8-propyl-2H-
2.88-2.81 (m, 2H), 2.20 (s, 3H),
chromene-3-
1.65-1.58 (m, 2H), 0.98 (t, J = 7.5 Hz, 3H).
carboxamide
48
N-[2-
2-(difluoromethoxy)aniline
(300 MHz, CDCl 3 ) δ 11.37 (s,
(difluoromethoxy)phenyl]-
[CAS 22236-04-0]
1H), 8.90 (s, 1H), 8.61 (d, J = 8.1 Hz,
7-
1H), 7.56 (d, J = 8.7 Hz, 1H),
methoxy-2-oxo-
7.29-7.21 (m, 2H), 7.14-7.09 (m,
8-propyl-2H-
1H), 6.96 (d, J = 8.7 Hz, 1H),
chromene-3-
6.66 (t, J = 73.2 Hz, 1H), 3.96 (s,
carboxamide
3H), 2.85 (t, J = 7.5 Hz, 2H),
1.65-1.57 (m, 2H), 0.98 (t, J = 7.5 Hz,
3H).
51
N-[4-
N-(4-amino-3-
(300 MHz, CDCl 3 ) δ 10.81 (s,
(acetylamino)-
methylphenyl)acetamide
1H), 8.93 (s, 1H), 8.23 (d, J = 8.7 Hz,
2-
[CAS 6375-20-8]
1H), 7.57 (d, J = 8.7 Hz, 1H),
methylphenyl]-
7.51 (s, 1H), 7.26-7.24 (m, 1H),
7-methoxy-2-
7.13 (s, 1H), 6.97 (d, J = 8.7 Hz,
oxo-8-propyl-
1H), 3.97 (s, 3H), 2.86 (t, J = 7.5 Hz,
2H-chromene-
2H), 2.41 (s, 3H), 2.17 (s,
3-carboxamide
3H), 1.66-1.56 (m, 2H), 0.99 (t, J = 7.2 Hz,
3H).
54
N-(2-
3-
(300 MHz, CDCl 3 ) δ 12.85 (s,
formylpyridin-
aminopicolinaldehyde
1H), 10.19 (s, 1H), 9.27 (d, J = 8.7 Hz,
3-yl)-7-
[CAS 55234-58-7]
1H), 8.87 (s, 1H), 8.54 (d,
methoxy-2-oxo-
J = 4.5 Hz, 1H), 7.57-7.52 (m,
8-propyl-2H-
2H), 6.96 (d, J = 8.7 Hz, 1H),
chromene-3-
3.97 (s, 3H), 2.86 (t, J = 7.5 Hz,
carboxamide
2H), 1.66-1.58 (m, 2H), 0.99 (t, J = 7.2 Hz,
3H).
56
N-{2-chloro-4-
N-(4-amino-3-
(600 MHz, DMSO-d 6 ) δ 11.18 (s,
[(methylsulfonyl)amino]phenyl}-
chlorophenyl)methanesulfonamide
1H), 9.91 (s, 1H), 9.01 (s, 1H),
7-methoxy-2-
[CAS 57165-03-4]
8.45 (d, J = 9.0 Hz, 1H), 7.95 (d,
oxo-8-propyl-
J = 9.0 Hz, 1H), 7.37 (s, 1H),
2H-chromene-
7.25-7.23 (m, 2H), 3.97 (s, 3H),
3-carboxamide
3.03 (s, 3H), 2.75 (t, J = 6.6 Hz,
2H), 1.58-1.54 (m, 2H), 0.93 (t, J = 7.8 Hz,
3H).
57
7-methoxy-2-
tert-butyl 2-(((4-
(600 MHz, CDCl 3 ) δ 10.64 (s,
oxo-N-{4-
aminophenyl)amino)methyl)piperidine-
1H), 8.90 (s, 1H), 7.57-7.49 (m,
[(piperidin-2-
1-
3H), 6.96 (d, J = 8.8 Hz, 1H),
ylmethyl)amino]phenyl}-
carboxylate
6.64 (d, J = 8.8 Hz, 2H), 4.03 (br.
8-
[CAS 1159976-36-
s., 1H), 3.97 (s, 3H), 3.17 (d, J = 12.6 Hz,
propyl-2H-
9] followed by
1H), 3.13-3.08 (m, 1H),
chromene-3-
deprotection with
3.06-2.94 (m, 2H), 2.90-2.84 (m,
carboxamide
HCl in CH 2 Cl 2 .
2H), 2.82-2.75 (m, 2H), 2.64 (td,
J = 2.6, 11.8 Hz, 2H),
1.88-1.82 (m, 1H), 1.65-1.58 (m, 2H),
1.47-1.36 (m, 2H), 1.27-1.15 (m, 1H),
0.99 (t, J = 7.3 Hz, 3H).
58
7-methoxy-2-
tert-butyl 3-(((4-
(600 MHz, CDCl 3 ) δ 10.64 (s,
oxo-N-{4-
aminophenyl)amino)methyl)piperidine-
1H), 8.90 (s, 1H), 7.58-7.51 (m,
[(piperidin-3-
1-
3H), 6.96 (d, J = 8.7 Hz, 1H),
ylmethyl)amino]phenyl}-
carboxylate
6.61 (d, J = 8.8 Hz, 2H), 3.97 (s,
8-
[CAS 1159976-35-
3H), 3.22-3.14 (m, 1H), 3.03 (d, J = 12.3 Hz,
propyl-2H-
8] followed by
2H), 3.01-2.96 (m,
chromene-3-
deprotection with
2H), 2.89-2.84 (m, 2H),
carboxamide
HCl in CH 2 Cl 2
2.63-2.57 (m, 1H), 2.40 (dd, J = 10.4, 11.7 Hz,
1H), 1.92 (dt, J = 1.8, 13.0 Hz,
1H), 1.80 (ddd, J = 3.6, 7.0,
13.9 Hz, 1H), 1.77-1.71 (m, 1H),
1.71-1.68 (m, 1H), 1.66-1.59 (m,
2H), 1.55-1.44 (m, 1H), 1.18 (qd,
J = 3.8, 12.0 Hz, 1H), 0.99 (t, J = 7.3 Hz,
3H).
59
7-methoxy-2-
tert-butyl 3-((4-
(300 MHz, CDCl 3 ) δ 10.66 (s,
oxo-8-propyl-N-
aminophenyl)amino)pyrrolidine-
1H), 8.91 (s, 1H), 7.56 (d, J = 4.4 Hz,
[4-(pyrrolidin-3-
1-
1H), 7.54 (d, J = 4.7 Hz, 2H),
ylamino)phenyl]-
carboxylate
6.96 (d, J = 8.8 Hz, 1H), 6.63 (d,
2H-chromene-
[CAS 1159976-32-
J = 8.8 Hz, 2H), 4.00-3.97 (m,
3-carboxamide
5] followed by
1H), 3.97 (s, 3H), 3.61 (q, J = 7.2 Hz,
deprotection with
1H), 3.18 (dd, J = 5.9, 11.4 Hz,
HCl in CH 2 Cl 2 .
1H), 3.13 (ddd, J = 7.1, 7.5,
10.6 Hz, 1H), 2.98 (ddd, J = 6.0,
8.3, 10.9 Hz, 1H), 2.90 (dd, J = 2.9,
11.4 Hz, 1H), 2.88-2.85 (m,
2H), 2.23-2.16 (m, 1H),
1.65-1.58 (m, 2H), 1.00 (t, J = 7.3 Hz, 3H).
60
7-methoxy-2-
tert-butyl 3-((4-
(600 MHz, CDCl 3 ) δ 10.64 (s,
oxo-N-[4-
aminophenyl)amino)piperidine-
1H), 8.90 (s, 1H), 7.54 (dd, J = 8.8,
(piperidin-3-
1-
14.4 Hz, 3H), 6.96 (d, J = 8.7 Hz,
ylamino)phenyl]-
carboxylate
1H), 6.64 (d, J = 9.0 Hz, 2H),
8-propyl-2H-
[CAS 1159976-34-
3.97 (s, 3H), 3.45 (d, J = 3.2 Hz,
chromene-3-
7] followed by
1H), 3.23 (dd, J = 2.4, 11.6 Hz,
carboxamide
deprotection with
1H), 2.94-2.88 (m, 1H),
HCl in CH 2 Cl 2 .
2.88-2.84 (m, 2H), 2.76-2.70 (m, 1H),
2.58 (dd, J = 7.6, 11.3 Hz, 1H),
1.98-1.92 (m, 1H), 1.80-1.70 (m, 5H),
1.62 (dq, J = 7.5, 15.0 Hz, 2H),
1.58-1.48 (m, 2H), 0.99 (t, J = 7.3 Hz,
3H).
61
(3S)-3-amino-4-
(S)-4-(tert-butoxy)-2-
(300 MHz, CDCl 3 ) δ 10.82 (s,
[(4-{[(7-
((tert-
1H), 9.48 (s, 1H), 8.95 (s, 1H),
methoxy-2-oxo-
butoxycarbonyl)amino)-
8.26 (d, J = 8.9 Hz, 1H),
8-propyl-2H-
4-oxobutanoic
7.64-7.60 (m, 1H), 7.58 (d, J = 8.8 Hz,
chromen-3-
acid
1H), 7.42-7.34 (m, 1H), 6.98 (d, J = 8.6 Hz,
yl)carbonyl]amino}-
[CAS 3057-74-7]
1H), 3.98 (s, 3H),
3-
followed by the
3.84-3.73 (m, 1H), 3.69-3.62 (m, 1H),
methylphenyl)amino]-
deprotection with
2.93-2.80 (m, 2H), 2.73-2.60 (m,
4-
HCl in CH 2 Cl 2 .
1H), 2.43 (s, 3H), 1.69-1.59 (m,
oxobutanoic
2H), 1.00 (t, J = 7.3 Hz, 3H).
acid
62
(4R)-4-amino-5-
(R)-5-(tert-butoxy)-2-
(600 MHz, DMSO-d 6 , 1-drop of
[(4-{[(7-
((tert-
AcOD-d 4 ) δ 8.93 (s, 1H), 8.18 (d,
methoxy-2-oxo-
butoxycarbonyl)amino)-
J = 8.7 Hz, 1H), 7.85 (d, J = 8.7),
8-propyl-2H-
5-oxopentanoic
7.48 (s, 1H), 7.46 (d, J = 8.8 Hz,
chromen-3-
acid
1H), 7.16 (d, J = 8.7 Hz, 1H),
yl)carbonyl]amino}-
[CAS 104719-63-3]
3.96 (t, J = 6.5 Hz, 1H), 3.93 (s,
3-
followed by the
3H), 2.74 (t, J = 7.5 Hz, 2H),
methylphenyl)amino]-
deprotection with
2.41-2.37 (m, 2H), 2.32 (s, 3 H),
5-
HCl in CH 2 Cl 2 .
2.08 (q, J = 7.3 Hz, 2H),
oxopentanoic
1.58-1.49 (m, 2H), 0.91 (t, 3H).
acid
63
N-[4-
Intermediate 3
(300 MHz, DMSO-d 6 ) δ 10.89 (s,
(aminosulfonyl)-
(used in place of
1H), 8.99 (s, 1H), 8.42 (d, J = 8.2 Hz,
2-
Intermediate 1) and
1H), 7.79 (d, J = 9.1 Hz, 1H),
methylphenyl]-
4-amino-3-
7.73-7.71 (m, 1H), 7.71-7.66 (m,
7,8-diethoxy-2-
methylbenzenesulfonamide
1H), 7.23-7.28 (m, 3H), 4.24 (q, J = 6.9 Hz,
oxo-2H-
[CAS
2H), 4.12 (q, J = 7.0 Hz,
chromene-3-
53297-70-4]
2H), 2.41 (s, 3H), 1.39 (t, J = 7.0 Hz,
carboxamide
3H), 1.32 (t, J = 7.0 Hz, 3H).
64
N-[4-
Intermediate 5
(300 MHz, DMSO-d 6 ) δ 10.88 (s,
(aminosulfonyl)-
(used in place of
1H), 9.00 (s, 1H), 8.42 (d, J = 8.2 Hz,
2-
Intermediate 1) and
1H), 7.81 (d, J = 9.1 Hz, 1H),
methylphenyl]-
4-amino-3-
7.74-7.69 (m, 1H), 7.67 (d, J = 1.8 Hz,
8-ethoxy-7-
methylbenzenesulfonamide
1H), 7.28 (s, 1H), 7.26 (s,
methoxy-2-oxo-
[CAS 53297-70-4
2H), 4.11 (q, J = 7.0 Hz, 2H),
2H-chromene-
3.96 (s, 3H), 2.41 (s, 3H), 1.32 (t,
3-carboxamide
J = 7.0 Hz, 3H).
65
N-[4-
8-isopropoxy-7-
(300 MHz, DMSO-d 6 ) δ 10.90 (s,
(aminosulfonyl)-
methoxy-2-oxo-2H-
1H), 9.00 (s, 1H), 8.43 (d, J = 8.5 Hz,
2-
chromene-3-
1H), 7.81 (d, J = 9.1 Hz, 1H),
methylphenyl]-
carboxylic acid and
7.73-7.69 (m, 1H), 7.68-7.66 (m,
8-isopropoxy-
4-amino-3-
1H), 7.28 (m, 1H), 7.25 (s, 2H),
7-methoxy-2-
methylbenzenesulfonamide
4.50-4.40 (m, 1H), 3.95 (s, 3H),
oxo-2H-
[CAS 53297-70-4]
2.41 (s, 3H), 1.28 (d, J = 6.2 Hz,
chromene-3-
6H).
carboxamide
69
7,8-diethoxy-N-
Intermediate 3
(300 MHz, CDCl 3 ) δ11.20 (s, 1H),
{4-
(used in place of
8.94 (s, 1H), 8.29 (d, J = 9.0 Hz,
[(methylsulfonyl)amino]-
Intermediate 1) and
1H), 7.56 (d, J = 2.4 Hz, 1H),
2-
N-(4-amino-3-
7.46-7.42 (m, 2H), 6.99 (d, J = 9.0 Hz,
(trifluoromethyl)phenyl}-
(trifluoromethyl)phenyl)methanesulfonamide
1H), 6.94 (s, 1H),
2-oxo-
[CAS 926228-44-6]
4.28-4.20 (m, 4H), 3.05 (s, 3H),
2H-chromene-
1.55-1.43 (m, 6H).
3-carboxamide
70
7-methoxy-2-
2-trifluoromethoxy-
(600 MHz, CDCl 3 ) δ 11.41 (s,
oxo-8-propyl-N-
phenylamine
1H), 8.92 (s, 1H), 8.65 (dd, J = 1.3,
[2-
[CAS 1535-75-7]
8.2 Hz, 1H), 7.57 (d, J = 8.7 Hz,
(trifluoromethoxy)phenyl]-
1H), 7.38-7.30 (m, 2H),
2H-
7.18-7.11 (m, 1H), 6.97 (d, J = 8.7 Hz,
chromene-3-
1H), 3.98 (s, 3H), 2.89-2.84 (m,
carboxamide
2H), 1.62 (sxt, J = 7.5 Hz, 2H),
1.00-0.97 (m, 2H).
71
N-[4-
Intermediate 2
(300 MHz, DMSO-d 6 ) δ 10.93 (s,
(aminosulfonyl)-
(used in place of
1H), 9.01 (s, 1H), 8.44 (d, J = 8.2 Hz,
2-
Intermediate 1) and
1H), 7.95 (d, J = 8.8 Hz, 1H),
methylphenyl]-
4-amino-3-
7.74-7.65 (m, 2H), 7.28-7.20 (m,
8-ethyl-7-
methylbenzenesulfonamide
3H), 3.97 (s, 3H), 2.84-2.74 (m,
methoxy-2-oxo-
[CAS 53297-70-4]
2H), 2.41 (s, 3H), 1.12 (t, J = 7.5 Hz,
2H-chromene-
3H).
3-carboxamide
72
N-[4-
4-amino-3-
(300 MHz, DMSO-d 6 ) δ 11.48 (s,
(aminosulfonyl)-
trifluoromethylbenzenesulfonamide
1H), 8.73 (s, 1H), 7.94 (d, J = 2.4 Hz,
2-
[CAS 39234-84-9]
1H), 7.84-7.79 (m, 2H),
(trifluoromethyl)phenyl]-
7.18 (d, J = 9.3 Hz, 1H), 6.90 (d, J = 8.7 Hz,
7-
1H), 6.73 (s, 1H), 3.92 (s,
methoxy-2-oxo-
1H), 2.69 (t, J = 7.8 Hz, 2H),
8-propyl-2H-
1.54-1.47 (m, 2H), 0.88 (t, J = 7.8 Hz,
chromene-3-
3H).
carboxamide
EXAMPLE 6
Compound 17
N-(2-Ethylpyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide
[0365] Step 1: A mixture of 2-bromo-3-nitropyridine [CAS 19755-53-4] (0.600 g, 2.90 mmol), LiCl (0.80 g, 0.019 mmol), PdCl 2 (PPh 3 ) 2 (0.20 g, 0.280 mmol) and tributyl(vinyl)stannane (1.0 g, 3.42 mmol) in DMF (5 mL) was heated at 90° C. overnight. After standard aqueous work up, the crude was purified by MPLC using (10% EtOAC/Hexanes) and gave a yellow oil.
[0366] Step 2: The yellow oil (0.25 g, 2.08 mmol) was hydrogenated at 50 psi over 10% Pd/C in MeOH (10 mL) for 16 hours. The mixture was then filtered and purified by MPLC using (5% MeOH in CH 2 Cl 2 ) to give 2-ethylpyridin-3-amine as a solid.
[0367] Step 3: 2-Ethylpyridin-3-amine was substituted in the method used in Example 1.
[0368] 1 H NMR (300 MHz, CDCl 3 ) δ 11.03 (s, 1H), 8.94 (s, 1H), 8.64 (d, J=8.1 Hz, 1H), 8.34 (d, J=4.8 Hz, 1H), 7.59 (d, J=8.7 Hz, 1H), 7.20 (dd, J=4.8, 8.4 Hz, 1H), 6.99 (d, J=8.7 Hz, 1H), 3.98 (s, 3H), 3.00 (q, J=7.5 Hz, 2H), 2.87 (t, J=7.8 Hz, 2H), 1.67-1.59 (m, 2H), 1.40 (t, J=7.5 Hz, 3H), 1.00 (t, J=7.5 Hz, 3H).
EXAMPLE 7
Compound 21
(4-{[(7-Methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)phosphonic acid
[0369] Step 1: A solution of 4-iodo-2-methylaniline [CAS 13194-68-8] (0.51 g, 2.21 mmol), diethyl phosphonate (0.30 mL, 2.32 mmol), TEA (0.325 mL, 2.33 mmol), Pd(PPh 3 ) 4 (cat.) was heated at 90° C. overnight. The solution was cooled to room temperature and EtOAc was added. After standard aqueous work up, the crude was purified by MPLC (30-50% EtOAc/Hexanes) and used in the next step.
[0370] Step 2: Diethyl (4-amino-3-methylphenyl)phosphonate was substituted in the method used in Example 1.
[0371] Step 3: A solution of the previous amide from Step 2 (0.08, 0.164 mmol), bromotrimethylsilane (0.55 g, 3.41 mmol) in CH 3 CN (5 mL) was heated at 80° C. overnight. After solution was allowed to cool to room temperature, evaporation to remove volatiles was done. The residue was purified by MPLC (NH 3 /MeOH) followed by trituration in CHCl 3 then MeOH to give Compound 21 as a yellow solid.
[0372] 1 H NMR (600 MHz, d-TFA) δ 9.32 (s, 1H), 8.24 (br s, 1H), 7.95-7.89 (m, 2H), 7.87 (d, J=9.0 Hz, 1H), 7.29 (d, J=8.4 Hz, 1H), 4.14 (s, 3H), 3.02 (t, J=6.6 Hz, 2H), 2.59 (s, 3H), 1.78-1.70 (m, 2H), 1.08 (t, J=7.2 Hz, 3H).
EXAMPLE 8
Compound 25
(3-Chloro-4-{[(7-methoxy-2-oxo-8-propyl-2H -chromen -3-yl)carbonyl]amino}phenyl)boronic acid
[0373] Step 1: 2-Chloro-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline [CAS 721960-43-6] is substituted in the method used in Example 1.
[0374] Step 2: To a mixture of the amide from Step 1 (0.15 g, 0.302 mmol) in THF/MeOH/H 2 O was added NaIO 4 (0.22 g, 1.03 mmol) at room temperature with stirring for 30 minutes. 1N HCl (0.30 mL, 0.30 mmol) was then added and stirring was allowed for 2 days. After 2 days water was added and the solid was filtered. The solid was washed with EtOAc and purified by MPLC (5% MeOH/CH 2 Cl 2 ) to give the title compound.
[0375] 1 H NMR (300 MHz, DMSO-d 6 ) δ 11.32 (s, 1H), 8.99 (s, 1H), 8.54-8.46 (m, 1H), 8.17 (s, 2H), 7.96-7.86 (m, 2H), 7.76-7.74 (m, 1H), 7.24-7.16 (m, 1H), 3.94 (s, 3H), 2.80-2.65 (m, 2H), 1.65-1.45 (m, 2H), 1.0-0.84 (m, 3H).
EXAMPLE 9
Compound 41
N-(4-Amino-2-methylphenyl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide
[0376] Step 1: tert-Butyl (4-amino-3-methylphenyl)carbamate [CAS 325953-41-1] was substituted in the method used in Example 1.
[0377] Step 2: The compound from Step 1 (0.48 g, 1.03 mmol) in CH 2 Cl 2 (25 mL) was treated with 4.0 M HCl in Dioxane (3.40 mL, 13.6 mmol) at room temperature and stirred overnight. The solution was evaporated and then triturated with ether followed by filtration to give the title compound.
[0378] 1 H NMR (300 MHz, DMSO-d 6 ) δ 0.70 (s, 1H), 8.96 (s, 1H), 8.23 (d, J=9.6 Hz, 1H), 7.93 (d, J=8.7 Hz, 1H), 7.24-7.16 (m, 3H), 3.95 (s, 3H), 3.55 (br s, 3H), 2.73 (t, J=8.1 Hz, 2H), 2.34 (s, 3H), 1.56-1.53 (m, 2H), 0.92 (t, J=7.5 Hz, 3H).
EXAMPLE 10
Compound 42
N-(6-Amino-2-methylpyridin-3-yl)-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide
[0379] Step 1: 6-Methyl-5-nitropyridin-2-amine [CAS 22280-62-2] (0.38 g, 2.48 mmol) was hydrogenated at 50 psi with 10% Pd/C (0.35 g) in MeOH/THF (10 mL) overnight to give 6-methylpyridine-2,5-diamine as a light yellow solid.
[0380] Step 2: 6-methylpyridine-2,5-diamine was substituted in the method used in Example 1. 1 H NMR (300 MHz, CDCl 3 ) δ 10.61 (s, 1H), 8.90 (s, 1H), 8.15 (d, J=8.7 Hz, 1H), 7.56 (d, J=8.7 Hz, 1H), 6.97 (d, J=8.7 Hz, 1H), 6.43 (d, J=9.0 Hz, 1H), 4.39 (br s, 2H), 3.97 (s, 3H), 2.88-2.84 (m, 2H), 2.48 (s, 3H), 1.70-1.60 (m, 2H), 0.99 (t, J=7.2 Hz, 3H).
EXAMPLE 11
Compound 46
7-Methoxy-N-{2-methyl-6-[(methylsulfonyl)amino]pyridin-3-yl}-2-oxo-8-propyl-2H-chromene-3-carboxamide
[0381] Compound 42 (0.20 g, 0.545 mmol) was treated with TEA (0.15 mL, 1.08 mmol) and methanesulfonyl chloride (0.90 mL) in DMF (20 mL) at 0° C. The reaction was stirred overnight at room temperature then heated to 40° C. overnight. After standard aqueous workup, the crude was purified by MPLC (50% EtOAc/Hexanes) to give the title compound.
[0382] 1 H NMR (600 MHz, DMSO-d 6 ) δ 10.55 (s, 1H), 10.39 (s, 1H), 8.93 (s, 1H), 8.27 (d, J=9.0 Hz, 1H), 7.90 (d, J=9.0 Hz, 1H), 7.20 (d, J=9.0 Hz, 1H), 6.87 (d, J=7.8 Hz, 1H), 3.94 (s, 3H), 3.29 (s, 3H), 2.73 (t, 7.8, 2H), 2.44 (s, 3H), 1.56-1.52 (m, 2H), 0.90 (t, J=7.8 Hz, 3H).
[0383] Compounds 49, 52 and 53 were prepared in a similar manner to the method described in Example 11 for Compound 46. The reagents used and the results are described below in Table 2.
[0000]
TABLE 2
Compound
1 H NMR δ (ppm) for
number
IUAPC name
Reagent (s) used
Compound
49
N-{4-
Compound 41 was
(300 MHz; CDCl 3 ) δ 10.86 (s,
[(ethylsulfonyl)amino]-
used in place of
1H), 8.95 (s, 1H), 8.23 (d, J = 8.4 Hz,
2-
Compound 42
1H), 7.59 (d, J = 8.7 Hz,
methylphenyl}-
Ethanesulfonyl
1H), 7.15 (d, J = 2.4 Hz, 1H),
7-methoxy-2-
chloride was used in
7.08 (dd, J = 2.4, 8.4 Hz, 1H),
oxo-8-propyl-
place of
6.98 (d, J = 9.0 Hz, 1H),
2H-chromene-
methanesulfonyl
6.54 (s, 1H), 3.98 (s, 3H), 3.12 (q, J = 7.5 Hz,
3-carboxamide
chloride
2H), 2.88-2.84 (m,
2H), 2.41 (s, 3H), 1.70-1.57 (m,
2H), 1.38 (t, J = 7.2 Hz, 3H),
0.99 (t, J = 7.2 Hz, 3H).
52
7-methoxy-N-
Compound 41 was
(300 MHz, DMSO-d 6 ) δ 10.58
{2-methyl-4-
used in place of
(s, 1H), 9.60 (br s, 1H), 8.94 (s,
[(methylsulfonyl)amino]phenyl}-
Compound 42
1H), 8.08 (d, J = 8.1 Hz, 1H),
2-oxo-8-
7.90 (d, J = 8.7 Hz, 1H),
propyl-2H-
7.20 (d, J = 8.7 Hz, 1H),
chromene-3-
7.08-7.04 (m, 2H), 3.94 (s, 3H), 2.93 (s,
carboxamide
3H), 2.80-2.70 (m, 2H), 2.28 (s,
3H), 2.60-2.50 (m, 2H), 0.90 (t,
J = 7.2 Hz, 3H).
53
4-{[(7-methoxy-
Compound 45 was
(300 MHz, CDCl 3 ) δ 10.94 (s,
2-oxo-8-propyl-
used in place of
1H), 8.94 (s, 1H), 8.40 (d, J = 9.3 Hz,
2H-chromen-3-
Compound 42
1H), 7.58 (d, J = 8.7 Hz,
yl)carbonyl]amino}-
1H), 7.18-7.15 (m, 2H), 6.98 (d,
3-
J = 9.0 Hz, 1H), 3.98 (s, 3H),
methylphenyl
3.14 (s, 3H), 2.86 (t, J = 7.5 Hz,
methanesulfonate
2H), 2.45 (s, 3H), 1.66-1.59 (m,
2H), 0.99 (t, J = 7.2 Hz, 3H).
EXAMPLE 12
Compound 50
N-[4-Hydroxy-2-(trifluoromethyl)phenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide
[0384] Step 1: 4-amino-3-(trifluoromethyl)phenol [CAS 445-04-5] (0.292 g, 1.65 mmol), imidazole (0.280 g, 4.11 mmol), and tert-butylchlorodimethylsilane (0.36 g, 2.32 mmol) in DMF (5 mL) were stirred at room temperature overnight. After standard aqueous work up, the crude was purified by MPLC using (10% EtOAc/Hexanes) to give an orange oil.
[0385] Step 2: 4-((tert-butyldimethylsilyl)oxy)-2-(trifluoromethyl)aniline was substituted in the method used in Example 1.
[0386] Step 3: The compound from Step 2 (0.23 g, 0.430 mmol) in THF (5 mL) was treated with 1.0 M TBAF (0.480 mL, 0.480 mmol) solution in THF at 0° C. for 30 minutes. Solvent was removed and residue was purified by MPLC (40% EtOAc/Hexanes) to give the title compound.
[0387] 1 H NMR (300 MHz, DMSO-d 6 ) δ 10.71 (s, 1H), 10.08 (s, 1H), 8.97 (s, 1H), 7.94-7.91 (m, 2H), 7.21 (d, J=8.7 Hz, 1H), 7.09-7.07 (m, 2H), 3.95 (s, 3H), 2.75-2.70 (m, 2H), 1.58-1.50 (m, 2H), 0.91 (t, J=7.2 Hz, 3H).
Example 13
Compound 55
7-Methoxy-N-{2-methyl-4-[(methylsulfonyl)methyl]phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide
[0388] Step 1: 4-(Bromomethyl)-2-methyl-1-nitrobenzene [CAS 141281-38-1] (1.45 g, 6.11 mmol) was added as a solid to sodium methanethiolate (0.50 g, 6.78 mmol) in DMF at 0° C. The reaction mixture was slowly warmed to room temperature overnight. After aqueous work up, crude was purified by MPLC (7.5% EtOAc/Hexanes) to give an oil which was used in the next step.
[0389] Step 2: To methyl(3-methyl-4-nitrobenzyl)sulfane (0.840 g, 4.26 mmol) in CH 2 Cl 2 (15 mL) was added m-CPBA (3.0 eq) at room temperature for 2 hours. After aqueous work up, crude was purified by MPLC (60% EtOAc/Hexanes) which was used in the next step.
[0390] Step 3: The previous compound from step 2, was hydrogenated at 50 psi with 10% Pd/C (0.084 g) in MeOH/THF (30 mL) for 3.5 hours. The reaction mixture was filtered and purified by MPLC (1% MeOH/CH 2 Cl 2 ) to give 2-methyl-4((methylsulfonyl) methyl) aniline as a light orange solid.
[0391] Step 4: 2-methyl-4-((methylsulfonyl)methyl)aniline was substituted in the method used in Example 1.
[0392] 1 H NMR (300 MHz, DMSO-d 6 ) δ 10.74 (s, 1H), 8.98 (s, 1H), 8.24 (d, J=7.8 Hz, 1H), 7.93 (d, J=9.3 Hz, 1H), 7.29-7.21 (m, 3H), 4.41 (s, 2H), 3.95 (s, 3H), 2.89 (s, 3H), 2.80-2.71 (m, 2H), 2.34 (s, 3H), 1.60-1.50 (m, 2H), 0.92 (t, J=7.2 Hz, 3H).
EXAMPLE 14
Compound 66
N-[4-(Aminosulfonyl)-2-methylphenyl]-7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamide
[0393] To a solution of Intermediate 1 (0.10 g, 0.381 mmol) in CH 2 Cl 2 (5.0 mL) was added diisopropyl ethyl amine (0.1 mL, 0.572 mmol) and a 50% solution of propylphosphonic anhydride in ethyl acetate (0.340 mL, 0.572 mmol). The mixture was stirred for 30 minutes at room temperature. 4-Amino-3-methylbenzenesulfonamide [CAS # 53297-70-4] (0.071 g, 0.381 mmol) was added to the reaction mixture at room temperature and stirred overnight. The reaction mixture was then poured onto ice water (25 mL) and CH 2 Cl 2 (25 mL) added. The organic layer was separated and washed with brine (25 mL), dried with Na 2 SO 4 , filtered and concentrated to dryness. The residue was triturated with CH 2 Cl 2 /Hexanes and then the solid was purified with a MPLC to give the title compound as a white solid.
[0394] 1 H NMR (300 MHz, DMSO-d 6 ) δ 10.95 (s, 1H), 9.03 (s, 1H), 8.46 (d, J=8.5 Hz, 1H), 7.97 (d, J=9.1 Hz, 1H), 7.79-7.65 (m, 2H), 7.33-7.18 (m, 3H), 3.98 (s, 3H), 2.81-2.71 (m, 2H), 2.43 (s, 3H), 1.64-1.50 (m, 2H), 0.94 (t, J=7.4 Hz, 3H).
EXAMPLE 15
Compound 67
3-{[(4-{[(7-Methoxy-2-oxo-8-propyl-2H-chromen-3-yl)carbonyl]amino}-3-methylphenyl)sulfonyl]amino}propanoic acid
[0395] Step 1: To a solution of 7-methoxy-N-(2-methylphenyI)-2-oxo-8-propyl-2H-chromene-3-carboxamide prepared following the procedure in WO2009019167 (0.104 g, 0.296 mmol) in CH 2 Cl 2 (5.0 mL) was added chlorosulfonic acid (0.196 mL, 2.96 mmol) in CH 2 Cl 2 (1.5 mL) dropwise at 0° C. The mixture was allowed to warm to room temperature and stirred overnight. The reaction mixture was cooled to 0° C. and carefully quenched with ice water (25 mL) and diluted with CH 2 Cl 2 (25 mL). The organic layer is separated and washed with brine (25 mL), dried with Na 2 SO 4 , filtered and concentrated to dryness. The yellow solid, 4-(7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamido)-3-methylbenzene-1-sulfonyl chloride was used as such in the next steps.
[0396] Step 2: To a solution of 4-(7-methoxy-2-oxo-8-propyl-2H-chromene-3-carboxamido)-3-methylbenzene-1-sulfonyl chloride (0.054 g, 0.122 mmol) in THF (7.0 mL) was added tert-butyl-3-aminopropanoate hydrochloride (0.028 g, 0.152 mmol) and diisopropylethylamine (0.086 mL, 0.500 mmol). After stirring at room temperature over night the solvent was concentrated to dryness and re-dissolved in CH 2 Cl 2 and washed with water. The organic layer was separated and dried with Na 2 SO 4 , filtered and concentrated to dryness to give a white solid.
[0397] 1 H NMR (300 MHz, DMSO-d 6 ) δ 10.97 (s, 1H), 9.02 (s, 1H), 8.50 (d, J=8.8 Hz, 1H), 7.96 (d, J=8.8 Hz, 1H), 7.69 (br s, 2H), 7.65 (s, 1H), 7.24 (d, J=8.8 Hz, 1H), 3.96 (s, 3H), 2.87-2.96 (m, 2H), 2.79-2.70 (m, 2H), 2.42 (s, 3H), 2.33 (t, J=7.3 Hz, 2H), 1.60-1.48 (m, 2H), 1.37 (s, 9H), 0.92 (t, J=7.3 Hz, 3H).
[0398] Step 3: The solid was dissolved in CH 2 Cl 2 (4.5 mL) and treated with TFA (0.5 mL). After stirring at room temperature for 5 hours the solvent was concentrated to dryness to give the title compound as a yellow solid.
[0399] 1 H NMR (300 MHz, DMSO-d 6 ) δ 10.91 (s, 1H), 8.96 (s, 1H), 8.44 (d, J=8.2 Hz, 1H), 7.91 (d, J=10.0 Hz, 1H), 7.64 (br s, 1H), 7.60 (s, 1H), 7.50 (t, J=6.0 Hz, 1H), 7.18 (d, J=10.0 Hz, 1H), 3.91 (s, 3H), 2.92-2.82 (m, 2H), 2.64-2.73 (m, 2H), 2.37 (s, 4H), 2.34-2.20 (m, 3H), 1.57-1.43 (m, 2H), 0.87 (t, J=7.5 Hz, 3H).
EXAMPLE 16
Compound 68
7-Methoxy-N-{2-methyl-4-[(methylamino)sulfonyl]phenyl}-2-oxo-8-propyl-2H-chromene-3-carboxamide
[0400] Compound 68 was prepared by substituting methylamine in Step 2 in the method of Example 15 for Compound 67.
[0401] 1 H NMR (300 MHz, DMSO-d 6 ) δ 10.97 (s, 1H), 9.01 (s, 1H), 8.50 (d, J=8.8 Hz, 1H), 7.96 (d, J=8.5 Hz, 1H), 7.67 (s, 1H), 7.64 (s, 1H), 7.32 (d, J=4.7 Hz, 1H), 7.24 (d, J=9.1 Hz, 1H), 3.96 (s, 3H), 2.74 (t, J=7.0 Hz, 2H), 2.42 (s, 3H), 1.62-1.49 (m, 2H), 0.92 (t, J=7.3 Hz, 3H).
EXAMPLE 17
GTP γ 35 S Binding Assay
[0402] The S1P1 activity of the compounds according to the invention, were tested using the GTP γ 35 S binding assay. The compounds were assessed for their ability to activate or block activation of the human S1P1 receptor in cells stably expressing the S1P1 receptor. Some of the results are presented in Table 3.
[0403] GTP γ 35 S binding was measured in the medium containing (mM) HEPES 25, pH 7.4, MgCl 2 10, NaCl 100, dithitothreitol 0.5, digitonin 0.003%, 0.2 nM GTP γ 35 S, and 5 μg membrane protein in a volume of 150 μl. Test compounds were included in the concentration range from 0.08 to 5,000 nM unless indicated otherwise. Membranes were incubated with 100 μM 5′-adenylylimmidodiphosphate for 30 min, and subsequently with 10 μM GDP for 10 min on ice. Drug solutions and membrane were mixed, and then reactions were initiated by adding GTP γ 35 S and continued for 30 min at 25° C. Reaction mixtures were filtered over Whatman GF/B filters under vacuum, and washed three times with 3 mL of ice-cold buffer (HEPES 25, pH7.4, MgCl 2 10 and NaCl 100). Filters were dried and mixed with scintillant, and counted for 35 S activity using a β-counter. Agonist-induced GTP γ 35 S binding was obtained by subtracting that in the absence of agonist. Binding data were analyzed using a non-linear regression method. In case of antagonist assay, the reaction mixture contained 10 nM S1P in the presence of test antagonist at concentrations ranging from 0.08 to 5000 nM.
[0404] Activity potency: S1P1 receptor from GTP γ 35 S:nM, (EC 50 ),
[0000]
TABLE 3
Compound
EC 50
number
IUPAC name
(nM)
6
N-(3-bromopyridin-4-yl)-7-methoxy-2-oxo-8-
19.0
propyl-2H-chromene-3-carboxamide
5
N-(2-bromophenyl)-7-methoxy-2-oxo-8-propyl-2H-
26.4
chromene-3-carboxamide
62
(4R)-4-amino-5-[(4-{[(7-methoxy-2-oxo-8-propyl-
3.1
2H-chromen-3-yl)carbonyl]amino}-3-
methylphenyl)amino]-5-oxopentanoic acid
38
N-[4-(aminosulfonyl)-2-bromophenyl]-7-methoxy-2-
3.5
oxo-8-propyl-2H-chromene-3-carboxamide
49
N-[4-(aminosulfonyl)-2-methylphenyl]-7-methoxy-
14.3
2-oxo-8-propyl-2H-chromene-3-carboxamide
EXAMPLE 18
Lymphopenia Assay in Mice
[0405] Test drugs are prepared in a solution containing 3% (w/v) 2-hydroxy propyl β-cyclodextrin (HPBCD) and 1% DMSO to a final concentration of 1 mg/ml, and subcutaneously injected to female C57BL6 mice (CHARLES RIVERS) weighing 20-25 g at the dose of 10 mg/Kg. Blood samples are obtained by puncturing the submandibular skin with a Goldenrod animal lancet at 5, 24, 48, 72, and 96 hrs post drug application. Blood is collected into microvettes (SARSTEDT) containing EDTA tripotassium salt. Lymphocytes in blood samples are counted using a HEMAVET Multispecies Hematology System, HEMAVET HV950FS (Drew Scientific Inc.).
[0406] (Hale, J. et al Bioorg. & Med. Chem. Lett. 14 (2004) 3351).
|
The present invention relates to novel 2-oxo-2H-chromene-3-carboxamide derivatives, processes for preparing them, pharmaceutical compositions containing them and their use as pharmaceuticals as modulators of sphingosine-1-phosphate receptors.
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INCORPORATION BY REFERENCE TO ANY PRIORITY APPLICATIONS
[0001] Any and all applications for which a foreign or domestic priority claim is identified in the Application Data Sheet as filed with the present application are hereby incorporated by reference under 37 CFR 1.57.
TECHNICAL FIELD
[0002] The invention pertains to a mobile robot for cleaning a floor or other surface. In particular, the invention pertains to a robot configured to implement a class of trajectories designed to efficiently scrub or otherwise clean the floor.
BACKGROUND
[0003] From their inception, robots have been designed to perform tasks that people prefer not to do or cannot do safely. Cleaning and vacuuming, for example, are just the type of jobs that people would like to delegate to such mechanical helpers. The challenge, however, has been to design robots that can clean the floor of a home well enough to satisfy the exacting standards of the people the live in it. Although robots have been designed to vacuum floors, robots designed to perform mopping present unique challenges. In particular, such a robot should be able to dispense cleaning solution, scrub the floor with the solution, and then effectively remove the spent cleaning solution. Robots tend to perform unsatisfactorily, however, because hard deposits on the floor may require time for the cleaning solution to penetrate and removal of the dirty solution may leave streak marks on the floor. There is therefore a need for a cleaning robot able to implement a cleaning plan that enables the robot to apply cleaning solution, repeatedly scrub the floor with the solution, and leave the floor free of streak marks.
SUMMARY
[0004] The present invention pertains to a mobile robot configured to travel across a residential floor or other surface while cleaning the surface with a cleaning pad and cleaning solvent. The robot includes a controller for managing the movement of the robot as well as the treatment of the surface with a cleaning solvent. The movement of the robot can be characterized by a class of trajectories that achieve effective cleaning. These trajectories seek to: maximize usage of the cleaning solvent, reduce streaking, utilize absorption properties of the pad, and use as much of the surface of the pad as possible. In an exemplary embodiment, the trajectory may include an oscillatory motion with a bias in a forward direction by repeatedly moving forward a greater distance than backward. In the same exemplary embodiment, the cleaning pad is a disposable sheet impregnated with solvent that is then applied to and recovered from the surface by means of the trajectory.
[0005] In one embodiment, the cleaning robot includes a cleaning assembly; a path planner for generating a cleaning trajectory; and a drive system for moving the robot in accordance with the cleaning trajectory. The cleaning trajectory is a sequence of steps or motions that are repeated a plurality times in a prescribed order to effectively scrub the floor. Repetition of the sequence, in combination with the forward and back motion, causes the cleaning assembly to pass of areas of the floor a plurality of times while allowing time for the cleaning solution to penetrate dirt deposits.
[0006] The sequence repeated by the cleaning trajectory preferably comprises: (i) a first path for guiding the robot forward and to the left; (ii) a second path for guiding the robot backward and to the right; (iii) a third path for guiding the robot forward and to the right; and (iv) a fourth path for guiding the robot backward and to the left. The first path and third path result in a longitudinal displacement of the robot (movement parallel to the direction of progression) referred to as a first distance forward, and the second path and fourth path result in a longitudinal displacement referred to as a second distance backward. The first distance is greater than the second distance, preferably twice as large. In addition, the second path results in a lateral displacement (movement perpendicular to the direction of progression) which is referred to as the third distance, and the fourth path moves the robot laterally by a fourth distance that is equal in magnitude but opposite in direction from the third distance. In the preferred embodiment, the first through fourth paths are arcuate paths.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] The present invention is illustrated by way of example and not limitation in the figures of the accompanying drawings, and in which:
[0008] FIG. 1A is an autonomous mobile robot, in accordance with a preferred embodiment;
[0009] FIG. 1B is the autonomous mobile robot moving in the forward direction, in accordance with a preferred embodiment;
[0010] FIG. 1C is the autonomous mobile robot moving in the backward direction, in accordance with a preferred embodiment;
[0011] FIG. 2 is a schematic diagram of a navigation system, in accordance with a preferred embodiment;
[0012] FIG. 3 is a cleaning trajectory for scrubbing a floor, in accordance with an exemplary embodiment;
[0013] FIGS. 4A-4D depict a sequence of steps that produce the trajectory of FIG. 3 ;
[0014] FIG. 5 is a cleaning trajectory for scrubbing a floor, in accordance with another exemplary embodiment;
[0015] FIGS. 6A-6D depict a sequence of steps that produce the trajectory of FIG. 5 ;
[0016] FIG. 7 is a cleaning trajectory for scrubbing a floor, in accordance with still another exemplary embodiment; and
[0017] FIGS. 8A-8B depict a sequence of steps that produce the trajectory of FIG. 7 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0018] Illustrated in FIG. 1A is an autonomous mobile robot 100 configured to clean or otherwise treat a floor or other surface using a trajectory designed to repeatedly scrub the floor. In the preferred embodiment, the mobile robot 100 includes a housing with a controller and navigation system (not shown) for generating a path to clean the entire floor, a drive system 110 configured to move the robot around a room or other space in a determined trajectory, and a cleaning assembly 120 A pivotably attached to the robot housing by means of a hinge 130 . The cleaning assembly 120 A preferably includes a curved bottom surface 122 configured to press a cleaning sheet to the floor. The mobile robot in the preferred embodiment is based on the cleaning robot taught in pending U.S. patent application Ser. No. 12/429,963 filed on Apr. 24, 2009, which is hereby incorporated by reference herein.
[0019] The cleaning component in the preferred embodiment is configured to scrub the floor with a disposable cleaning sheet, preferably a wet cleaning sheet impregnated with cleaning solution. In other embodiments, the cleaning assembly is configured to dispense cleaning solution directly on the floor and then scrub the floor with a dry cleaning sheet. In still other embodiments, the cleaning assembly is configured to employ cleaning components for brushing, dusting, polishing, mopping, or vacuuming the floor, which may be a wood, tile, or carpet, for example.
[0020] Illustrated in FIG. 2 is a schematic diagram of the navigation system in the preferred embodiment. The navigation system 200 includes a navigation module 210 configured to maintain an estimate of the robot's current pose while it navigates around its environment, preferably an interior room bounded by walls. The pose 212 , which includes both the position and orientation, is based on multiple sensor readings including wheel odometry 214 provided by encoders integrated into the wheels 110 , orientation readings 216 from a gyroscope (not shown) on board the robot, and position coordinates from an optical sensor configured to sense light reflected from the room's ceiling. The optical sensor may include one or more photo diodes, one or more position sensitive detectors (PSDs), or one or more laser range finders, for example. The optical sensor employed in the preferred embodiment is taught in U.S. Pat. No. 7,720,554, which is hereby incorporated by reference herein.
[0021] The navigation system further includes a path planner 220 for generating or executing logic to traverse a desired trajectory or path 222 to scrub the entire floor with no gaps. In path 222 designed by the path planner 220 is a combination of a first trajectory from a room coverage planner 222 and a second trajectory from a local scrub planner 226 , which are discussed in more detail below. Based on the current pose 212 and the desired path 222 , the motion controller generates motion commands 232 for the robot drive 240 . The commands in the preferred embodiment include the angular velocity for each of a pair of wheels 110 , which are sufficient to control the speed and direction of the mobile robot. As the robot navigates through its environment, the navigation module 210 continually generates a current robot pose estimate while the path planner 220 updates the desired robot path.
[0022] The first trajectory is designed to guide the robot throughout the entire room until each section of the floor has been traversed. The second trajectory is a pattern including a plurality of incremental steps that drive the cleaning assembly both forward and backward, and optionally left and right. The first trajectory ensures every section of the floor is traversed with the cleaning assembly while the second trajectory ensures each section of floor traversed is effectively treated with cleaning solution and scrubbed with multiple passes of the cleaning assembly.
[0023] The first trajectory may take the form of any of a number of space-filling patterns intended to efficiently traverse each part of the room. For example, the first trajectory may be a rectilinear pattern in which the robot traverses the entire width of the room multiple times, each traversal of the room covering a unique swath or row adjacent to the prior row traversed. The pattern in repeated until the entire room is covered. In another embodiment, the robot follows a path around the contour of the room to complete a loop, then advances to an interior path just inside the path traversed in the preceding loop. Successively smaller looping patterns are traversed until the center of the room is reached. In still another embodiment, the robot traverses the room in one or more spiral patterns, each spiral including a series of substantially concentric circular or substantially square paths of different diameter. These and other cleaning contours are taught in U.S. patent application Ser. No. 12/429,963 filed on Apr. 24, 2009.
[0024] The second trajectory scrubs the floor using a combination of forward and backward motion. The step in the forward direction is generally larger than the step in the backward direction to produce a net forward movement. If the second trajectory includes lateral movement, the steps to the left and right are generally equal. The repeated forward/backward motion, in combination with hinge 130 , causes the orientation of the cleaning assembly to oscillate between a small angle forward or a small angle backward as shown in FIGS. 1B and 1C , respectively. When driven in the forward direction, the cleaning assembly 120 B pivots forward which presses the front half of the cleaning pad against the floor while lifting the back half away from the floor. When driven in the reverse direction, the cleaning assembly 120 C pivots backward to press the back half of the cleaning pad against the floor while lifting the front half away from the floor. As a result, the front half of the cleaning sheet (1) scrubs the floor with the cleaning sheet impregnated with cleaning solution and (2) captures/collects dirt and debris as the robot advances in the forward direction (see FIG. 1B ). On the other hand, the back half of the cleaning sheet, which remains generally free of debris, scrubs the floor with cleaning solution released from the cleaning sheet. This serves to: (i) evenly apply cleaning solution, (ii) recover the cleaning solution mixed with dissolved dirt, (iii) produce an elapse time between application and recovery of the cleaning solution, (iv) mechanically agitate the cleaning solution on the floor, and (v) produce little or no visible streak marks on the floor. In the exemplary embodiment, the cleaning sheet is impregnated with a cleaning solution that is transferred to the floor by contact. In another embodiment the mobile robot includes a reservoir with at least one nozzle configured to either spray cleaning solution on the floor surface in front of the cleaning assembly or diffuse the cleaning solution directly into the upper surface of the sheet through capillary action.
[0025] Illustrated in FIG. 3 is an example of a second trajectory for scrubbing a floor. The trajectory is produced by repetition of the sequence of steps shown in FIGS. 4A-4D . The solid line 310 represents the path traced by the midpoint of the leading edge of the cleaning assembly 120 while the shaded region 320 represents the region of floor scrubbed by the cleaning assembly. When this sequence is employed, the robotic cleaner oscillates in the forward direction of motion as well as laterally. For each oscillation, the forward displacement (defined as the “fwd_height”) exceeds the backward displacement (defined as the “back_height”) so the robot advances in a generally forward direction (defined as the “direction of progression”). The robot also moves left and right equal amounts (defined as the fwd_width) which causes the robot to travel in a generally straight line.
[0026] The trajectory shown in trajectory in FIG. 3 is produced by repetition of the sequence of steps illustrated in FIG. 4A-4D in the prescribed order. Each step or leg comprises a motion with an arcuate path. The first leg 410 of the sequence shown in FIG. 4A advances the robot forward by fwd_height and to the left. In the second leg 420 shown in FIG. 4B , the robot moves backward by back_height and to the right. In the third leg 430 shown in FIG. 4C , the robot moves forward by fwd_height and to the right. In the fourth leg 440 shown in FIG. 4D , the robot moves backward by back_height and to the left. The forward arcing motions have a larger radius than the back motions such that the robot is oriented parallel to the direction of progression upon completion of the backward motion.
[0027] Trajectories that include arced or arcuate paths can provide several benefits over trajectories having only straight paths. For example, the trajectory shown in FIG. 3 , which consists of arcuate paths, causes the robot to continually turn or rotate while in motion. This rotation, in turn is detected by the on-board gyroscope and monitored by the navigation system for purposes of detecting slippage of the wheels 110 . When the detected rotation is different than the rotation associated with the curvature of the path, the robot can confirm slippage due to loss of traction, for example, and correct the robots course accordingly. In contrast, trajectories with straight paths make it difficult to detect slippage when, for example, both wheels slip at the same rate which cannot be detect with the gyro.
[0028] For the trajectory shown in FIGS. 3 and 4 A- 4 D, the parameters are as follows:
(a) fwd_height: the distance traveled in the direction of progression on the forward legs or strokes has a value of approximately 1.5 times with width of the cleaning assembly 120 , the width being measured in the direction perpendicular to the direction of progression; (b) back_height: the distance traveled in the direction opposite the direction of progression on the backward legs or strokes has a value of approximately 0.75 times the width of the cleaning assembly 120 ; and (c) fwd_width: the distance traveled orthogonal to the direction of progression on the forward legs or strokes has a value of approximately 0.3 times the width of the cleaning assembly 120 .
[0032] In general, however, fwd_height may range between one and five times the width of the cleaning assembly 120 , the back_height may range between one third and four times the width of the cleaning assembly 120 , and the elapse time of a cleaning single sequence may range between five second and sixty seconds.
[0033] Where the cleaning sheet is a Swiffer(R) Wet Cleaning Pad, for example, each sequence of the trajectory is completed in a time between 15 to 30 seconds, which enables the cleaning solution to remain on the floor long enough to dissolve dirt but not so long that it first evaporates.
[0034] Illustrated in FIG. 5 is another example of a second trajectory for scrubbing a floor. The trajectory is produced by repetition of the sequence of steps shown in FIGS. 6A-6D . The solid line 510 represents the path traced by the midpoint of the leading edge of the cleaning assembly 120 while the shaded region 520 represents the region of floor scrubbed by the cleaning assembly. When this sequence is employed, the robotic cleaner oscillates in the forward direction of motion as well as laterally. For each oscillation, the forward displacement (“fwd_height”) exceeds the backward displacement (“back_height”) so the robot advances in a generally forward direction (“direction of progression”). The robot also moves left and right equal amounts (fwd_width) which causes the robot to travel in a generally straight line.
[0035] The trajectory shown ion trajectory in FIG. 5 is produced by repetition of the sequence of steps illustrated in FIG. 6A-6D . Each step or leg comprises a motion with an arcuate path. The first leg 610 of the sequence shown in FIG. 6A advances the robot forward by fwd_height and to the left with a predetermined radius. In the second leg 620 shown in FIG. 4B , the robot moves backward by back_height and to the right along the same radius as leg 610 . In the third leg 630 shown in FIG. 6C , the robot moves forward by fwd_height and to the right with the same predetermined radius. In the fourth leg 640 shown in FIG. 6D , the robot moves backward by back_height and to the left with the same radius as above. The forward arcing motions progress a greater distance than the back motions so that the robot generally progresses in the forward direction.
[0036] For the trajectory shown in FIGS. 5 and 6 A- 6 D, the parameters are as follows:
(a) fwd_height: the distance traveled in the direction of progression on the forward legs or strokes has a value of approximately 1.5 times with width of the cleaning assembly 120 , namely the direction perpendicular to the direction of progression; (b) back_height: the distance traveled in the direction opposite the direction of progression on the backward legs or strokes has a value of approximately 0.75 times the width of the cleaning assembly 120 ; and (c) radius: the radius of each arc is approximately equal to the diameter of the mobile robot, although the radius may range between 0.5 and 3 times the width of the cleaning assembly.
[0040] Illustrated in FIG. 7 is another example of a second trajectory for scrubbing a floor. The trajectory is produced by repetition of two legs that are both straight and parallel, as shown in FIGS. 7A-7B . The solid line 710 represents the path traced by the midpoint of the leading edge of the cleaning assembly 120 while the shaded region 720 represents the region of floor scrubbed by the cleaning assembly. When this sequence is employed, the robotic cleaner oscillates in the forward direction but not laterally. For each oscillation, the forward displacement (“fwd_height”) of the forward leg 810 exceeds the backward displacement (“back_height”) of the back leg 820 , so the robot advances in a generally forward direction.
[0041] In some embodiments, the robot further includes a bump sensor for detecting walls and other obstacles. When a wall is detected, the robot is configured to make a U-turn by completing a 180 degree rotation while moving the robot to one side, the distance moved being approximately equal to the width of the cleaning assembly. After completing the turn, the robot is then driven across the room along a row parallel with and adjacent to the preceding row traversed. By repeating this maneuver each time a wall is encountered, the robot is made to traverse a trajectory that takes the robot across each portion of the room.
[0042] The trajectory is preferably based, in part, on the pose of the robot which is tracked over time to ensure that the robot traverses a different section of the floor with each pass, thereby avoiding areas of the floor that have already been cleaned while there are areas still left to be cleaned.
[0043] One or more of the components of the mobile robot, including the navigation system, may be implemented in hardware, software, firmware, or any combination thereof. Software may be stored in memory as machine-readable instructions or code, or used to configure one or more processors, chips, or computers for purposes of executing the steps of the present invention. Memory includes hard drives, solid state memory, optical storage means including compact discs, and all other forms of volatile and non-volatile memory.
[0044] Although the description above contains many specifications, these should not be construed as limiting the scope of the invention but as merely providing illustrations of some of the presently preferred embodiments of this invention.
[0045] Therefore, the invention has been disclosed by way of example and not limitation, and reference should be made to the following claims to determine the scope of the present invention.
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A mobile robot configured to travel across a residential floor or other surface while cleaning the surface with a cleaning pad and cleaning solvent is disclosed. The robot includes a controller for managing the movement of the robot as well as the treatment of the surface with a cleaning solvent. The movement of the robot can be characterized by a class of trajectories that achieve effective cleaning. The trajectories include sequences of steps that are repeated, the sequences including forward and backward motion and optional left and right motion along arcuate paths.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application No. 60/409,310; filed Sep. 6, 2002, which is herein incorporated by reference for all purposes.
FIELD OF THE INVENTION
The invention relates to the discovery of a selective cell surface marker that permits the selection of a unique subset of pancreatic stems cells having a high propensity to differentiate into insulin producing cells or into insulin producing cell aggregates.
BACKGROUND OF THE INVENTION
In attempting to cultivate adult pancreatic islet cells, the objective has long been to isolate pancreatic progenitor cells that are capable of proliferation and differentiation into pancreatic β cells. One important step in isolation of pancreatic progenitor cells would be to identify recognizable cell markers, specific for the progenitor cells. Both intracellular and extracellular markers have been investigated for this purpose.
Once identified, extracellular markers would offer the advantage that the cells expressing the marker can be sorted under sterile conditions and kept alive to continue their study. Epithelial cell adhesion molecules such as Ep-CAM and integrins have been investigated as pancreatic islet progenitor markers. See e.g., Cirulli et al., J. Cell Biol. 140:1519-1534 (1998); and Cirulli et al., J. Cell Biol. 150:1445-1460 (2000). Cells selected by these makers have been shown to express transcription factors, such as PDX-1, indicating that they belong to the cell lineage in pancreatic development. However those cells have not been shown to be able to produce endocrine hormones such as insulin. Id.
Intracellular markers, particularly those from embryonic cells that develop into mature islet cells, have been extensively studied as progenitor markers. Transcription factors such as PDX-1, Ngn3, and Hlxb9, for example, have been studied. They are expressed in cells that are programmed during embryonic development to become pancreatic endocrine cells. However, these intracellular markers offer less practical value than extracellular makers in selecting progenitor cells, because analysis of expression of those markers requires either the killing the cells or permanent modification of the cells by genetic engineering of reporter genes into the cells.
Thus, there is a great need to identify extracellular marker(s) that allow the identification and selection of human adult pancreatic endocrine progenitor cells. The present invention solves this and other problems.
BRIEF SUMMARY OF THE INVENTION
This invention provides cell cultures of propagating pancreatic cells comprising progenitors of insulin producing pancreatic β cells. At least 50% of the cells exhibit the CD56 molecule as a cell surface marker and have an insulin:actin mRNA ratio less than 1:1. In one embodiment, at least 70% of the cells exhibit the CD56 molecule as a cell surface marker and have an insulin:actin mRNA ratio less than 1:1. In a further embodiment, at least 70% of the cells exhibit the CD56 molecule as a cell surface marker and have an insulin:actin mRNA ratio less than 1:100. In another embodiment, at least 90% of the cells exhibit CD56 as a cell surface marker and have an insulin:actin mRNA ratio less than 1:100. The invention also encompasses a cell culture of insulin producing cell aggregates produced from the propagating pancreatic progenitor cell culture.
This invention also includes a method of obtaining the culture of propagating pancreatic cells by isolating from a pancreas, and contacting the cells with a CD56 binding reagent to allow selection of CD56 positive pancreatic cells and separation of CD56 positive cells from CD56 negative cells. In some embodiments, the CD56 binding reagent is labeled. In some embodiments, the step of selecting is done by fluorescence activated cell sorting. In some embodiments, the step of selecting is done by panning. In one embodiment, CD56 binding reagent is an antibody that specifically binds to the CD56 protein. In one embodiment, the CD56 binding reagent is an antibody that specifically binds to an oligosaccharide linked to the CD56 protein. In another embodiment, the CD56 binding reagent is a lectin that specifically binds to an oligosaccharide linked to the CD56 protein. In another embodiment, the CD56 binding reagent is a ligand of the CD56 protein. In a further embodiment, the ligand is selected from the group consisting of soluble CD56, heparin, and heparin sulfate. In one embodiment, the pancreas is from a human.
In a further aspect of the invention, the CD56 positive pancreatic cells are propagated and differentiated into an aggregate of insulin producing cells. In some embodiments, the step of differentiating the cells comprises culturing the cells on plates coated with collagen IV. In one embodiment, the step of differentiating the cells comprises culturing the cells in a media comprising a differentiation factor. Many differentiation factors can be used including hepatocyte growth factor, keratinocyte growth factor, exendin-4, basic fibroblast growth factor, insulin-like growth factor-I, nerve growth factor, epidermal growth factor and platelet-derived growth factor.
The invention also includes a method of producing an aggregate of insulin producing pancreatic cells by isolating from a pancreas, contacting the cells with a CD56 binding reagent to allow selection of CD56 positive propagating pancreatic cells and separation of CD56 positive cells from CD56 negative cells, and differentiating the CD56 positive propagating pancreatic cell culture into an aggregate of insulin producing pancreatic cells. In some embodiments, the CD56 binding reagent is labeled. In some embodiments, the step of selecting is done by fluorescence activated cell sorting. In some embodiments, the step of selecting is done by panning. In one embodiment, CD56 binding reagent is an antibody that specifically binds to the CD56 protein. In one embodiment, the CD56 binding reagent is an antibody that specifically binds to an oligosaccharide linked to the CD56 protein. In another embodiment, the CD56 binding reagent is a lectin that specifically binds to an oligosaccharide linked to the CD56 protein. In another embodiment, the CD56 binding reagent is a ligand of the CD56 protein. In a further embodiment, the ligand is selected from the group consisting of soluble CD56, heparin, and heparin sulfate. In one embodiment, the pancreas is from a human. In some embodiments, the step of differentiating the cells comprises culturing the cells on plates coated with collagen IV. In one embodiment, the step of differentiating the cells comprises culturing the cells in a media comprising a differentiation factor. In another embodiment, the differentiation factor is selected from the group consisting of hepatocyte growth factor, keratinocyte growth factor, exendin-4, basic fibroblast growth factor, insulin-like growth factor-I, nerve growth factor, epidermal growth factor and platelet-derived growth factor.
The invention also encompasses a method of providing pancreatic endocrine function to a mammal in need of such function, by isolating a CD56 positive propagating cell culture, and implanting into a mammal the CD56 positive propagating cell culture in an amount sufficient to produce a measurable amount of insulin in the mammal. In a further embodiment the CD56 positive propagating cell culture differentiates further into insulin producing cells in vivo, e.g., within the mammal. In another embodiment, the CD56 positive propagating cell culture is differentiated into insulin producing aggregates in vitro, and then the aggregates of insulin producing pancreatic cells are implanted into the mammal in an amount sufficient to produce a measurable amount of insulin in the mammal. In one embodiment, the mammal is a human. In another embodiment, a human pancreas is used as a source of the CD56 positive propagating cell culture.
The invention also encompasses a method of monitoring a culture of propagating pancreatic cells by contacting the pancreatic cells with a CD56 binding reagent; and determining the quantity of cells that exhibit CD56 as a cell surface marker. In one embodiment, the detecting step is done by fluorescence activated cell sorting. In another embodiment, the CD56 binding reagent is an antibody that binds specifically to the CD56 protein. Monitoring the propagating pancreatic cell culture is useful to determine the potential of the culture to form aggregates of insulin producing cells.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 demonstrates the relative gene expression levels of unsorted cells, CD56 positive cells and CD56 negative cells. Gene expression was expressed as a ratio of mRNA copy number of the gene of interest (such insulin mRNA copy number) over that of β-actin (mRNA copy number of β-actin). For comparison, the levels of gene expression expressed by unsorted cells were normalized to 1, while the levels of gene expressions expressed by CD56 positively sorted and negatively sorted cells were plotted as folds of increase or decrease relative to that of unsorted cells.
FIG. 2 demonstrates the insulin/β-actin ratios of CD56 positive HD440B cells during proliferation. The CD56 positive cells were selected with magnetic beads.
FIG. 3 provides the composition of maturation media (MM).
FIG. 4 provides the results of Static Glucose Stimulation (SGS) assays in passage 8 cells derived CD56 negative cells (left panel) and in passage 8 cells derived from CD56 positive cells (right panel).
FIG. 5 demonstrates in vitro insulin expression of cells derived from CD56 positive cells that were selected and passaged and then matured at P11/13 in MM media.
FIG. 6 demonstrates the blood glucose levels of a diabetic SCID mouse that was transplanted with encapsulated, aggregated cells derived from CD56 positive cells.
DEFINITIONS
As used herein, a “cell culture of propagating pancreatic cells” is a culture of cells derived from pancreatic tissue that is able to undergo cell division and to be passaged from one culture vessel to another over time. A culture of propagating pancreatic cells that exhibits CD56 as a cell surface marker refers to a culture of pancreatic progenitor cells that, in addition to detectable CD56 cell surface expression, exhibits low levels of insulin mRNA and is capable of differentiation into mature pancreatic cells, including insulin-producing pancreatic β cells. In some embodiments the CD56 positive pancreatic cells have insulin:actin mRNA ratios less than 1:1. Other insulin:actin mRNA ratios are also encompassed by the present invention, e.g., 1:50, 1:20, 1:10, 1:5, and 1:2. In some embodiments, the CD56 positive pancreatic cells have insulin:actin mRNA ratios less than 1:100. In some embodiments the insulin mRNA levels in CD 56 positive propagating progenitor cells will only be detectable using very sensitive methods, e.g., in situ hybridization.
As used herein, “CD56 protein” refers to a cell surface glycoprotein thought to play a role in embryogenesis, development, and contact mediated interactions between cells. Because of differential transcript splicing, the majority of CD56 protein are found in three major sizes: 180 kDa, 140 kDa, and 120 kDa. Exemplary CD56 proteins include human CD56 proteins, for example the 120 kDal form, Accession Number P13592; the 140 kDal form, Accession Number P13591, and the 180 kDal form, see e.g., Hemperly, J. et al., J. Mole Neurosci. 2:71-78 (1990).
The term “CD56 binding reagent” is used herein to refer to a compound that specifically binds to a CD56 protein or to molecules covalently linked to a CD56 protein, such as oligosaccharides. In a preferred embodiment, the CD56 binding reagent is an antibody that specifically binds to the CD56 protein. The term “CD56 binding reagent” also encompasses compounds that are specifically bound by the CD56 protein, for example heparin and heparin sulfate. The term encompasses ligands and lectins as defined herein. CD56 binding reagents are used to identify or select cells that express CD56 protein as a cell surface marker.
Cells that “exhibit CD56 as a cell surface marker” are cells that exhibit a sufficient quantity of CD56 on the cell surface to allow the cells to be selected or picked out from a population of cells using conventional CD56 specific binding reagents and methods described herein, such as FACS, immunocytochemistry, immunoadsorbtion, and panning. In a preferred embodiment a CD56 antibody is used to select cells that “exhibit CD56 as a cell surface marker.”
“Insulin:actin mRNA ratios are measured by band density using gel scanner or by real time PCR using different labels for insulin and actin. With these methods, insulin:actin mRNA ratios are an average across a population of cells. Insulin:actin mRNA rations can also be measured on an individual cell basis using in situ hybridization.
“Antibody” refers to a polypeptide comprising a framework region from an immunoglobulin gene or fragments thereof that specifically binds and recognizes an antigen. The recognized immunoglobulin genes include the kappa, lambda, alpha, gamma, delta, epsilon, and mu constant region genes, as well as the myriad immunoglobulin variable region genes. Light chains are classified as either kappa or lambda. Heavy chains are classified as gamma, mu, alpha, delta, or epsilon, which in turn define the immunoglobulin classes, IgG, IgM, IgA, IgD and IgE, respectively. Typically, the antigen-binding region of an antibody will be most critical in specificity and affinity of binding.
An exemplary immunoglobulin (antibody) structural unit comprises a tetramer. Each tetramer is composed of two identical pairs of polypeptide chains, each pair having one “light” (about 25 kD) and one “heavy” chain (about 50-70 kD). The N-terminus of each chain defines a variable region of about 100 to 110 or more amino acids primarily responsible for antigen recognition. The terms variable light chain (V L ) and variable heavy chain (V H ) refer to these light and heavy chains respectively.
Antibodies exist, e.g., as intact immunoglobulins or as a number of well-characterized fragments produced by digestion with various peptidases. Thus, for example, pepsin digests an antibody below the disulfide linkages in the hinge region to produce F(ab)′ 2 , a dimer of Fab which itself is a light chain joined to V H -C H 1 by a disulfide bond. The F(ab)′ 2 may be reduced under mild conditions to break the disulfide linkage in the hinge region, thereby converting the F(ab)′ 2 dimer into an Fab′ monomer. The Fab′ monomer is essentially Fab with part of the hinge region (see Fundamental Immunology (Paul ed., 3d ed. 1993). While various antibody fragments are defined in terms of the digestion of an intact antibody, one of skill will appreciate that such fragments may be synthesized de novo either chemically or by using recombinant DNA methodology. Thus, the term antibody, as used herein, also includes antibody fragments either produced by the modification of whole antibodies, or those synthesized de novo using recombinant DNA methodologies (e.g., single chain Fv) or those identified using phage display libraries (see, e.g., McCafferty et al., Nature 348:552-554 (1990))
For preparation of antibodies, e.g., recombinant, monoclonal, or polyclonal antibodies, many technique known in the art can be used (see, e.g., Kohler & Milstein, Nature 256:495-497 (1975); Kozbor et al., Immunology Today 4: 72 (1983); Cole et al., pp. 77-96 in Monoclonal Antibodies and Cancer Therapy , Alan R. Liss, Inc. (1985); Coligan, Current Protocols in Immunology (1991); Harlow & Lane, Antibodies, A Laboratory Manual (1988); and Goding, Monoclonal Antibodies: Principles and Practice (2d ed. 1986)). The genes encoding the heavy and light chains of an antibody of interest can be cloned from a cell, e.g., the genes encoding a monoclonal antibody can be cloned from a hybridoma and used to produce a recombinant monoclonal antibody. Gene libraries encoding heavy and light chains of monoclonal antibodies can also be made from hybridoma or plasma cells. Random combinations of the heavy and light chain gene products generate a large pool of antibodies with different antigenic specificity (see, e.g., Kuby, Immunology (3 rd ed. 1997)). Techniques for the production of single chain antibodies or recombinant antibodies (U.S. Pat. Nos. 4,946,778, 4,816,567) can be adapted to produce antibodies to polypeptides of this invention. Also, transgenic mice, or other organisms such as other mammals, may be used to express humanized or human antibodies (see, e.g., U.S. Pat. Nos. 5,545,807; 5,545,806; 5,569,825; 5,625,126; 5,633,425; 5,661,016, Marks et al., Bio/Technology 10:779-783 (1992); Lonberg et al., Nature 368:856-859 (1994); Morrison, Nature 368:812-13 (1994); Fishwild et al., Nature Biotechnology 14:845-51 (1996); Neuberger, Nature Biotechnology 14:826 (1996); and Lonberg & Huszar, Intern. Rev. Immunol . 13:65-93 (1995)). Alternatively, phage display technology can be used to identify antibodies and heteromeric Fab fragments that specifically bind to selected antigens (see, e.g., McCafferty et al., Nature 348:552-554 (1990); Marks et al., Biotechnology 10:779-783 (1992)). Antibodies can also be made bispecific, i.e., able to recognize two different antigens (see, e.g., WO 93/08829, Traunecker et al., EMBO J . 10:3655-3659 (1991); and Suresh et al., Methods in Enzymology 121:210 (1986)). Antibodies can also be heteroconjugates, e.g., two covalently joined antibodies, or immunotoxins (see, e.g., U.S. Pat. No. 4,676,980, WO 91/00360; WO 92/200373; and EP 03089).
Methods for humanizing or primatizing non-human antibodies are well known in the art. Generally, a humanized antibody has one or more amino acid residues introduced into it from a source which is non-human. These non-human amino acid residues are often referred to as import residues, which are typically taken from an import variable domain. Humanization can be essentially performed following the method of Winter and co-workers (see, e.g., Jones et al., Nature 321:522-525 (1986); Riechmann et al., Nature 332:323-327 (1988); Verhoeyen et al., Science 239:1534-1536 (1988) and Presta, Curr. Op. Struct. Biol . 2:593-596 (1992)), by substituting rodent CDRs or CDR sequences for the corresponding sequences of a human antibody. Accordingly, such humanized antibodies are chimeric antibodies (U.S. Pat. No. 4,816,567), wherein substantially less than an intact human variable domain has been substituted by the corresponding sequence from a non-human species. In practice, humanized antibodies are typically human antibodies in which some CDR residues and possibly some FR residues are substituted by residues from analogous sites in rodent antibodies.
A “chimeric antibody” is an antibody molecule in which (a) the constant region, or a portion thereof, is altered, replaced or exchanged so that the antigen binding site (variable region) is linked to a constant region of a different or altered class, effector function and/or species, or an entirely different molecule which confers new properties to the chimeric antibody, e.g., an enzyme, toxin, hormone, growth factor, drug, etc.; or (b) the variable region, or a portion thereof, is altered, replaced or exchanged with a variable region having a different or altered antigen specificity.
In one embodiment, the antibody is conjugated to an “effector” moiety. The effector moiety can be any number of molecules, including labeling moieties such as radioactive labels or fluorescent labels, or can be a therapeutic moiety. In one aspect the antibody modulates the activity of the protein.
The phrase “specifically (or selectively) binds” to an antibody or “specifically (or selectively) immunoreactive with,” when referring to a protein or peptide, refers to a binding reaction that is determinative of the presence of the protein, often in a heterogeneous population of proteins and other biologics. Thus, under designated immunoassay conditions, the specified antibodies bind to a particular protein at least two times the background and more typically more than 10 to 100 times background. Specific binding to an antibody under such conditions requires an antibody that is selected for its specificity for a particular protein. For example, polyclonal antibodies raised to CD56 proteins, polymorphic variants, alleles, orthologs, and conservatively modified variants, or splice variants, or portions thereof, can be selected to obtain only those polyclonal antibodies that are specifically immunoreactive with CD56 proteins and not with other proteins. This selection may be achieved by subtracting out antibodies that cross-react with other molecules. A variety of immunoassay formats may be used to select antibodies specifically immunoreactive with a particular protein. For example, solid-phase ELISA immunoassays are routinely used to select antibodies specifically immunoreactive with a protein (see, e.g., Harlow & Lane, Antibodies, A Laboratory Manual (1988) for a description of immunoassay formats and conditions that can be used to determine specific immunoreactivity). Specific binding can also be used to describe the interaction of other molecules that specifically bind to CD56 protein, e.g. CD56 ligands and lectins that recognize CD56.
An “antigen” is a molecule that is recognized and bound by an antibody, e.g., peptides, carbohydrates, organic molecules, or more complex molecules such as glycolipids and glycoproteins. The part of the antigen that is the target of antibody binding is an antigenic determinant and a small functional group that corresponds to a single antigenic determinant is called a hapten.
A “label” or a “detectable moiety” is a composition detectable by spectroscopic, photochemical, biochemical, immunochemical, chemical, or other physical means. For example, useful labels include 32 P, fluorescent dyes, electron-dense reagents, enzymes (e.g., as commonly used in an ELISA), biotin, digoxigenin, or haptens and proteins which can be made detectable, e.g., by incorporating a radiolabel into the peptide or used to detect antibodies specifically reactive with the peptide.
As used herein, “insulin producing cells” refers to cells that secrete detectable amounts of insulin. “Insulin producing cells” can be individual cells or collections of cells. One example of a collection of “insulin producing cells” is “insulin producing cell aggregates” e.g., an organized collection of cells with a surrounding mantle of CK-19 positive cells and an inner cell mass. “Aggregate” in the context of cells refers to a three dimensional structure. “CK-19” is a 40 kD acidic keratin, cytokeratin 19. “Mantle” refers to an envelope of cells surrounding in three dimensions the inner cell mass.
The term “contacting” is used herein interchangeably with the following: combined with, added to, mixed with, passed over, incubated with, flowed over, etc.
An “oligosaccharide linked to CD56” is a polysaccharide molecule that is covalently linked to the CD56 protein. In a preferred embodiment, the oligosaccharide is linked through an asparagine residue.
The term “lectin” refers to protein that recognize specific carbohydrate molecules. In a preferred embodiment the carbohydrate is all or part of an oligosaccharide linked to a CD56 protein molecule.
A “ligand” is a molecule that is specifically bound by a protein. As an example, heparin and heparin sulfate are bound by the CD56 molecule. The term also encompasses molecules that bind to a protein, for example, an antibody that specifically binds to a protein. In some instances the ligand binds to a molecule that is covalently linked to a protein, for example, a carbohydrate or an oligosaccharide.
The terms “heparan or heparin and heparin sulfate” are known to those of skill in the art. Heparin and heparin sulfate are examples of glycosaminoglycans.
The term “FACS” refers to fluorescence activated cell sorting, a technique used to separate cells according to their content of particular molecules of interest. The molecule of interest can be specific for a type of cell or for particular cell state. The molecule of interest can be fluorescently labeled directly by binding to a fluorescent dye, or by binding to a second molecule, which has been fluorescently labeled, e.g., an antibody or lectin that has been fluorescently labeled and that specifically binds to the molecule of interest. In a preferred embodiment, a fluorescently labeled CD56 specific antibody is used to separate CD56 positive cells from CD56 negative cells.
The term “panning” refers to a method of selecting cells that bind to a CD56 binding reagent. A flat surface, e.g., a culture dish, is coated with a CD56 binding reagent. Pancreatic cells are added to the surface and allowed to bind to the CD56 binding reagent. The culture dishes are then washed, removing the CD56 negative cells from the dish. In a preferred embodiment, a CD56 specific antibody is used to coat a culture dish and “pan” for CD56 positive cells in a population of pancreatic cells.
“Differentiate” or “differentiation” refers to a process where cells progress from an undifferentiated state to a differentiated state or from an immature state to a mature state. For example, undifferentiated pancreatic cells are able to proliferate and express characteristics markers, like PDX-1. Mature or differentiated pancreatic cells do not proliferate and secrete high levels of pancreatic endocrine hormones. E.g., mature β-cells secrete insulin at high levels. Changes in cell interaction and maturation occur as cells lose markers of undifferentiated cells or gain markers of differentiated cells. Loss or gain of a single marker can indicate that a cell has “matured or differentiated.”
The term “differentiation factors” refers to a compound added to pancreatic cells to enhance their differentiation to mature insulin producing β cells. Exemplary differentiation factors include hepatocyte growth factor, keratinocyte growth factor, exendin-4, basic fibroblast growth factor, insulin-like growth factor-I, nerve growth factor, epidermal growth factor and platelet-derived growth factor.
The term “providing pancreatic function to a mammal in need of such function” refers to a method of producing pancreatic hormones within the body of a mammal unable to produce such hormones on its own. In a preferred embodiment, insulin is produced in the body of a diabetic mammal. The pancreatic function is provided by implanting or transplanting aggregates of insulin producing pancreatic cells, produced by the methods of this disclosure into the mammal. The number of aggregates implanted is an amount sufficient to produce a measurable amount of insulin in the mammal. The insulin can be measured by Western blotting or by other detection methods known to those of skill in the art, including assays for insulin function, such as maintenance of blood glucose levels. Insulin can also be measured by detecting C-peptide in the blood. In another preferred embodiment, the provision of pancreatic function is sufficient to decrease or eliminate the dependence of the mammal on insulin produced outside the body.
“Encapsulation” refers to a process where cells are surrounded by a biocompatible acellular material, such as sodium alginate and polylysine. Preferably small molecules, like sugars and low molecular weight proteins, can be taken up from or secreted into an environment surrounding the encapsulated cells. At the same time access to the encapsulated cells by larger molecules and immune cells is limited.
“Implanting” is the grafting or placement of the cells into a recipient. It includes encapsulated cells and non-encapsulated. The cells can be placed subcutaneously, intramuscularly, intraportally or interperitoneally by methods known in the art.
A “population” of cells refers to a plurality of cells obtained by a particular isolation or culture procedure. While the selection processes of the present invention yield populations with relatively uniform properties, a population of cells may be heterogeneous when assayed for marker expression or other phenotype. Properties of a cell population are generally defined by a percentage of individual cells having the particular property (e.g., the percentage of cells staining positive for a particular marker) or the bulk average value of the property when measured over the entire population (e.g., the amount of mRNA in a lysate made from a cell population).
“Passage” of cells usually refers to a transition of a seeded culture container from a partially confluent state to a confluent state, at which point they are removed from the culture container and reseeded in a culture container at a lower density. However, cells may be passaged prior to reaching confluence. Passage typically results in expansion of the cell population as they grow to reach confluence. The expansion of the cell population depends on the initial seeding density but is typically a 1 to 10, 1 to 5, 1 to 3, or 1 to 2 fold expansion. Thus, passaging generally requires that the cells be capable of a plurality of cell divisions in culture.
DETAILED DESCRIPTION OF THE INVENTION
I. Introduction
For the first time, the CD56 protein, also known as Neural Cell Adhesion Molecule (N-CAM) has been shown to be an extracellular marker for progenitors of pancreatic β cells. CD56 was originally isolated from developing neural tissue, but is also found in nonneural tissues. CD56 is expressed on neurons, muscle cells, adrenal medulla cells, astrocytes, Schwann cells, NK cells and a subset of activated T cells including those that are β cell antigen-specific and known to cause Type 1 diabetes. See e.g., Shliakhovenko et al., Vrach Delo 2:453-459 (1991); Mechtersheimer et al., Ann. NY Acad. Sci. 650:311-316 (1992); Leon et al., Brain Res. Dev. Brain Res. 70:109-121 (1992); Pierre et al. Neuroscience 103:133-142 (2001); Hung et al. Glai 38:363-370 (2002); and Ami et al., Clin. Exp Immunol. 128:453-459 (2002). CD56 has a developmental role in pattern formation, by facilitating cell-cell interactions. Known binding partners of CD 56 include other CD56 proteins and heparin or heparin sulfate.
CD 56 is a cell surface molecule that is evolutionarily conserved. CD56 family members have been found in chickens, mice, rats, humans, and frogs. The majority of CD56 proteins are found in three isoforms resulting from differential splicing of mRNA: a 180 kDal form, a 140 kDal form, and a 120 kDal form. CD56 proteins are extensively post-translationally modified. Post translational modifications include addition of asparagine linked oligosaccharides, sulfation of oligosaccharides, phosphorylation of serine and threonine residues, and fatty acid acylation of the protein.
Experiments described herein revel for the first time that CD56 can be used as an extracellular marker of pancreatic progenitor cells. Experiments and examples provided herein also demonstrate that the CD56 positive pancreatic cells identified are capable of being propagated and can also be differentiated into aggregates of insulin producing pancreatic cells.
II. Isolation of CD56 Positive Pancreatic Cells
Those of skill in the art will recognize that a variety of sources and methods can be used to isolate CD56 positive pancreatic cells.
A. Isolation of Pancreas from a Donor
Pancreatic cells isolated for subsequent culturing are obtained from one or more donated pancreases. The methods described herein are not dependent on the age of the donated pancreas. Accordingly, pancreatic material isolated from donors ranging in age from embryos to adults can be used.
In another embodiment, pancreatic cells are isolated from a cultured source. For example, cells prepared according to the microencapsulation method of U.S. Pat. No. 5,762,959 to Soon-Shiong, et al., entitled “Microencapsulation of cells,” can be harvested as a source of donor cells.
1. Isolation of Pancreatic Cells from Pancreas
Once a pancreas is harvested from a donor, it is typically processed to yield individual cells or small groups of cells for culturing using a variety of methods. One such method calls for the harvested pancreatic tissue to be cleaned and prepared for enzymatic digestion. Enzymatic processing is used to digest the connective tissue so that the parenchyma of the harvested tissue is dissociated into smaller units of pancreatic cellular material. The harvested pancreatic tissue is treated with one or more enzymes to separate pancreatic cellular material, substructures, and individual pancreatic cells from the overall structure of the harvested organ. Collagenase, DNAse, Liberase preparations (see U.S. Pat. Nos. 5,830,741 and 5,753,485) and other enzymes are contemplated for use with the methods disclosed herein.
Isolated source material can be further processed to enrich for one or more desired cell populations. However, unfractionated pancreatic tissue, once dissociated for culture, can also be used directly in the culture methods of the invention without further separation, and will yield the intermediate cell population. In one embodiment the isolated pancreatic cellular material is purified by centrifugation through a density gradient (e.g., Nycodenz, Ficoll, or Percoll). For example the gradient method described in U.S. Pat. No. 5,739,033, can be used as a means for enriching the processed pancreatic material in islets. The mixture of cells harvested from the donor source will typically be heterogeneous and thus contain α-cells, β-cells, δ-cells, ductal cells, acinar cells, facultative progenitor cells, and other pancreatic cell types.
A typical purification procedure results in the separation of the isolated cellular material into a number of layers or interfaces. Typically, two interfaces are formed. The upper interface is islet-enriched and typically contains 10 to 100% islet cells in suspension. The second interface is typically a mixed population of cells containing islets, acinar, and ductal cells. The bottom layer is the pellet, which is formed at the bottom of the gradient. This layer typically contains primarily (>80%) acinar cells, some entrapped islets, and some ductal cells. Ductal tree components can be collected separately for further manipulation.
The cellular constituency of the fractions selected for further manipulation will vary depending on which fraction of the gradient is selected and the final results of each isolation. When islet cells are the desired cell type, a suitably enriched population of islet cells within an isolated fraction will contain at least 10% to 100% islet cells. Other pancreatic cell types and concentrations can also be harvested following enrichment. For example, the culture methods described herein can be used with cells isolated from the second interface, from the pellet, or from other fractions, depending on the purification gradient used.
In one embodiment, intermediate pancreatic cell cultures are generated from the islet-enriched (upper) fraction. Additionally, however, the more heterogeneous second interface and the bottom layer fractions that typically contain mixed cell populations of islets, acinar, and ductal cells or ductal tree components, acinar cells, and some entrapped islet cells, respectively, can also be used in culture. While both layers contain cells capable of giving rise to the CD56 positive population described herein, each layer may have particular advantages for use with the disclosed methods.
B. Selection of CD56 Positive Pancreatic Cells
Once a source of pancreatic cells have been chosen, CD56 positive cells can be selected and then separated from cells that do not express CD56. Those of skill in the art will recognize that a variety of methods can be used to select CD56 positive cells and separate those cells from CD56 negative cells.
1. Detection of CD56 Positive Cells using Molecules that Bind CD56
Those of skill in the art will recognize that there are many methods to detect CD56 protein. For example, antibodies that bind specifically to the CD56 protein can be used to detect CD56. Antibodies specific to the CD56 protein are known to those of skill in the art and are commercially available from, for example, Research Diagnostics, Inc.; Abcam; Ancell Immunology Research Products; eBioscience; the Hybridoma Bank of the University of Iowa; and Zymed Laboratories, Inc. Antibodies that recognize the extracellular portion of CD56 can be used in the present invention.
The CD 56 protein is extensively post-translationally modified. Antibodies can also be used to detect molecules added as part of those modifications, e.g., sugars and oligosaccharide molecules.
In addition to antibodies, other molecules that bind specifically to CD56 can be used to identify CD56 positive cells. For example, lectins are molecules that bind specifically to particular sugars or oligosaccharides. Lectins that bind specifically to CD56 can be used in the present invention. CD56 also binds specifically to particular ligands, including other CD56 proteins and heparin or heparin sulfate. These, too, can be used to practice the present invention.
Those of skill in the art will recognize that molecules that bind specifically to CD56 are particularly useful if they are labeled and thus able to be detected by some means. A “label” is a composition detectable by spectroscopic, photochemical, biochemical, immunochemical, chemical, or other physical means. For example, useful labels include 32 P, fluorescent dyes, electron-dense reagents, enzymes (e.g., as commonly used in an ELISA), biotin, digoxigenin, or haptens and proteins which can be made detectable, e.g., by incorporating a radiolabel into the peptide or used to detect antibodies specifically reactive with the peptide.
2. FACS to Select CD56 Positive Cells
Fluorescently labeled molecules that bind specifically to CD56, most commonly antibodies, are used to select CD56 positive cells in conjunction with a Fluorescence Activated Cell Sorter (FACS). Briefly, pancreatic cells are incubated with fluorescently-labeled antibody and after the antibody binding, the cells are analyzed by FACS. The cell sorter passes single cells suspended in liquid through a fluorimeter. The amount of fluorescence is measured and cells with fluorescence levels detectably higher than control, unlabeled, cells are selected as positive cells.
FACS can also be used to physically separate cell populations based on measurement of fluorescence. The flowing cells are deflected by electromagnetic fields whose strength and direction are varied according to the measured intensity of the fluorescence signal. Labeled CD56 positive cells can be deflected into a separate container and thus, separated from unlabeled CD56 negative cells.
After pancreatic cells are isolated from pancreas, the cells are first cultured for one to two passages and then labeled with a CD56 specific antibody. The cells are then scanned using FACS to separate CD56 positive from CD56 negative cells. Up to 80% of the cells are deemed negative for CD56.
While this example has discussed FACS analysis with labeled antibodies, other molecules that specifically bind to CD56, e.g., lectins and other CD56 binding partners, such as other CD56 molecules and heparin or heparin sulfate, can also be used to practice the invention.
Many different fluorescent molecules are available for conjugation to antibodies, for example fluorescien or rhodamine. Those of skill are aware that in some instances more than one extracellular marker can be detected by using different antibodies conjugated to fluorescent molecules. FACS analysis can be done under conditions to identify more than one extracellular marker of interest.
3. Affinity Adsorbing CD56 Positive Cells onto a Solid Support.
CD56 positive cells can also be separated from CD56 negative cells by using CD56 specific binding molecules attached to a solid support. Those of skill in the art will recognize that CD56 specific antibodies can be bound to a solid support through an antibody binding molecule, such as protein G or protein A or alternatively, can be conjugated to a solid support directly. Solid supports with attached CD56 antibodies are commercially available, e.g., StemSep™ and EasySep™, magnetic beads from both from Stem Cell Technologies.
CD56 positive cells can also be separated from CD56 negative cells through the technique of panning. Panning is done by coating a solid surface with a CD56 binding reagent and incubating pancreatic cells on the surface for a suitable time under suitable conditions. A flat surface, e.g., a culture dish, is coated with a CD56 binding reagent. Pancreatic cells are added to the surface and allowed to bind to the CD56 binding reagent. The culture dishes are then washed, removing the CD56 negative cells from the dish. In a preferred embodiment, a CD56 specific antibody is used to coat a culture dish and “pan” for CD56 positive cells in a population of pancreatic cells.
III. Cell Culture and Cultivation of CD56 Positive Cells and Their progeny
A. General Cell Culture Procedures
Once the pancreatic cells are obtained and isolated, they are cultured under conditions that select for propagation of the desired CD56 positive population, or in other embodiments, for the differentiation of more mature cell types. General cell culture methodology may be found in Freshney, Culture of Animal Cells: A Manual of Basic Technique 4 th ed ., John Wiley & Sons (2000). Typically, pancreatic cells are cultured under conditions appropriate to other mammalian cells, e.g., in humidified incubators at 37° C. in an atmosphere of 5% CO 2 . Cells may be cultured on a variety of substrates known in the art, e.g., borosilicate glass tubes, bottles, dishes, cloning rings with negative surface charge, plastic tissue culture tubes, dishes, flasks, multi-well plates, containers with increased growth surface area (GSA) or Esophageal Doppler Monitor (EDM) finish, flasks with multiple internal sheets to increase GSA, Fenwal bags, and other culture containers.
Once the pancreatic cellular material has been harvested and selected for culture, or once a population is confluent and is to be transferred to a new substrate, a population of cells is seeded to a suitable tissue culture container for cultivation. Seeding densities can have an effect on the viability of the pancreatic cells cultured using the disclosed methods, and optimal seeding densities for a particular culture condition may be determined empirically by seeding the cells at a range of different densities and monitoring the resulting cell survival and proliferation rate. A range of seeding densities has been shown to be effective in producing hormone secreting cells in culture. Typically, cell concentrations range from about 10 2 to 10 8 cells per 100 mm culture dish, e.g., 10 2 , 10 3 , 10 4 , 10 5 , 10 6 , 10 7 , 10 8 cells per 100 mm culture dish, although lower cell concentrations may be employed for cloning procedures. Cell concentration for other culture vessels may be adjusted by computing the relative substrate surface area and/or medium gas exchange surface area for a different culture vessel. For example, a typical 100 mm culture dish has a substrate surface area of 55 square centimeters (see Freshney, supra), and a cell concentration of 10,000 cells per dish corresponds to about 180 cells per square centimeter, while a cell concentration of 100,000 cells per dish corresponds to about 1,800 cells per square centimeter. Cell concentration in terms of culture vessel surface area may be related to cell concentration in terms of media volume by using the appropriate media volume per culture surface area (0.2-0.5 ml/cm 2 are typical ranges for static culture). To determine if a 10 fold expansion has occurred, the cells are removed by enzymatic digestion and counted under microscope in a known volume of fluid. Cells may also be grown on culture surfaces pre-coated with defined extracellular matrix components to encourage growth and differentiation (e.g., fibronectin, Collagen I, Engelbreth-Holm-Swarm matrix, and, preferably, collagen IV or laminin).
Standard cell culture propagation techniques are suitable for practice of the invention. When cells are growing attached to a culture surface, they are typically grown as a monolayer until 80%-90% confluence is reached, at which point the cells are released from the surface by proteolytic digestion and split 1:2 or 1:3 for culture in new vessels. Higher dilutions of the cells are also suitable, generally between the ranges of 1:4 to 1:10, although even lower cell concentrations are appropriate in cloning procedures. Concentrations of proteolytic enzymes and chelating agents are usually lowered when cells are passaged in serum-free media (e.g., 0.025% trypsin and 0.53 mM EDTA). Culture medium is typically changed twice weekly or when the pH of the medium indicates that fresh medium is needed.
The pancreatic cells of the present invention may be cultured in a variety of media. As described herein, media containing or lacking particular components, especially serum, are preferred for certain steps of the isolation and propagation procedures. For example, cells freshly isolated from the pancreas may be maintained in high serum medium to allow the cells to recover from the isolation procedure. Conversely, low serum medium favors the selection and propagation of an intermediate stage population. Accordingly, a number of media formulations are useful in the practice of the invention. The media formulations disclosed here are for exemplary purposes, and non-critical components of the media may be omitted, substituted, varied, or added to simply by assaying the effect of the variation on the replication or differentiation of the cell population, using the assays described herein. See, e.g., Stephan et al., Endocrinology 140:5841-54 (1999)).
Culture media usually comprise a basal medium, which includes inorganic salts, buffers, amino acids, vitamins, an energy source, and, in some cases, additional nutrients in the form of organic intermediates and precursors that are involved in protein, nucleic acid, carbohydrate, or lipid metabolism. Basal media include F12, Eagle's MEM, Dulbecco's modified MEM (DMEM), RPMI 1640, a 1:1 mixture of F12 and DMEM, and others. See Freshney, supra. To support the growth of cells, basal medium is usually supplemented with a source of growth factors, other proteins, hormones, and trace elements. These supplements encourage growth, maintenance, and/or differentiation of cells, compensate for impurities or toxins in other medium components, and provide micronutrients lacking in the basal medium. In many culture media, serum is the source of these supplements. Serum can be supplied from a variety of mammalian sources, such as human, bovine, ovine, equine, and the like, and from adult, juvenile, or fetal sources. See Freshney, supra. Fetal bovine serum is a commonly used supplement. Concentrations of serum are expressed in terms of volume of serum as a percentage of the total medium volume, and typically range from about 0.1 to 25%, e.g., about 0.1, 0.2, 0.5, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 15, 20, or 25%. In some applications, the basal medium is supplemented with defined or semi-defined mixtures of growth factors, hormones, and micronutrients, rather than with serum. Formulas for serum replacement supplements are disclosed herein; others are known in the art or available from commercial sources (see Freshney, supra). For some embodiments, the concentration of serum is lowered but not eliminated, and defined or semi-defined supplement mixtures are added to the basal medium. Preferred applications for media containing high or low concentrations of serum are described herein.
B. Maintenance and Propagation of Isolated Pancreatic Cells in Media Containing High Serum
Cells harvested from a donor pancreas have usually undergone a period of warm or cold ischemia between the death of the donor and the beginning of the isolation procedure. Moreover, during the isolation procedure, pancreatic cells are usually subjected to proteolytic digestion as well as mechanical and shear stresses. Without wishing to be bound by a particular theory, the various traumas experienced by these cells may up-regulate various cellular processes that result in the expansion of pancreatic stem cell populations, such as facultative progenitor cells. Intermediate cell populations may be generated with satisfactory efficiency by placing cells into low serum media directly after isolation or purification. Nonetheless, because the trauma experienced by cells during the isolation procedures may have adverse effects on cell survival and adaptation to culture, it is sometimes desirable to maintain the freshly isolated cells in a stabilizing medium containing high concentrations of serum (e.g., >4%) to improve the efficiency of the culturing process. This maintenance period may be brief (e.g., overnight). Optionally, cells may be maintained for an extended propagation period in high serum medium.
High serum media for stabilization will typically contain at least 4% serum, and, in some embodiments, will contain a higher concentration of serum such as 10% or 20%. Media used for stabilization or propagation may be derived from a basal medium such as RPMI 1640, available from many commercial sources and described by Moore et al., J Am Med Assoc 199:519-524 (1967)). Exemplary high serum media for maintenance or propagation include Medium 3 (RPMI 1640+10 mM HEPES, 2 mM glutamine, 5 μM ZnSO 4 , and 10% fetal bovine serum (FBS)) and Medium 7 (RPMI 1640+10 mM HEPES, 2 mM glutamine, 5 μM ZnSO 4 , and 20% FBS). High serum media may also be derived by mixing a particular volume of high serum medium such as Medium 3 or Medium 7 with a particular volume of serum-free medium such as SM95, SM96, or SM98 (described herein) to arrive at a desired serum concentration (e.g., 4%-9%).
For stabilization after harvest, cells are conveniently cultured in a culture vessel at relatively high densities in a high serum medium (e.g., 10 9 cells in 70 ml of Medium 7 (20% FBS)). However, lower cell densities and serum concentrations may be employed as well. Cells are typically maintained in the original vessel for a relatively short time (e.g., overnight) to allow for recovery from the harvesting procedure.
Following the maintenance period, cells may be transferred to low serum media for selection and propagation of the CD56 positive cell population as described herein. Optionally, the cells may be cultured in a high serum medium to allow for proliferation of the mixed cell population. In a typical embodiment, cells from the maintenance culture are reseeded into a new culture vessel containing Medium 3 (10% FBS), Medium 7 (20% FBS), or a mixture of Medium 3 and Medium 7 (15% FBS), or other AmCyte culture media. Cells are typically cultured in this medium for 7-10 days, during which time they may grow to confluence. Once the cells have reached confluence, they may be passaged into low serum media for selective expansion of the intermediate cell population described herein.
C. Expansion and Propagation of a CD56 Positive Pancreatic Cell Population by Culture in Media Containing Low serum
Once the pancreatic cells have been isolated, the cells are then transferred to a selective medium to promote the emergence of a propagating intermediate stage population. This selective medium favors propagation of cells which retain the ability to secrete pancreatic endocrine hormones, or which retain the potential to mature into more differentiated cells which secrete high levels of pancreatic endocrine hormones. In general, selective medium will favor propagation of epithelial or epithelial-like cells at the expense of fibroblasts and mesenchymal cells, although pure epithelial cultures have not been shown to be required for the advantageous use of pancreatic cells in the methods of the invention. Typically, epithelial-selective media will yield a population of nearly pure (e.g., <10% fibroblasts or mesenchymal cells) cells after a certain period of growth in culture, e.g., 2, 3, 4, or 5 passages depending on the expansion of the population in each passage.
One type of selective medium which has been employed to favor epithelial cell growth from embryonic tissues is serum-free medium (see, e.g., Stephan et al., supra; Peehl and Ham, In Vitro 16:526-40 (1980)). Epithelial-specific media, and, more preferably, low serum media containing a source of growth hormone, may be employed to select for a distinct population of propagating pancreatic cells from adult mammals that retain markers of pancreatic cell development (e.g., PDX-1), but can be further differentiated under appropriate conditions to express high levels of pancreatic endocrine hormones. Particular epithelial-selective media suitable for culture of pancreatic cells are disclosed herein, but other medium formulations known in the art to favor the preferential expansion of epithelial or epithelial-like cells may also be employed.
The transfer to epithelial-selective low serum medium may be accomplished after a period of maintenance in high serum medium (“weaning”), or by transferring the cells directly into selective low serum medium following the isolation and separation procedure (“shock”). Either methodology is suitable for generation of the desired intermediate cell population.
1. Growth Hormones and Preferred Examples
Epithelial selective culture media containing growth hormone (GH) is used promote the emergence of a valuable pancreatic cell population of intermediate differentiation. Without wishing to be bound by a particular theory, it is hypothesized that GH can replace the mitogenic substances ordinarily found in serum that support cell growth, but that serum contains other mitogenic factors that promote the overgrowth of less desirable cell populations (e.g., fibroblasts and mesenchymal cells). Hence, replacement of serum with a supplemental mixture containing GH selects for propagation of a cell population with an intermediate state of differentiation. While the functions of GH in serum-free medium may be substituted with other supplemental ingredients in alternative embodiments of the invention, the ready availability of GH in natural extracts or as recombinant protein makes GH-containing media suitable epithelial-selective media for the methods disclosed herein.
Growth hormones, also known as somatotropins, are polypeptide hormones synthesized in the anterior pituitary which promote normal body growth and lactation and influence various aspects of cellular metabolism. GH has both direct effects on cells and indirect effects mediated by IGF-I and similar molecules; in the intact pancreas, islet cell growth has been connected to the expression of GH and the homologous hormones prolactin and lactogen (see, e.g., Nielsen et al., J Mol Med 77(1):62-6 (1999). In humans, mature GH contains 191 amino acid residues and displays a molecular mass of 22 kDa. However, in addition to the commonly observed disulfide dimer, two peptides made of portions of human GH (residues 1-43 and 44-191) have been detected in serum and have distinct effects on adult islet tissue (see Lewis et al., Endocr J 47 Suppl:S1-8 (2000)). Various naturally occurring derivatives, variants, metabolic products, and engineered derivatives of human GH are known, including glycosylated GH, methionyl GH, 20 kDa GH, acetylated GH, proteolytically cleaved GH, desamido GH, sulfoxide GH, and truncated forms of GH.
GH is a member of a conserved family of hormones including, in humans, GH-V1 and GH-V2, choriomammotropin and prolactin and proteins from other vertebrates such as rodent placental lactogens I and II and other bovine and sheep lactogens, murine proliferin I, II, and III and proliferin-related protein, bovine prolactin-related proteins I, II, and III, rat prolactin-like proteins A and B, and somatolactins from various fishes. Members of this family are characterized by the consensus sequences C-x-[ST]-x(2)-[LIVMFY]-x-[LIVMSTA]-P-x(5)-[TALIV]-x(7)-[LIVMFY]-x(6)-[LIVMFY]-x(2)-[STA]-W(SEQ ID NO:7) or C-[LIVMFY]-x(2)-D-[LIVMFYSTA]-x(5)-[LIVMFY]-x(2)-[LIVMFYT]-x(2)-C (SEQ ID NO:8).
Growth hormone suitable for practice of the invention may be obtained from a variety of natural and artificial sources. In contrast to therapeutic uses of GH, which often require GH of the same species, GH from a range of primate, mammalian, or vertebrate species may be employed in formulation of low serum media for culture of pancreatic cells. A convenient source of growth hormone is bovine pituitary extract (BPE), which is a rich source of natural GH. BPE (75 μg/ml protein) may be included in the culture medium at about 0.1 to 100 μl/ml, preferably at 0.5 to 50 μl/ml, and most preferably at 5 μl/ml or 37.5 mg/l. Pituitary extracts available from other species (e.g., porcine, ovine, and the like) may also be employed at similar concentrations. Other factors present in pituitary extract may potentiate its effect, but satisfactory results may also be achieved with purified GH, and with recombinant GH. Recombinant bovine and human GH are widely available and are a suitable source of GH activity. Recombinant GH may be added to culture medium at between 0.01 and 100 mg/l, preferably between 0.1 and 10 mg/l, more preferably at about 0.2, 0.5, 0.75, 1, 1.25, 2, or 5 mg/l, and most preferably at about 1.25 mg/L, where 1 mg of recombinant protein is about equivalent to 3 IU of GH.
2. Other Supplements
Typical ingredients added to basal media for complete serum-free media include recombinant human insulin (0.1 to 100 μg/ml), transferrin (0.1 to 100 μg/ml), epidermal growth factor (0.1 to 100 ng/ml), ethanolamine (0.1 to 100 μg/ml), aprotinin (0.1 to 100 μg/ml), glucose (0.1 to 100 mg/ml), phosphoethanolamine (0.1 to 100 μM), triiodothyronone (0.1 to 100 μM), selenium (0.1 to 100 nM), hydrocortisone (0.01 to 100 μM), progesterone (0.1 to 10 nM), forskolin (0.1 to 100 μM), heregulin (0.1 to 100 nM), and bovine pituitary extract (0.1 to 500 μg/ml). Not all supplemental ingredients are required to support cell growth; the optimal concentration or necessity for a particular supplement may be determined empirically, by leaving out or reducing the concentration of a single ingredient and observing the effect on cell proliferation. See e.g., Stephan et al., supra.
In general, supplemental ingredients may be replaced by natural or synthetic products that have the same biological properties. For example, triiodothyronone, hydrocortisone, and progesterone may all be replaced by natural or synthetic hormones known to activate the same intracellular receptors (thyroid receptors, glucocorticoid receptors, and progesterone receptors). Insulin and EGF are typically human proteins produced by recombinant DNA methodology, but may be replaced by polypeptides purified from natural sources, by polypeptides from other species, or by other agonists of the insulin and EGF receptors. GH may, in some cases, be substituted with other antagonists of the GH receptor. Likewise, heregulin, a ligand of the ErbB3 receptor, may be replaced by heregulin isoforms and other ErbB3 agonists such as NRG2, NRG3, and NRG4, sensory and motor neuron-derived factor, neurestin, and Ebp-1, heregulin α, heregulin β, heregulin γ, neuregulin-1 and neuregulin-2 (NRG-1 alpha, NRG-1beta, NRG-2 alpha, and NRG-2beta.
Exemplary serum-free media include the basal medium SM96 and the complete medium SM95, which consists of SM96 supplemented as shown in the following tables. SM98 consists of 1:1 F12/DMEM supplemented with a modification of medium supplement 14F described by Stephan et al., supra. SM98 contains less heregulin (1 ng/ml v. 8 ng/ml) than 14F. Thus, SM 98 consists of 1:1 μl 2/DMEM supplemented with recombinant human insulin, 10 μg/ml; transferrin, 10 μg/ml; epidermal growth factor, 10 ng/ml; ethanolamine, 61 ng/ml; aprotinin, 25 μg/ml; glucose, 5 mg/ml; phosphoethanolamine, 141 ng/ml; triiodothyronone, 3.365 μg/ml; selenium, 4.325 ng/ml; hydrocortisone, 181 ng/ml; progesterone, 3.15 ng/ml; forskolin, 410 ng/ml; heregulin, 1 ng/ml; and bovine pituitary extract, 75 μg/ml. Exemplary sources of EGH and heregulin in SM95 and SM98 are recombinant human EGF (Sigma E9644) and the EGF domain (amino acids 176-246) of human heregulin-β1 (R&D systems 396-HB/CF).
Mg/L
RPMI 1640 Media
(Moore, et al., A. M. A., 199: 519 (1967))
INORGANIC SALTS
Ca(NO 3 ) 2 —4H 2 O
100
KCl
400.00
MgSO 4 (anhyd.)
48.84
NaCl
5850.00
Na 2 HPO 4 (anhyd.)
800.00
OTHER COMPONENTS
D-Glucose
2000.00
Glutathione (reduced)
1.0
HEPES
5958.00
Phenol Red
5.00
AMINO ACIDS
L-Arginine
200.00
L-Asparagine (free base)
50.00
L-Aspartic Acid
20.00
L-Cystine•2HCl
65.00
L-Glutamic Acid
20.00
L-Glutamine
300.00
Glycine
10.00
L-Histidine (free base)
15.00
L-Isoleucine
50.00
L-Leucine
50.00
AMINO ACIDS
L-Lysine•HCl
40.00
L-Methionine
15.00
L-Phenylalanine
15.00
L-Proline
20.00
L-Serine
30.00
L-Threonine
20.00
L-Tryptophan
5.00
L-Tyrosine•2Na 2 H 2 0
29.00
L-Valine
20.00
VITAMINS
Biotin
0.20
D-Ca Panthothenate
0.25
Choline Chloride
3.00
Folic Acid
1.00
i-Inositol
35.00
Niacinamide
1.00
Pyridoxine•HCl
1.00
Riboflavin
0.20
Thiamine•HCl
1.00
Thymidine
0.005
Vitamin B 12
1.04
SM95
INORGANIC SALTS
CaCl 2
78.3
CuS0 4 •5H 2 0
0.00165
Fe(NO 3 ) 3 •9H 2 O
0.025
FeSO 4 •7H 2 0
0.61
KCl
271
MgCl 2
28.36
MgSO 4
39.06
KH 2 PO 4
34
NaCl
7262.75
NaHCO 3
1600
Na 2 HPO 4
101.5
NaH 2 PO 4 •H 2 O
31.25
ZnS0 4 •7H 2 O
0.416
AMINO ACIDS
L-Alanine
11.225
L-Arginine•HCl
283.75
L-Asparagine•H 2 0
18.75
L-Aspartic Acid
16.325
L-Cysteine•H 2 0(non-animal)
43.78
L-Cystine•2HCl
15.65
L-Glutamic Acid
18.675
L-Glutamax I
328.5
Glycine
89.375
Glycyl-Histidyl-Lysine
0.000005
L-Histidine HC1•H 2 0
38.69
L-Isoleucine
31.24
L-Leucine
42.5
L-Lysine•HCl
82.125
L-Methionine
13.12
L-Phenylalanine
22.74
L-Proline
43.625
L-Serine
23.625
L-Threonine
38.726
L-Tryptophan
6.51
L-Tyrosine•2Na 2 H 2 0(non-animal)
35.9
L-Valine
38.125
OTHER COMPONENTS
D-Glucose
3000
HEPES
1787.25
Na Hypoxanthine
3.2
Linoleic Acid
0.066
Lipoic Acid
0.1525
Phenol Red
4.675
Na Putrescine•2HCl
0.191
Na Pyruvate
137.5
VITAMINS
Biotin
0.037
Ascorbic Acid
22.5
D-Ca Pantothenate
1.37
Choline Chloride
11.49
Folic Acid
1.826
L-Inositol
24.3
Niacinamide
1.03
Pyridoxine•HCl
1.046
Riboflavin
0.13
Thiamine•HCl
1.23
Thymidine
0.5325
Vitamin B 12
1.04
SUPPLEMENTS
Na Selenous Acid
0.0034
Epithelial Growth Factor
0.005
Ethanolamine
0.03
Phosphoethanolamine
0.07
Aprotinin
12.5
Progesterone
0.0016
Forskolin
0.205
HeregulinB
0.004
Bovine Pituitary Extract
37.5
Hydrocortisone
0.0923
r.h. insulin
5.05
T 3
0.0000015
L-Thyroxine Na
0.00002
Bovine Transferrin APG
7.5
SM96
INORGANIC SALTS
CaCl 2
78.3
CuS0 4 •5H 2 0
0.00165
Fe(NO 3 ) 3 •9H 2 O
0.025
FeSO 4 •7H 2 0
0.61
KCl
271
MgCl 2
28.36
MgSO 4
39.06
KH 2 PO 4
34
NaCl
7262.75
NaHCO 3
1600
Na 2 HPO 4
101.5
NaH 2 PO 4 •H 2 O
31.25
ZnS0 4 •7H 2 O
0.416
AMINO ACIDS
L-Alanine
11.225
L-Arginine•HCl
283.75
L-Asparagine•H 2 0
18.75
L-Aspartic Acid
16.325
L-Cysteine•H 2 0(non-animal)
43.78
L-Cystine•2HCl
15.65
L-Glutamic Acid
18.675
L-Glutamax I
328.5
Glycine
89.375
Glycyl-Histidyl-Lysine
0.000005
L-Histidine HCl•H 2 0
38.69
L-Isoleucine
31.24
L-Leucine
42.5
L-Lysine•HCl
82.125
L-Methionine
13.12
L-Phenylalanine
22.74
L-Proline
43.625
L-Serine
23.625
L-Threonine
38.726
L-Tryptophan
6.51
L-Tyrosine•2Na 2 H 2 0(non-animal)
35.9
L-Valine
38.1261
OTHER COMPONENTS
D-Glucose
3000
HEPES
1787.25
Na Hypoxanthine
3.2
Linoleic Acid
0.066
Lipoic Acid
0.1525
Phenol Red
4.675
Na Putrescine•2HCl
0.191
Na Pyruvate
137.5
VITAMINS
Biotin
0.037
Ascorbic Acid
22.5
D-Ca Pantothenate
1.37
Choline Chloride
11.49
Folic Acid
1.826
i-Inositol
24.3
Niacinamide
1.03
Pyridoxine•HCl
1.046
Riboflavin
0.13
Thiamine•HCl
1.23
Thymidine
0.6325
Vitamin B 12
1.04
3. Transfer of Cells to Low Serum Media
Transferring a culture of pancreatic cells to low serum media promotes the selection of a defined population of cells with an intermediate state of differentiation. This cell population will continue to proliferate if subcultured, but maintains high expression levels of pancreatic markers such as PDX-1. Unstimulated, this population secretes relatively low levels of pancreatic endocrine hormones such as insulin, but can be matured according to the methods of the invention to yield high-secreting cells. To transfer a culture of pancreatic cells to low serum medium, the cells may be weaned from high serum to low serum media, or may be placed directly in low serum media following isolation. Medium such as SM95 and SM98 are suitable low serum media, although SM95 yields slightly improved insulin secretion upon maturation the of pancreatic cells.
The CD56 positive cell population and its progeny typically retains both the ability to proliferate and the ability for further differentiation into high-secreting endocrine cells. As the CD56 positive cells proliferate, the strength of CD56 expression can become less pronounced, and in some cases is detectable only by RT-PCR.
The ability of CD56 cells to proliferate provides an advantage in their ability to expand and increase the number of cells available for later maturation into glucose-secreting, insulin-producing aggregates. Proliferative ability is generally assessed by the ability of a culture seeded at a one density to expand to a second density; e.g., cells plated at 180 cells per square centimeter may be expanded to 1,800 cells per ml in a single passage. By repeated cycles of propagation and passage, a starting population of isolated pancreatic cells may be expanded by about 10,000-fold or more (e.g., about 100-fold, 500-fold, 1000-fold, 5000-fold, 10,000-fold, 50,000-fold, 100,000-fold, 500,000-fold, or 1,000,000 fold) while retaining endocrine markers such as PDX-1 and insulin mRNA expression, and retaining the ability to differentiate into mature high-secreting endocrine cells.
IV. Differentiation-Induction of Insulin Producing Aggregates
Cell differentiation of CD56 positive cells can be induced through induction of cell aggregation. As the CD56 positive cells differentiate, the strength of CD56 expression can become less pronounced. Cell aggregation can be induced in a variety of ways. For example, aggregation and differentiation can be induced by growing the cells to confluence. Aggregation and differentiation can also be induced by growing cells on conditioned culture dishes.
A variety of substrates can be used to condition culture dishes. Conditioned culture dishes can be culture dishes that have been used previously to grow intermediate stage pancreatic stem cells. Once the cells have formed a monolayer (typically about 5 days, depending on the initial subculture seeding density), they are removed by trypsinization. Growth of a 100% confluent cell culture is not required to produce a conditioned culture dish. A lowered concentration of trypsin (typically ½ or ¼ of the concentration employed in standard cell culture techniques) is preferred to prevent extensive degradation of the matrix. Alternatively, the cell monolayer may be removed by extracting the substrate with detergent, which will remove the cells but leave behind the secreted matrix (see Gospodarowicz et al., Proc Natl Acad Sci USA 77:4094-8 (1980)).
Conveniently, the removed cells which previously grew on the substrate or culture dish may be split and reseeded on the same, now conditioned, culture dish. However, the culture which conditions the substrate and the culture which is seeded on the substrate need not be the same culture. Accordingly, one culture of cells may be grown on a substrate to condition the substrate, the cells removed, and cells from another culture seeded upon the conditioned substrate. The conditioning cells may be from the same or different donor or species as the cells subsequently cultured.
In another embodiment, plates conditioned with collagen coating are used in the invention. Collagen coated plates are commercially available. In a preferred embodiment, collagen IV coated plates are used to induce aggregation and differentiation of pancreatic cells.
Differentiation of CD56 positive cells into mature insulin producing cells can also be enhanced by growth of the cells in the presence of differentiation factors. Preferred differentiation factors include hepatocyte growth factor, keratinocyte growth factor, and exendin-4. Hepatocyte growth factor has been shown to effect differentiation of pancreatic cells in culture and in transgenic animals. See e.g., Mashima, H. et al., Endocrinology , 137:3969-3976 (1996); Garcia-Ocana, A. et al., J. Biol. Chem . 275:1226-1232 (2000); and Gahr, S. et al., J. Mol. Endocrinol . 28:99-110 (2002). Keratinocyte growth factor has been shown to effect differentiation of pancreatic cells in transgenic animals. See e.g., Krakowski, M. L., et al., Am. J. Path . 154:683-691 (1999) and Krakowski, M. L., et al., J. Endochrinol . 162:167-175 (1999). Exendin-4 has been shown to effect differentiation of pancreatic cells in culture. See e.g., Doyle M. E. and Egan J. M., Recent Prog. Horm. Res . 56:377-399 (2001) and Goke, R., et al., J. Biol. Chem . 268:19650-19655 (1993). bFGF has been shown to increase the insulin secretion in microencapsulated pancreatic islets. See e.g., Wang W., et al., Cell Transplant 10(4-5): 465-471 (2001). IGF-I has an effect on differentiation of pancreatic ductal cells and IGF-I replacement therapy has been used for type I diabetes treatment. See e.g., Smith FE., et al., Proc. Natl. Acad. Sci. USA . 15;88(14): 6152-6156 (1991), Thrailkill KM. et al., Diabetes Technol. Ther . 2(1): 69-80 (2000). Evidence has shown that NGF plays an important autoregulatory role in pancreatic beta-cell function. See e.g. Rosenbaum T. et al., Diabetes 50(8): 1755-1762 (2001), Vidaltamayo R. et al., FASEB 16(8): 891-892 (2002), and Pierucci D. et al., Diabetologia 44(10): 1281-1295 (2001). EGF has been shown to promote islet growth and stimulate insulin secretion. See e.g., Chatterjee A K. et al., Horm. Metab. Res . 18(12): 873-874 (1986). PDGF has been shown to have an effect on the survival of CD56-positive cells. See e.g., Ben-Hur T. et al., J. Neurosci . 18(15): 5777-5788 (1998).
V. Characterization of CD56 Positive Cells and Their Progeny
Those of skill in the art will recognize that it can be useful to determine the differentiation state of CD56 positive cells and their progeny. The differentiation state of pancreatic cells can be determined in a variety of ways, including measurement of protein and mRNA markers of differentiation and functional assays of pancreatic cells, e.g. ability to secrete insulin in response to glucose stimulation.
A. Phenotypic Assays
To know when mature pancreatic cells are present, it is useful to assay the phenotypes of pancreatic cells at particular stages of culture. Since expression of particular proteins correlates with cell identity or differentiation state, cells may be analyzed for the expression of a marker gene or protein to assess their identity or differentiation state. For example, in freshly isolated pancreatic tissue, expression of amylase identifies the cell as an exocrine acinar cell, while expression of insulin identifies the cell as an endocrine islet cell. Likewise, islet cells at an early stage of differentiation are usually positive for the cytokeratin CK-19, while mature islet cells show less expression of CK-19.
Phenotypic properties may be assayed on a cell-by-cell basis or as a population average. The mode of assay will depend on the particular requirements and methodology of the assay technique. Thus, assays of marker expression by immunohistochemistry, performed on fixed sections or on suspended cells by FACS analysis, measure the frequency and intensity with which individual cells express a given marker. On the other hand, it may be desirable to measure properties such as the average insulin to actin mRNA expression ratio over an entire population of cells. In such cases, the assay is typically performed by collecting mRNA from a pool of cells and measuring the total abundance of insulin and actin messages. Many phenotypic properties may be assayed either on a cell or population basis. For example, insulin expression may be assayed either by staining individual cells for the presence of insulin in secretory granules, or by lysing a pool of cells and assaying for total insulin protein. Similarly, mRNA abundance may be measured over a population of cells by lysing the cells and collecting the mRNA, or on an individual cell basis by in situ hybridization.
1. Cell Differentiation Markers
There are a number of cellular markers that can be used to identify populations of pancreatic cells. Donor cells isolated and cultured begin to display various phenotypic and genotypic indicia of differentiated pancreatic cells. Examples of the phenotypic and genotypic indicia include various molecular markers present in the facultative progenitor cell population that are modulated (e.g., either up or down regulated). These molecular markers include CK-19, which is hypothesized to be a marker of the pancreatic facultative stem cell.
Typically, mammalian stem cells proceed through a number of developmental stages as they mature to their ultimate developmental endpoint. Developmental stages often can be determined by identifying markers present or absent in developing cells. Because human endocrine cells develop in a similar manner, various markers can be used to identify cells as they transition from a stem cell-like phenotype to pseudoislet phenotype.
The expression of markers in cells induced to proliferate or differentiate by the methods of the present invention bears some similarity to the sequence of marker expression in normal human pancreas development. Very early in development, the primordial epithelial cells express PDX-1, an early cellular marker that is a homeodomain nuclear factor. As the cells develop, they begin to bud out and form a duct. These cells express cytokeratin 19, a marker for epithelial ductal cells, and temporally express PDX-1 leading developmentally to endocrine cells. As these cells continue to develop, they gain the ability to express insulin, somatostatin, or glucagon. The final differentiated cells are only able to express one and become the α cells (glucagon), β cells (insulin), and δ cells (somatostatin). The CD56 positive cell population used herein is believed to be at a less than fully differentiated stage of development, retaining the ability to proliferate and the potential to differentiate into mature endocrine cells. Whether the cells are indeed examples of a precursor in the development pathway or simply a result of in vitro manipulation, the CD56 positive cells are able to proliferate as well as to express endocrine hormones and, therefore, have the potential for being used to correct a deficiency in any type of islet cell.
Markers of interest are molecules that are expressed in temporal- and tissue-specific patterns in the pancreas (see Hollingsworth, Ann N Y Acad Sci 880:38-49 (1999)). These molecular markers are divided into three general categories: transcription factors, notch pathway markers, and intermediate filament markers. Examples of transcription factor markers include PDX-1, NeuroD, Nkx-6.1, Isl-1, Pax-6, Pax-4, Ngn-3, and HES-1. Examples of notch pathway markers include Notch1, Notch2, Notch3, Notch4, Jagged1, Jagged2, Dll1, and RBPjk. Examples of intermediate filament markers include CK19 and nestin. Examples of markers of precursors of pancreatic β cells include PDX-1, Pax-4, Ngn-3, and Hb9. Examples of markers of mature pancreatic, cells include insulin, somatostatin, glp-9, and glucagon.
Methods for assessing expression of protein and nucleic acid markers in cultured or isolated cells are standard in the art and include quantitative reverse transcription polymerase chain reaction (RT-PCR), Northern blots, and in situ hybridization (see, e.g., Current Protocols in Molecular Biology (Ausubel et al., eds. 2001 supplement)) and immunoassays, such as immunohistochemical analysis of sectioned material, Western blotting, and, for markers that are accessible in intact cells, flow cytometry analysis (FACS) (see, e.g., Harlow and Lane, Using Antibodies: A Laboratory Manual , New York: Cold Spring Harbor Laboratory Press (1998)). Conventional histochemical markers of endocrine cell differentiation may also be employed. Cells to be examined by immunohistochemistry may be cultured on glass chamber slides for microscopic examination. Alternatively, cells grown in conventional tissue culture may be manually removed from the culture and embedded in paraffin for sectioning. PDX-1 antibody can be made following the teachings of Leonard J. et al., Mol. Endocrinol., 1993, Oct 7, (10) 1275-83.
Cell differentiation markers are varied and can be detected by conventional immunohistochemistry. A generally applicable protocol follows.
The staining process begins with removing chamber portion of the slides. Cells were very gently rinsed with in buffers and fixed in paraformaldehyde solution. Cells are then incubated in a blocking solution containing normal serum at room temperature. Cells were permeabilized with non-ionic detergent in blocking solution. Primary antibodies as listed below are prepared in blocking solution at appropriate dilution and added to cells and incubated. Following incubating with primary antibody, cells were rinsed in buffer and reblocked in blocking solution.
Secondary antibody prepared in blocking solution at appropriate dilution is added to the cells and incubated in the dark. Following incubation the cells are rinsed and nuclei were counterstained with Hoechst dye. Excess fluid is removed and the slides are mounted and covered with coverslides. The slides dry and are stored in the dark.
Alternatively the cells can be prepared for immunocytochemistry using the ABC method. In brief, the cells are embedded in parafin and slides with paraffin sections are dried at 37° C. overnight. The cells are deparaffinized and immersed in a hydrogen peroxide methanol solution to inhibit endogenous peroxidase activity. Slides were boiled in 0.01 citrate buffer (pH 6.0) for 30 minutes to recover certain epitopes. Slides were rinsed with buffer and blocked using normal serum at room temperature in a moist chamber.
Primary antibody prepared in blocking solution are added to the samples and incubated in a moist chamber. Slides are washed and incubated with secondary antibody prepared in blocking solution. Slides were again rinsed with buffer and incubated with Avidin-Horse Reddish Peroxides reagent or ABC complex from a commercial kit (e.g. Dako Corporation). Slides are again rinsed and incubated with diaminobenzidin developing solution; urea hydrogen peroxides in a gold wrap. After washes with distilled water, slides are immersed in Mayer's Hematoxylin for 5 minutes, then kept slides in running tap water until water turned colorless and nuclei were blue. Slides are dehydrated and mounted for viewing.
2. Insulin mRNA Expression
One marker that may be used to characterize pancreatic cell identity, differentiation, or maturity is the level of insulin mRNA. For example, the intermediate cell population of the present invention show expression of insulin mRNA within a defined range. Method for quantitating insulin mRNA include Northern blots, nuclease protection, and primer extension. In one embodiment, RNA is extracted from a population of cultured cells, and the amount of proinsulin message is measured by quantitative reverse transcription PCR. Following reverse transcription, insulin cDNA is specifically and quantitatively amplified from the sample using primers hybridizing to the insulin cDNA sequence, and amplification conditions under which the amount of amplified product is related to the amount of mRNA present in the sample (see, e.g., Zhou et al., J Biol Chem 272:25648-51 (1997)). Kinetic quantification procedures are preferred due to the accuracy with which starting mRNA levels can be determined.
Frequently, the amount of insulin mRNA is normalized to a constitutively expressed mRNA such as actin, which is specifically amplified from the same RNA sample using actin-specific primers. Thus, the level of expression of insulin mRNA may be reported as the ratio of insulin mRNA amplification products to actin mRNA amplification products, or simply the insulin:actin mRNA ratio. The expression of mRNAs encoding other pancreatic hormones (e.g., somatostatin or glucagon) may be quantitated by the same method. Insulin and actin mRNA levels can also be determined by in situ hybridization and then used to determine insulin:actin mRNA ratios. In situ hybridization methods are known to those of skill in the art.
B. Functional Assays
a) Glucose Stimulated Insulin Secretion
One of the important functions of a beta cell is to adjust its insulin secretion according to the glucose level. Typically, a static glucose stimulation (SGS) assay can be performed on the proliferating adherent pancreatic cells to identify whether they are able to secrete insulin in response to different glucose levels. Cells are generally cultured on an appropriate substrate until nearly confluent. Three days prior to the SGS test, the culture medium is replaced by a medium of similar character but lacking insulin and containing only 1 g/L of glucose. The medium is changed each day for three days and the SGS test is performed on day four.
Before the test, the culture medium may be collected for glucose and insulin analysis. To prepare cells for the test, cells are washed twice with Dulbecco's phosphate-buffered saline (DPBS)+0.5% BSA, incubating for 5 minutes with each wash, and then once with DPBS alone, also incubating for 5 minutes. After washing, the cells are incubated with 10 ml (in a 100 mm dish) or 5 ml (in a 60 mm dish) of Krebs-Ringers SGS solution with 60 mg/dl glucose (KRB-60) for 30 minutes in a 37° C. incubator. This incubation is then repeated.
To perform the SGS assays, cells are incubated in 3 ml (100 mm dish) or 4 ml (T75 flask) or 2 ml (60 mm dish) KRB-60, at 37° C. for 20 minutes. The medium is aspirated and spun, and is collected for insulin assay as LG-1 (low glucose stimulated step). KRB-450+theo (KRB with 450 mg/dl glucose and 10 mM theophylline) is then added with the same volume as above, and cells are cultured under the same condition as above. The supernatant is collected for insulin assay as HG (high glucose stimulated). The cells are then incubated again with KRB-60 and the medium collected as LG-2, and another time as LG-3. The media are collected for insulin analysis, and stored at −20° C. until insulin content is determined by radioimmunoassay (RIA) or other suitable assay.
The results of the SGS test are often expressed as a stimulation index, defined as the HG insulin value divided by the LG-1 insulin value. Generally, a stimulation index of about 2 or greater is considered to be a positive result in the SGS assay, although other values (e.g., 1.5, 2.5, 3.0, 3.5, etc.) may be used to define particular cell populations.
VI. Implantation of CD56 Positive Cells or Their Progeny and Restoration of Pancreatic Endocrine Function
Those of skill in the art will recognize that propagating CD56 positive cells provide a renewable resource for implantation and restoration of pancreatic function in a mammal. Propagating CD56 positive pancreatic cells are first differentiated before implantation into the mammal. If desired by the user, CD56 cells can be encapsulated before implantation.
A. Encapsulation
Encapsulation of the CD56 positive cells results in the formation of cellular aggregates in the capsules. Encapsulation can allow the pancreatic cells to be transplanted into a diabetic host, while minimizing the immune response of the host animal. The porosity of the encapsulation membrane can be selected to allow secretion of biomaterials, like insulin, from the capsule, while limiting access of the host's immune system to the foreign cells.
Encapsulation methods are known in the art and are disclosed in the following references: van Schelfgaarde & de Vos, J. Mol. Med . 77:199-205 (1999), Uludag et al. Adv. Drug Del Rev . 42:29-64 (2000) and U.S. Pat. Nos. 5,762,959, 5,550,178, and 5,578,314. Below is a general description of encapsulation of intermediate stage pancreatic stem cells. Specific examples are found in Examples 5 and 9 of this application.
Encapsulation methods are described in detail in co-pending application PCT/US02/41616; herein incorporated by reference.
B. Implantation
Implantation or transplantation into a mammal and subsequent monitoring of endocrine function may be carried out according to methods commonly employed for islet transplantation; see, e.g., Ryan et al., Diabetes 50:710-19 (2001); Peck et al., Ann Med 33:186-92 (2001); Shapiro et al., N Engl J Med 343(4):230-8 (2000); Carlsson et al., Ups J Med Sci 105(2):107-23 (2000) and Kuhtreiber, W M, Cell Encapsulation Technology and Therapeutics, Birkhauser, Boston, 1999. Preferred sites of implantation include the peritoneal cavity, the liver, and the kidney capsule.
One of skill in the art will be able to determine an appropriate dosage of microcapsules for an intended recipient. The dosage will depend on the insulin requirements of the recipient. Insulin levels secreted by the microcapsules can be determined immunologically or by amount of biological activity. The recipients body weight can also be taken into account when determining the dosage. If necessary, more than one implantation can be performed as the recipient's response to the encapsulated cells is monitored. Thus, the response to implantation can be used as a guide for the dosage of encapsulated cells. (Ryan et al., Diabetes 50:710-19 (2001))
C. In Vivo Measure of Pancreatic Endocrine Function
The function of encapsulated cells in a recipient can be determined by monitoring the response of the recipient to glucose. Implantation of the encapsulated cells can result in control of blood glucose levels. In addition, evidence of increased levels of pancreatic endocrine hormones, insulin, C-peptide, glucagon, and somatostatin can indicate function of the transplanted encapsulated cells.
One of skill in the art will recognize that control of blood glucose can be monitored in different ways. For example, blood glucose can be measured directly, as can body weight and insulin requirements. Oral glucose tolerance tests can also be given. Renal function can also be determined as can other metabolic parameters. (Soon-Shiong, P. et al., PNAS USA 90:5843-5847 (1993); Soon-Shiong, P. et al., Lancet 343:950-951 (1994)).
All references and patent publications referred to herein are hereby incorporated by reference herein.
As can be appreciated from the disclosure provided above, the present invention has a wide variety of applications. Accordingly, the following examples are offered for illustration purposes and are not intended to be construed as a limitation on the invention in any way.
EXAMPLES
Example 1
Isolation and Initial Culture of Pancreatic Cells (Passage 1 and 2)
Typically, the CD56 positive pancreatic stem cells are isolated from donor pancreas. A mixed population of isolated pancreatic cells is cultured under conditions to promote the growth of the CD56 positive pancreatic progenitor cells.
Organ Procurement
HD407 adult pancreas was harvested from a 20 year old female organ donor. The organ was digested for islet isolation using the following procedure.
To remove the pancreas from the donor, the abdominal aorta was first cannulated below the junction of renal artery. Portal perfusion was done via cannulation of the inferior mesenteric vein. The cannula was inserted up to and above the junction of the portal vein and the splenic vein. A 2-0 tie was put around the splenic vein at the junction of the portal vein. Another 2-0 tie was put around the splenic artery.
The splenic vein was ligated and cut open on the spleen side immediately before the perfusion was started. This method makes pancreatic perfusion more efficient without building up high pressure, which can damage the islets. It also avoids draining the perfusant from spleen and pancreas into the liver. The lesser sac was opened and normal saline slush was applied to pancreas. After one liter of Aortic perfusion, the splenic artery was ligated.
The pancreas was well-protected when the liver and kidney teams dissected the splenic vein and lower gastric vessels. The pancreas was divided at the edge of duodenum, reducing the risk of damage to the pancreas and also reducing the risk of contamination.
The organ was stored in plastic bag filled with UW solution and set in a Nalgene jar with sterile normal saline slush for transportation.
Isolation of Human Islets from Donor Pancreas
Pancreatic tissue was dissociated by mechanical disruption and digestion with Liberase in HBSS (1.5 mg/ml). Two hundred and forty milliliters of Liberase solution was infused into the pancreas via ductal cannulation. The organ was incubated in an 800 ml tempering beaker, at 37° C. until the tissue became soft, about 10 to 20 minutes.
The main duct was removed from the tissue mass which was then transferred into a metal digestion chamber; automatic circulating digestion was started. When free islets appeared in the sample, 200 ml digestant was collected and 120 ml (0.75 mg/ml) fresh Liberase solution was added into the system for further digestion.
After the majority of islets were released from the surrounding tissue the digestant was collected and diluted with Medium A2 (2% FBS in RPMI). The cells were washed with A10 (10% FBS in RPMI) three times, by centrifugation at 4° C. 1,000 rpm, for two minutes.
Islets were separated from acinar cells by a three-layer density gradient separation in a solution of PIPS (Nycodenz (Nycomed AS, Norway) in UW solution) as described in U.S. Pat. No. 5,739,033.
The pellet of washed pancreatic cells was mixed with 320 ml PIPS (density 1.114) and incubated on ice for 10 minutes. Eight 250 ml flat-bottom centrifuge tubes were filled with 70 ml PIPS (density 1.090). Forty milliliters of cell/PIPS suspension was under-laid into each tube. Sixty milliliters of RPMI with 2% FBS was over-laid on top of the PIPS. Tubes were centrifuged using a Sorvall RC-3C Plus with a 05, ARC rotor at 1,500 rpm, for six minutes without braking.
The upper interface, lower interface (mixture of entrapped islets, fragmental islets, acinar and ductal cells), and the pellet (mainly acinar and ductal cells) were collected separately.
Cells were washed two more times with Medium A10. Cells between density gradients 1,090 and 1,114, which contained about 10% of the islet cells, were collected and seeded in tissue culture flasks. The isolated cells were cultured in a mixture of SM95 and M3 medium at a 4:1 ratio. Within 3-5 days, after cells attached to the flask, the cells were switched to 100% SM95 media. The cells were then sub-cultured on day 8 (passage 1, P1), and sub-cultured again (passage 2, P2) on day 12.
Example 2
Selection of CD56 Positive Cells by FACS Sorting
Isolated pancreatic cells are first incubated with a CD56 specific antibody, followed by incubation with a fluorescently-labeled secondary antibody, specific for the CD56 specific antibody. Labeled CD56 positive cells are separated from CD56 negative cells by FACS.
Four dishes of P2 cells were incubated with 0.5% trypsin/0.2% EDTA (Sigma, T3924) for 5 minutes and washed twice in 4° C. PBS. Cells were then washed through a 40 μM cell strainer. Seven million cells were collected. One million cells were used as an isotype staining control; the rest of the cells were used for FACS sorting.
Cells were blocked with 50% normal goat serum at 4° C. for ten minutes and then stained with a 1:20 dilution of anti-CD56 antibody as primary antibody (Hybridoma Bank of University of Iowa) for one hour at 4° C. The cells were washed with 4° C. PBS twice to remove nonbinding antibody and then blocked with 50% normal goat serum at 4° C. for 10 minutes. The cells were then incubated with 1:100 diluted secondary antibody conjugated with FITC for 30 min.
For the control sample, the above primary antibody was replaced by isotype control antibody, anti-mouse IgG. The other steps were same as above.
The FACS machine, a FACSCalibur system from Becton Dickinson, was sterilized by running 10% bleach for 30 minutes and then sterile PBS for 1 hour before use.
The negative control area of FITC intensity on histogram was determined by running the isotype control sample. To avoid noise signal from cell debris, a gate was created for the main cell population. A histogram was generated from this scan. The stained area was marked as negative area (M1). Any stronger stain intensity beyond the M1 is considered a positive result.
The anti-CD56 antibody stained cells were then FACS scanned to determine the percentage of positive staining in the cell population. The intensity in this scan shifted from M1 to stronger side. The area beyond M1 is considered positive staining and was marked as M2.
A sort gate was created in the M2 area before sorting. Any cells located in the gate were considered CD56-positive and were collected by the machine. CD56-positive cells were collected in tubes coated with 4% BSA and five milliliters of M7 to help maintain cell integrity and viability.
Collected cells were centrifuged at 1200 rpm for five minutes and counted. The collected cells were seeded in two 60 millimeter dishes at a density of approximately 1.4×10 5 per dish and cultured in Medium #7 initially. Cells were switched to SM95 media for proliferation.
Example 3
Expansion and Differentiation of CD56 Positive Cells
CD56 positive cells can be grown and expanded in culture for up to ten passages. CD56 cells can be induced to differentiate by increasing culture time and by growing cells on culture dishes coated with collagen IV. Differentiation factors, e.g., hepatocyte growth factor, keratinocyte growth factor, exendin-4, basic fibroblast growth factor, insulin-like growth factor-I, nerve growth factor, epidermal growth factor and platelet-derived growth factor; can be added to augment the differentiation process.
Cell Expansion
Passage 3
The FACS-sorted CD56-positive cells were cultured in M7. An estimated 5% of seeded cells attached to the culture dishes after seven days. The cultures were switched to a mixture media of SM95+M7 medias at a 4:1 ratio for three weeks until sub-cultured.
Passage 4
P3 cells were sub-cultured into a single 1×100 mm culture dish (approximately 8.4×10 4 cells) on day 28 to become passage 4 (P4) cells. The culture of P4 cells was incubated in SM95 media for seven days. During this period the cell growth rate increased significantly.
Passage 5
P4 cells were sub-cultured into two 100 mm culture dishes and a single 60 mm collagen IV coated culture dish. Cells in the 60 mm collagen IV coated culture dish were cultured for one day and fixed for cell identification by in situ insulin mRNA staining.
Passage 6
After six days, the two 100 mm dishes of P5 cells were sub-cultured into two 100 mm culture dishes (P6) and two 6-well plates (P6). One of the 6-well plates was coated with collagen IV. The cells in the 100 mm dishes were cultured in SM95 medium. After seven days, cells from one plate were frozen in liquid nitrogen.
Cells in the 6-well plates were cultured in SM95 for five days and then differentiation or growth factors were added. The following growth factor combinations were used: SM95 only, SM95+50 ng/ml hepatocyte growth factor (HGF or H), SM95+10 ng/ml keratinocyte growth factor (KGF or K), SM95+1 nM Exendin-4 (E), SM95+E+H, and SM95+E+K. Cells were incubated with the growth factors for 48 hours. The plates were fixed and sent for insulin detection by in situ hybridization.
Passage 7
One 100 mm dish of P6 cells was sub-cultured into three 100 mm culture dishes and 2×6-well plates. The original P6 plate was reused for cell culture of P7 cells.
Passage 8
Some of the three 100 mm culture dishes of P7 cells were sub-cultured into three 100 mm dishes to become P8 cells. One of the 100 mm dishes was collagen coated. The remaining P7 cells were sub-cultured into two six-well plates (one collagen IV coated) and two tubes for cryopreservation.
P7 cells from the 6-well collagen IV coated plate were sub-cultured into a second 6-well plate using the same conditions described for passage 6. After incubation, cells were sent for analysis by RT PCR. P7 cells from the uncoated 6-well plate cells were sub-cultured into one 100 mm dish. The 100 mm dish of P8 cells was cultured with SM95.
The P8 cells in the two 6-well plates that were sub-cultured from 100 mm P7 dishes were also grown under the same conditions as P6 cells (one collagen IV coated, one regular). After incubation, the cells were fixed for in situ insulin mRNA staining.
Passage 9
P8 cells from the two uncoated 100 mm culture dishes were sub-cultured into five 100 mm dishes. The cells in the 100 mm collagen IV coated dish were sub-cultured into two 100 mm collagen IV coated dishes.
Part of the cells in the other 100 mm dish was frozen in four tubes and the rests were sub-cultured into two 6-well plates (one collagen IV coated) and cultured in SM95 medium for 5 days, then changed to SM95 media with added factors as listed in passage 6 for two days and fixed for in situ insulin mRNA staining.
Passage 10
Two 100 mm P9 dishes were used for transplantation into two STZ-induced diabetic mice. Two 100 mm P9 dishes were used for CD56 scanning. Two 100 mm P9 dishes were cryopreserved. One 100 mm dish (#9) was subcultured into one 100 mm dish (P10) and cells were also saved for RT-PCR and ICC studies.
Cell Differentiation
Cell differentiation was induced by cell aggregation. Cell aggregation was induced by increasing culture time and coating plates with collagen IV. The differentiation process was augmented by addition of growth and differentiation factors, e.g., hepatocyte growth factor, keratinocyte growth factor, and SM95+1 nM Exendin-4.
Example 4
Characterization of CD56 Sorted Cells and Progeny of CD56 Cells.
After two passages, insulin expression was detected in 70% of the CD56 positive cells by in situ hybridization. After five passages (passage 8) an insulin positive clone developed in CD56 positive cells and was detected using in situ hybridization. Both insulin expression and expression of markers of progenitors of β cells were also detected by PCR in CD56 positive cells treated with differentiation factors at passage 8.
In Situ Hybridization
Cell differentiation was determined by insulin expression, as measured by in situ insulin mRNA assay. Some cell aggregates were washed off at the time of media change. The remaining adherent cells were analyzed.
The protocol used was essentially that of Chitnis et al. and Henrique et al. See e.g., Chitnis et al. Nature 375:761-766 (1995); and Henrique et al Nature 375:787-790 (1995).
Briefly, cultured cells were washed once with PBS and then fixed using 4% formaldehyde in PBS, either for one to two hours at room temp or for two hours to overnight at 4° C. Cells were then washed three times in PBS with 0.1% Tween-20 (PTW). Each wash was ten minutes. Cells were then transferred to 100% MeOH.
Cells were rehydrated with successive washes of 75%, 50%, 25% MeOH/PTW and then washed three times with PTW only. Cells were then treated with 1 μg/ml proteinase K in PTW for 10 minutes at 37° C. using prewarmed solutions. After proteinase K removal, cells were rinsed twice briefly with PTW, and post-fixed for twenty minutes in 4% HCHO+0.1% Glutaraldehyde, in PTW. Cells were then rinsed and washed once with PTW.
For pre-hybridization, cells were rinsed once with 1:1 PTW/hybridisation mix and then rinsed with one milliliter hybridisation mix. One milliliter of fresh hybridisation mix was added and cells were incubated with gentle mixing at least one hour at 65° C.
For hybridization, one milliliter pre-warmed hybridization mix with 1 μg/ml DIG-labeled RNA probe was added to the cells. Cells were incubated with gentle mixing at 65° C./overnight.
The following hybridization mix was used.
TABLE 1
Formamide
50%
25
ml
SSC (20x pH 5 w citric acid!!)
1.3 × SSC
3.25
ml
EDTA (0.5M, pH8)
5 mM
0.5
ml
Yeast RNA (20 mg/ml)
50 μg/ml
125
μl
Tween-20 (10%)
0.2%
1
ml
CHAPS (10%)
0.5%
2.5
ml
Heparin (50 mg/ml)
100 μg/ml
100
μl
H 2 O
17.5
ml
Total
50
ml
After hybridization cells were rinsed twice with hybridization mix pre-warmed to 65° C. Cells were then washed for ten minutes at 65° C. with pre-warmed hybridization mix. Cells were then washed three times for thirty minutes at 65° C. with Washing Solution 1 (50% Formamide/1×SSC/0.1% Tween-20), also prewarmed to 65° C.
A ten minute wash at 65° C. with prewarmed 1:1 Washing solution 1/Maleic Acid Buffer (MABT: 100 mM maleic acid, 150 mM NaCl, 0.1% Tween-20, pH 7.5) followed. Two washes for thirty minutes with MABT followed. Cells were then washed for one hour at room temperature in MABT+2% Boehringer Blocking Reagent.
For secondary antibody, cells were preincubated in two milliliters of MABT+2% BBR+20% heat treated goat serum (65° C. for 30 min), for 1-2 hours. A solution of MABT+2% BBR+20% serum, with a 1/3000 dilution of anti-DIG-AP antibody was added for an overnight incubation at 4° C.
After incubation with secondary antibody, cells were rinsed three times with MABT and then washed three times for one hour with ten to twenty milliliters MABT. Cells were then washed three times for ten minutes with NTMT. (See below.)
Cells were incubated with 1.5 milliliters of NTMT+4.5 μl/ml NBT+3.5 μl/ml BCIP with rocking for first twenty minutes.
Color was developed for a period of thirty minutes to three days. Cells were then washed three times with PTW. Cells were refixed in 4% HCHO/0.1% Glutaraldehyde/PTW, overnight, followed by washes with PTW and storage in PTW/0.1% azide, at +4° C. Cells were then cleared in 50% glycerol/PTW then 80% glycerol/PTW/0.02% azide.
TABLE 2
NTMT:
5M NaCl
1
ml
2M TrisHCl pH9.5
2.5
ml
2M MgCl 2
1.25
ml
10% Tween-20
5
ml
H 2 0
40.25
ml
Total
50
ml
Populations of P2 cells, (e.g., before CD-56 sorting) had very few insulin positive cells. Using in situ hybridization analysis, insulin expression was detected in 70% of CD56-sorted cells at P5. Insulin expression was also detected by in situ hybridization in cells from P6 grown in the absence or presence of various growth factors on collagen IV coated plates or untreated plates.
Insulin positive cells were detected by in situ hybridization in CD56 sorted cells at P8. In addition, an insulin-positive clone was detected in P8 cells grown in the presence of hepatocyte growth factor. Insulin positive cells were still detected by in situ hybridization at P9, although FACS analysis showed CD56 negative cells were present in the P9 cell population.
RT-PCR
PCR was also used to analyze the differentiation state of the cells. Real time RT-PCR was used for analysis of insulin, glucagons, and somatostatin. Regular RT-PCR was used to assay for Hlex9, Pax4, and GLP-1R.
For detection of human Pax4 transcripts, which encode a paired-like homeobox protein, the following PCR primers were used.
Forward primer: 5′GAGGCACTGGAGAAAGAGTT 3′
(SEQ ID NO:1)
Reverse primer: 5′ACTTGAGCTTCTCTTGCCGA 3′
(SEQ ID NO:2)
PCR cycles started with a single three minute incubation at 95° C. The following cycle was repeated forty times: thirty seconds at 95° C.; thirty seconds at 55° C.; one minute at 72° C. PCR ended with a five minute extension at 72° C.
For detection of human Hlxb9 transcripts, a homeobox gene, the following PCR primers were used.
Forward primer: 5′ATGATCCTGCCTAAGATGCC 3′
(SEQ ID NO:3)
Reverse primer: 5′CCATTTCATCCGCCGGTTCTG 3′
(SEQ ID NO:4)
PCR cycles started with a single three minute incubation at 95° C. The following cycle was repeated forty times: thirty seconds at 95° C.; forty-five seconds at 59° C.; one minute at 72° C. PCR ended with a five minute extension at 72° C.
For detection of human Glp-1R transcripts, which encode a glucagons like peptide receptor, the following PCR primers were used.
Forward primer: 5′GTGTGGCGGCCAATTACTAC 3′
(SEQ ID NO:5)
Reverse primer: 5′CTTGGCAAGTCTGCATTTGA 3′
(SEQ ID NO:6)
PCR cycles started with a single three minute incubation at 95° C. The following cycle was repeated forty times: thirty seconds at 95° C.; forty-five seconds at 58° C.; one minute at 72° C. PCR ended with a five minute extension at 72° C.
RT-PCR was used to determine the presence or absence of markers for precursors of beta cells and markers for mature beta cells. Results for markers of mature beta cells, insulin, somatostatin, glucagon, and a glucose transporter isoform (GLUT2) are presented in Table X
TABLE 3
Samples
insulin
Ins/actin
SST/actin
Glucagon/actin
GLUT2/actin
YYY + P8
20800
0.027
0.0012
0.011
9.81E − 05
SM95, collagen IV
YYY + P8
17910
0.024
0.0012
0.013
8.5E − 05
SM95 + HGF
collagen IV
YYY + P8
19020
0.036
0.0014
0.013
0.000123
SM95 + KGF, collagen IV
YYY + P8
21440
0.039
0.0026
0.024
0.000173
SM95 +
exendin-4 collagen IV
YYY + P8
16410
0.033
0.0050
0.017
8.47E − 05
SM95 + E + H collagen IV
YYY + P8
18620
0.034
0.0013
0.018
0.00025
SM95 + E + K collagen IV
Progenitor markers for Beta cell and the beta-cell markers were also detected by RT-PCR. Hb-9 and Pax-4 are transcription factors expressed in the precursor beta cells. Both Hb-9 and Pax-4 were detected in all the CD56-sorted cells at P8 on collagen IV plate, treated with various growth factors. Hb-9 was also expressed in mature beta cells.
The GLP-1 receptor is a marker for mature beta cells. GLP-1 receptor transcript was detected in our CD56-sorted cells at P8, which indicates that the CD56 sorted cells have lineage relation to mature β-cells.
Example 5
In Vivo Function of CD56 Positive Cells and Their Progeny.
Passage 9 cells derived from CD56 positive cells were implanted into SCID mice. After implantation, human C-peptide was detected in the mice indicating the implanted cells secreted insulin in vivo.
Two SCID mice were injected with two million CD56 sorted cells from P9 culture dishes. (E.g., 100 milliliter dish of cells per mouse.) One dish was injected intraperitoneally into SCID mouse #2-22. The other dish was injected subcutaneously into SCID mouse #2-23.
To assess in vivo function of the injected P9 cells, human C-peptide was measured five days after transplantation using an RIA kit from LINCO. Both mice were positive for human C-peptide at day five. The blood Human C-peptide level in SCID mouse #2-22 was 0.1 ng/ml, and in SCID mouse #2-23 was 0.3 ng/ml. This indicates that the CD56 sorted P9 cells had differentiated into mature beta cells and retained their ability to secrete insulin after transplantation.
Example 6
A Time Course Study of the Emergence and Development of CD56+ Cells in Pancreatic Culture
HD418 adult pancreas cells were harvested from a 40 year old female donor. The organ was digested as described above. A mixed population of isolated pancreatic cells were either fixed for CD56 staining with a monoclonal antibody against human CD56 (5.1 H11 antibody) before culture or seeded into four well chamber slides for culture in SM95/M7 (1:1). The cultured cells were fixed and stained with 5.1H11 anti CD56 antibody at day 1, 2, 3, and 9 post seeding.
CD56 expression was determined using immunocytochemical techniques. (Data not shown.) Before culture no CD56 positive cell were detected in the human pancreatic cells enriched with islets. No CD56 positive cells were detected in culture at day one. Detection of CD 56 positive cells begun at 2 days post seeding and CD56 positive cells appeared to increase in cell number from day 2 to day 9.
During the time course, CD56 positive cells largely stayed on top of other cells. CD56 positive cells showed a larger and flattened morphology when they became in direct contact with the plastic surface.
The staining pattern of the CD56 positive cells changed over the time course. At early time points, CD56 staining was evenly distributed throughout the cell surface, but at later time points, the staining became localized to cell borders.
The time course study suggests that, 1) CD56 positive cells emerge as the result of culture, 2) CD56 positive cells are capable of proliferation, and 3) CD56 positive cells undergo dynamic changes in terms of staining patterns and cell morphology in culture.
Example 7
RT-PCR Analysis of CD56 Positively and Negatively Selected Cultured Pancreatic Cells
HD421 adult pancreas was harvested from an 11 year old male donor. The organ was digested as described above. HD421 mixed population pancreatic cells at P0 were cultured in SM95/M7 for a week. 10 7 cells were collected and labeled with 5.1 H11 anti-CD56 antibody for FACS sorting. Five hundred thousand CD56 positive cells and five hundred thousand CD56 negative cells were obtained. Cell aliquots of CD56 positive cells, CD56 negative cells, and unsorted cells were collected for RT-PCR analysis. Genes expressed by mature pancreatic endocrine cells (Ins, Gcg, Sst, GLUT-2, Pax6 and Pdx1) and by pancreatic endocrine progenitor cells (Neuro D, Ngn3,) were analyzed. (See e.g., Wilson M. E. et al, Mechanisms of Development 120:65-80 (2003)).
FIG. 1 demonstrates the relative gene expression levels of unsorted cells, CD56 positive cells and CD56 negative cells. Gene expression was expressed as a ratio of mRNA copy number of the gene of interest (such insulin mRNA copy number) over that of β-actin (mRNA copy number of β-actin). For comparison, the levels of gene expression expressed by unsorted cells were normalized to 1, while the levels of gene expressions expressed by CD56 positively sorted and negatively sorted cells were plotted as folds of increase or decrease relative to that of unsorted cells.
FIG. 1 shows that CD56 positive cells have greater endocrine gene expression than do unsorted cells. Additionally, non-sorted cell have higher endocrine gene expression than do CD56 negative cells.
Example 8
Pancreatic Endocrine Phenotype of Cultured Human Pancreatic Cells Derived from CD56 Positive Cells and CD56 Negative Cells
The endocrine phenotype of cultured pancreatic cells derived from CD56 positive and CD56 negative cells selected using magnetic beads was analyzed. HD440 adult pancreas was harvested from a 45 year old female donor. The organ was digested as described above. The mixed pancreatic cell population was cultured as described above and similar CD56 expression was seen.
Human pancreatic cells collected from HD440 were cultured first in 8:2 ratio of SM95 and M7. The medium was changed to 100% SM95 at the time of first medium change between 2-3 days post seeding and was used for subsequent cultures. At cell passage 1, cultured cells were separated into CD56 (+) and CD56 (−) populations with EasySep Human Positive Selection Cocktail (StemCell Technology, Vancouver, BC, Canada) by the procedures below:
1. The human pancreatic cells were trypsinized and suspended at a concentration of 1×10 8 cells/ml in PBS. The cells then were placed in 12×75 mm polystyrene tubes for placement into the EasySep Magnet. 2. EasySep Positive Selection Cocktail (anti CD56 antibody) was added at 100 μl/ml cells, mixed well, and incubated at room temperature for 15 minutes. 3. Magnetic Nanoparticles were added at 50 μl/ml cells, mixed well, and incubated at room temperature for 10 minutes. 4. The cell suspension was adjusted to a total volume of 2.5 ml by adding PBS. The tube was placed into magnet and set aside for 5 minutes. 5. The supernatant fraction containing CD56-negative cells was poured off. The magnetically labeled cells CD56 positive cells remained inside the tube, held by the magnetic field of the EasySep Magnet. 6. The tube was removed from the magnet and 2.5 ml of PBS was added to the cell suspension and mixed well by gently pipetting up and down 2-3 times. The tube was placed back on the magnet and set aside for five minutes. 7. Steps 5 and 6 were repeated twice for a total of three 5-minutes separations in the magnet. The tube was removed from the magnet, suspended the CD56-positive cells were suspended in the cell culture medium SM95, and incubated in a 5% CO 2 incubator at 37° C. 8. The supernatants containing CD56-negative cells were combined and centrifuged at 1200 rpm for 3 minutes. Cells were suspended in culture medium SM95, and incubated in a 5% CO 2 incubator at 37° C.
The CD56 positive and negative cells were cultured separately, until P8, when they were subjected to differentiation treatment. The levels of insulin gene expression of CD56 positive and negative cells from P2 to P8 were analyzed by RT-PCR. The results are shown in FIG. 2 . Insulin gene expression was consistently higher in CD56 positive cells than in CD56 negative cells throughout the culture period.
P8 cells were cultured in SM 95 for three days, followed by culture in MM1 differentiation media for three days on coated dishes with Poly-ornithine, and then switched to MM2 for another three days.
Step 1: Media component, MM1: Maturation Medium (FIG. 3 )+25 ng/ml bFGF Dish: 15 μg/ml poly-L-ornithine coated Cells: After the cells are trypsinized and neutralized, cells are taken from the supernatant. Cells density: 2 millions/100 mm dish or half millions per well Time: 3˜6 days Media change; every second day Step 2: Media component, MM2: Maturation Medium (FIG. 3 )+10 mM Nicotinomide Dish: 15 μg/ml poly-L-ornithine coated Time: 3˜6 days Media change: every second day
Aggregated cells were assayed for insulin function by using the Static Glucose Stimulation (SGS) assay. CD56 positive cells showed a greater than two fold increase in insulin release in response to glucose challenge. (See, e.g., FIG. 4 .) CD56 negative cells did not show an increase in insulin release in response to glucose challenge. (See, e.g., FIG. 4 .)
Example 9
Proliferation, Cryopreservation, Differentiation, and Functional Characterization of Cultured Human Pancreatic Cells Derived from CD56 (+) Cells
Cultured primary pancreatic cells were FACS sorted at P2 for CD56 positive cells; these cells were continuously cultured as described above. CD56 positive cells at P6 and P8 were cryopreserved and stored in liquid nitrogen. After 15 months of cryopreservation, one vial each of P6 and P8 cells was revived and cultured in a 100 mm tissue culture dishes containing 8 ml of SM95 and 2 ml of M7 media. The two cultures were combined at a subsequent passage to become P8/10. After combination cells were cultured in SM95 media. At P10/12 cells were cultured in SM 95 for three days and passaged into MM1 differentiation media for three days on coated dishes with Poly-ornithine and then switched to MM2 media for another three days. Aggregated cells were collected for RT-PCR in vitro analysis and for transplantation into a diabetic SCID mice for in vivo analysis following alginate encapsulation.
Cultured cells collected at P7 and P9 post thawing, but prior to combination, as well as the combined cells collected at P8/10, P9/11, P10/12 and post maturation treatment at P11/13 were analyzed for insulin gene expression by RT-PCR. As shown in FIG. 5 , the level of insulin gene expression decreased with passage during the proliferation phase. However, the level of insulin gene expression increased following differentiation treatment at P11/13 suggesting that endocrine precursor cells were present in the culture from CD56 positive cells. Those precursor cells responded to the differentiation treatment to mature into cells that produce higher level of insulin than their predecessors cells.
The high level of insulin gene expression was confirmed by the presence of strong insulin producing cells detected by immuno-cytochemstry (ICC) analysis. (Data not shown.) Strong insulin producing cells were not detected in the proliferating cultures prior to the differentiation treatment.
To test in vivo function, P11/13 post differentiation treated cells were macro-encapsulated and transplanted into STZ induced diabetic mice. Aggregated cells were encapsulated using 2% High G alginate, (batch #V4046-02F). The gel was mixed with cell pellet (1:1) and dropped into MC2 (batch # V4011) solution through an 18 gauge needle and allowed to sit for 5 minutes. The beads were then washed 3 times with MCS (V4008).
Mice were prepared for transplantation with anesthesia consisting of Ketamine 50 mg+Rompun 10 mg/kg BW by intramuscular injection. The animal was skin prepped and a med-line incision was made. The alginate beads were implanted into the peritoneal cavity with a scoop. The wound was closed using 4-0 silk stitches.
Cell aggregates derived from cultured HD407 CD56 (+) P11/13 cells were transplanted into the abdominal cavity of diabetic SCID mouse #6 at the dose of approximately 10,000 IEQ/kg. Blood glucose was measured pre- and post-operatively. The result is shown in FIG. 6 . Before transplantation, the mouse blood glucose level was 520 mg/dl. On day 11 after transplantation, the mouse blood glucose was reduced to 409 mg/dl. By day 18, mouse blood glucose levels were 121 mg/dl.
All publications and patent applications cited in this specification are herein incorporated by reference as if each individual publication or patent application were specifically and individually indicated to be incorporated by reference.
Although the foregoing invention has been described in some detail by way of illustration and example for purposes of clarity of understanding, it will be readily apparent to one of ordinary skill in the art in light of the teachings of this invention that certain changes and modifications may be made thereto without departing from the spirit or scope of the appended claims.
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The invention relates to the discovery of a selective cell surface marker that permits the selection of a unique subset of pancreatic stems cells having a high propensity to differentiate into insulin producing cells or into insulin producing cell aggregates.
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BACKGROUND
1. Field
Methods and apparatuses consistent with exemplary embodiments relate to a method of transmitting a moving image and a surveillance system using the method, and more particularly, to a method of transmitting, by a host apparatus, a live-view moving image from a camera or a playback moving image from an image storing apparatus to a client apparatus through a communication network, and a surveillance system using the method.
2. Description of the Related Art
An example of a system that enables a host apparatus to transmit a live-view moving image from a camera or a playback moving image from an image storing apparatus to a client apparatus through a communication network includes a surveillance system.
The resolution of a moving image generated by a photoelectric conversion device of a camera, such as a charge coupled device (CCD), is relatively high. However, it is almost impossible to transmit a live-view moving image having high resolution to a client apparatus through a communication network.
Accordingly, a host apparatus drastically reduces the resolution of a moving image and then transmits the moving image having low resolution to the client apparatus. Thus, a user of the client apparatus may feel inconvenience due to an unclear moving image in a region of interest.
SUMMARY
One or more exemplary embodiments include a method of transmitting a moving image, wherein, when a host apparatus transmits a live-view moving image from a camera or a playback moving image from an image storing apparatus to a client apparatus through a communication network, the host apparatus is able to transmit a moving image effective to a user to the client apparatus regardless of a data amount, i.e., even if the data amount is relatively small, and a surveillance system using the method.
Additional aspects will be set forth in part in the description which follows and, in part, will be apparent from the description, or may be learned by practice of the exemplary embodiments.
According to an aspect of an exemplary embodiment, there is provided a method of transmitting a moving image, the method including: receiving a frame image having a first resolution from a camera; generating a first frame image having the first resolution and a second frame image having a second resolution with respect to the frame image of the moving image; extracting an image of a setting region from the first frame image having the first resolution that is higher than the second resolution; generating a combined frame image by combining the extracted image of the setting region and the second frame image having the second resolution; and transmitting the combined frame image to a client apparatus.
The transmitting of the combined frame image may include transmitting the second frame image having the second resolution and the extracted image of the setting region together.
According to an aspect of another exemplary embodiment, there is provided a method of transmitting a moving image, the method including: receiving a frame image having a first resolution from a camera; generating a first frame image having the first resolution and a second frame image having a second resolution with respect to the frame image of the moving image; extracting an image of a setting region from the second frame image having the second resolution that is lower than the first resolution; generating a combined frame image by combining the extracted image of the setting region and the first frame image having the first resolution; and transmitting the combined frame image to a client apparatus.
According to an aspect of another exemplary embodiment, there is provided a method of transmitting a moving image, the method including: receiving a frame image of the moving image from a camera; generating two frame images having different resolutions with respect to the frame image of the moving image; extracting an image of a setting region from one of the two frame images; generating a combined frame image by combining the extracted image of the setting region and the other one of the two frame images; and transmitting the combined frame image to a client apparatus.
According to an aspect of another exemplary embodiment, there is provided a surveillance system which uses the method of transmitting a moving image.
BRIEF DESCRIPTION OF THE DRAWINGS
These and/or other aspects will become apparent and more readily appreciated from the following description of the exemplary embodiments, taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a diagram of a surveillance system using a method of transmitting a moving image, according to an exemplary embodiment;
FIG. 2 is a diagram for describing the method of FIG. 1 , according to a first exemplary embodiment;
FIG. 3 is a flowchart for describing operations of a host apparatus of FIG. 1 performing the method according to the first exemplary embodiment of FIG. 2 ;
FIG. 4 is a diagram of an example of a frame image having a second resolution in FIG. 2 ;
FIG. 5 is a diagram of an example of a frame image having a first resolution, which is obtained by enlarging a setting region of the frame image of FIG. 4 ;
FIG. 6 is a diagram of an example of a combined frame image transmitted according to the first exemplary embodiment of FIG. 2 ;
FIG. 7 is a diagram for describing a method of transmitting a moving image, according to a second exemplary embodiment;
FIG. 8 is a flowchart for describing operations of the host apparatus of FIG. 1 performing the method according to the second exemplary embodiment of FIG. 7 ; and
FIG. 9 is a diagram of an example of a combined frame image transmitted according to the second exemplary embodiment of FIG. 7 .
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
The following descriptions and accompanying drawings are for understanding one or more exemplary embodiments, and well-known functions or constructions are not described in detail since they would obscure the exemplary embodiments with unnecessary detail.
Also, the descriptions and drawings are not provided to limit one or more exemplary embodiments, and the range of one or more exemplary embodiments shall be determined by claims. Terms used herein shall be construed as having meanings and concepts corresponding to technical aspects of the one or more exemplary embodiments to most suitably describe the one or more embodiments.
Reference will now be made in detail to exemplary embodiments which are illustrated in the accompanying drawings, wherein like reference numerals refer to like elements throughout. Expressions such as “at least one of,” when preceding a list of elements, modify the entire list of elements and do not modify the individual elements of the list.
FIG. 1 is a diagram of a surveillance system using a method of transmitting a moving image, according to an exemplary embodiment.
In FIG. 1 , D IMA denotes moving image data input to a communication network 4 , for example, the Internet, from each of cameras 1 a through 1 n , or moving image data input from the communication network 4 to each of client apparatuses 3 a through 3 n.
D COM denotes a communication signal between each of the cameras 1 a through 1 n and the communication network 4 , or a communication signal between the communication network 4 and each of the client apparatuses 3 a through 3 n.
D IMAT denotes complex moving image data input from the communication network 4 to a host apparatus 2 , or complex moving image data input from the host apparatus 2 to the communication network 4 .
D COMT denotes a complex communication signal between the host apparatus 2 and the communication network 4 .
Referring to FIG. 1 , the host apparatus 2 is connected to the cameras 1 a through 1 n and the client apparatuses 3 a through 3 n through the communication network 4 , such as the Internet. Here, the number of client apparatuses 3 a through 3 n is generally higher than the number of cameras 1 a through 1 n.
The cameras 1 a through 1 n transmit the moving image data D IMA of a live-view to the host apparatus 2 while communicating with the host apparatus 2 .
The host apparatus 2 may store and transmit the moving image data D IMA from the cameras 1 a through 1 n while loading the moving image data D IMA in a volatile memory, or store the moving image data D IMA in a nonvolatile memory. For example, the host apparatus 2 may transmit the moving image data D IMA loaded according to channels from the volatile memory to the client apparatuses 3 a through 3 n , or store, in a recording medium such as a hard disk drive, the moving image data D IMA .
The host apparatus 2 may generate two frame images having different resolutions, extract an image of a setting region from one of the two frame images, and combine the extracted image of the setting region and the other one of the two frame images to obtain a combined frame image. Here, the setting region may be a region fixed by a user, or a variable region, such as a motion detecting region. Since technologies of motion detection and face recognition are well known, descriptions thereof are not provided.
By transmitting the combined frame image to at least one of the client apparatuses 3 a through 3 n , a moving image may be effectively transmitted to the at least one of the client apparatuses 3 a through 3 n even if the moving image has a relatively low amount of data.
For example, if a resolution of the image of the setting region is relatively high and a region of interest to a user of the at least one of the client apparatuses 3 a through 3 n is the setting region, the user may conveniently view the moving image since the region of interest may be clear. This will be described in more detail with reference to FIGS. 2 through 6 .
On the other hand, if the resolution of the image of the setting region is relatively low and a photographing refrain region, such as private region, is the setting region, a function of the photographing refrain region may be conveniently performed and an amount of transmission data may be reduced. This will be described in more detail later with reference to FIGS. 7 through 9 .
FIG. 2 is a diagram for describing the method of FIG. 1 , according to a first exemplary embodiment. FIG. 3 is a flowchart for describing operations of the host apparatus 2 of FIG. 1 performing the method according to the first exemplary embodiment of FIG. 2 . The method according to the first exemplary embodiment will now be described with reference to FIGS. 1 through 3 .
Any one of the cameras 1 a through 1 n transmits a frame image 201 having a first resolution, i.e., a high resolution, to the host apparatus 2 . If the frame image 201 is compressed, the host apparatus 2 restores the frame image 201 . That is, the frame image 201 is a restored frame image. For example, the frame image 201 may be a playback moving image from an image storing apparatus included in the host apparatus 2 .
When the frame image 201 is input from the any one of the cameras 1 a through 1 n in operation S 301 , the host apparatus 2 generates a frame image 203 having a second resolution that is lower than the first resolution in operation S 303 .
In other words, the host apparatus 2 generates a frame image 203 H having the first resolution, i.e., the high resolution, and the frame image 203 L having the second resolution, i.e., the low resolution, according to a resolution changing program 202 . Since a resolution changing algorithm is well known, descriptions thereof are not provided.
The frame image 201 and the frame image 203 H are the same frame images. In other words, the host apparatus 2 only generates the frame image 203 L according to the resolution changing program 202 . Alternatively, the host apparatus 2 may generate the frame image 203 H having a resolution that is higher than the second resolution and lower than the first resolution according to the resolution changing program 202 .
Next, the host apparatus 2 extracts an image 204 of a setting region from the frame image 203 H, in operation S 305 .
Then, the host apparatus 2 generates a combined frame image 205 by combining the image 204 and the frame image 203 L, in operation S 307 .
Then, the host apparatus 2 transmits a compressed combined frame image 208 to at least one of the client apparatuses 3 a through 3 n , together with a compressed frame image 207 having the second resolution and a compressed image 206 of the setting region, in operation S 309 .
In operation S 309 , the host apparatus 2 compresses the image 204 , the frame image 203 L, and the combined frame image 205 to generate the compressed image 206 , the compressed frame image 207 , and the compressed combined frame image 208 , respectively.
Then, the host apparatus 2 transmits the compressed combined frame image 208 , together with the compressed frame image 207 and the compressed image 206 . The host apparatus 2 may transmit only the compressed combined frame image 208 to the at least one of the client apparatuses 3 a through 3 n.
By transmitting the compressed frame image 207 and the compressed image 206 in operation S 309 , the at least one of the client apparatus 3 a through 3 n may display the compressed frame image 207 and the compressed image 206 together in a form of picture-in-picture (PIP). Accordingly, the user of the at least one of the client apparatuses 3 a through 3 n may immediately determine whether the compressed image 206 is located in the compressed frame image 207 . A reference numeral 209 in FIG. 2 denotes a PIP image obtained by restoring the compressed frame image 207 and the compressed image 206 by the at least one of the client apparatuses 3 a through 3 n . Also, a reference numeral 210 of FIG. 2 denotes a main image obtained by restoring the compressed combined frame image 208 by the at least one of the client apparatuses 3 a through 3 n.
Operations S 301 through S 309 are repeated until an end signal is received in operation 5311 .
FIG. 4 is a diagram of an example of a frame image 401 having a second resolution in FIG. 2 . FIG. 5 is a diagram of an example of a frame image 501 having a first resolution, which is obtained by enlarging a setting region of the frame image 401 of FIG. 4 . FIG. 6 is a diagram of an example of a combined frame image 601 transmitted according to the first exemplary embodiment of FIG. 2 .
Referring to FIGS. 4 through 6 , an image 601 A of a setting region in the combined frame image 601 is clearer than an image 401 A of a setting region in the frame image 401 .
When a resolution of the image 601 A of the setting region is relatively high and a region of interest to the user of the at least one of the client apparatuses 3 a through 3 n is the image 601 A of the setting region, the user may conveniently view a moving image since the region of interest is clear.
According to the first exemplary embodiment described above with reference to FIGS. 2 through 6 , since the combined frame image 601 is transmitted to the at least one of the client apparatuses 3 a through 3 n , a moving image may be effectively transmitted to the at least one of the client apparatuses 3 a through 3 n even if the moving image has a relatively low amount of data.
FIG. 7 is a diagram for describing a method of transmitting a moving image, according to a second exemplary embodiment. FIG. 8 is a flowchart for describing operations of the host apparatus 2 of FIG. 1 performing the method according to the second exemplary embodiment of FIG. 7 . The method according to the second exemplary embodiment will now be described with reference to FIGS. 1, 7, and 8 .
Any one of the cameras 1 a through 1 n transmits a frame image 701 having the first resolution, i.e., the high resolution, to the host apparatus 2 . Here, if the frame image 701 is compressed, the host apparatus 2 restores the frame image 701 . That is, the frame image 701 is a restored frame image. For example, the frame image 701 may be a playback moving image from the image storing apparatus included in the host apparatus 2 .
When the frame image 701 is input from the any one of the cameras 1 a through 1 n in operation S 801 , the host apparatus 2 generates a frame image 703 L having the second resolution that is lower than the first resolution in operation S 803 .
In other words, the host apparatus 2 generates a frame image 703 H having the first resolution, i.e., the high resolution, and the frame image 703 L having the second resolution, i.e., the low resolution, according to a resolution changing program 702 . Since a resolution changing algorithm is well known, descriptions thereof are not provided.
The frame image 701 and the frame image 703 H are the same frame images. In other words, the host apparatus 2 generates only the frame image 703 L according to the resolution changing program 702 . Alternatively, the host apparatus 2 may generate the frame image 703 H having a resolution that is higher than the second resolution and lower than the first resolution.
Then, the host apparatus 2 extracts an image 704 of a setting region from the frame image 703 L in operation S 805 .
Next, the host apparatus 2 generates a combined frame image 705 by combining the image 704 and the frame image 703 H in operation S 807 .
Then, the host apparatus 2 transmits the combined frame image 705 to at least one of the client apparatuses 3 a through 3 n in operation S 809 . The host apparatus 2 may generate a compressed combined frame image by compressing the combined frame image 705 , and transmit the compressed combined frame image to the at least one of the client apparatuses 3 a through 3 n . A reference numeral 710 of FIG. 7 denotes an image obtained by restoring the compressed combined frame image by the at least one of the client apparatuses 3 a through 3 n.
Operations S 801 through S 809 are repeated until an end signal is received in operation 5811 .
FIG. 9 is a diagram of an example of a combined frame image 901 transmitted according to the second exemplary embodiment of FIG. 7 .
Referring to FIG. 9 , when a resolution of an image 901 A of a setting region is relatively low, and a photographing refrain region, such as a private region, is the image 901 A of the setting region, a function of the photographing refrain region may be conveniently performed and an amount of transmission data may be reduced.
According to the second exemplary embodiment described with reference to FIGS. 7 through 9 , by transmitting the combined frame image 901 to at least one of the client apparatuses 3 a through 3 n , a moving image may be effectively transmitted to the at least one of the client apparatuses 3 a through 3 n even if a data mount of the moving image is relatively low.
As described above, according to one or more exemplary embodiments, after two frame images having different resolutions are generated, an image of a setting region is extracted from one of the two frame images and the extracted image is combined to the other one of the two frame images to obtain a combined frame image.
By transmitting the combined frame image to a client apparatus, a moving image may be effectively transmitted to the client apparatus even if the moving image has a relatively low amount of data.
For example, if a resolution of the image of the setting region is relatively high, and a region of interest to a user of the client apparatus is the setting region, the user may conveniently view the moving image since the region of interest is clear.
On the other hand, if the resolution of the image of the setting region is relatively low, and a photographing refrain region, such as a private region, is the setting region, a function of the photographing refrain region may be conveniently performed and an amount of transmission data may be reduced.
The exemplary embodiments can be implemented through computer readable code on a computer readable recording medium to control at least one processing element to implement any above-described embodiment. The computer readable recording medium may be any type of recording device that stores data which can be read by a computer system.
The computer readable recording medium may include read-only memory (ROM), random-access memory (RAM), CD-ROMs, magnetic tapes, floppy disks, optical data storage devices, etc. The computer readable recording medium can also be distributed over a network coupled to computer systems so that the computer readable code is stored and executed in a distributive manner. Furthermore, the processing element may include a processor or a computer processor, and processing elements may be distributed and/or included in a single device.
It should be understood that the exemplary embodiments described herein should be considered in a descriptive sense only and not for purposes of limitation. Descriptions of features or aspects within each exemplary embodiment should typically be considered as available for other similar features or aspects in other exemplary embodiments.
While one or more exemplary embodiments have been described with reference to the figures, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the inventive concept as defined by the appended claims.
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A method of transmitting a moving image and surveillance system using the method are provided. The method includes: receiving a frame image having a first resolution from a camera; generating a first frame image having the first resolution and a second frame image having a second resolution with respect to the frame image of a moving image; extracting an image of a setting region from the first frame image having the first resolution that is higher than the second resolution; generating a combined frame image by combining the extracted image of the setting region and the second frame image having the second resolution; and transmitting the combined frame image to a client apparatus.
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BACKGROUND OF THE INVENTION
(1) Field of the Invention
The present invention relates generally to the field of coatings compositions generally classified in class 106 and/or class 428 of the U.S. Pat. and Trademark Office classification system.
This application relates to the general field of co-pending U.S. Ser. No. 382,853 filed May 24, 1982, now abandoned.
(2) Description of the Prior Art
The known art for drying or curing resins including principally alkyd resins comprises metal-catalyzed oxidation reactions through the unsaturation of the body of the resin polymer. These conventional types of drying agents have been used for many years and the research is voluminous on this subject. The oxidative process is very useful and produces most of the alkyd coatings used commercially today. However, the oxidative process has always been limited by the concentration of the unsaturation of the resin polymer. Therefore, a very long or long oil type alkyd (e.g. produced using more than 60% by weight of the fatty acid oil) could not be satisfactorily cured by the oxidative method. Even medium length alkyd polymers are hindered by the oxidative curing process because of the time required and the heat energy and heating apparatus necessary to shorten the cure time to meet commercial production schedules. The higher molecular weight alkyd resins of the very long to medium long oil types are conventionally caused to dry by cross linking them by the addition of melamine type driers and/or substitution of urea-formaldehyde type resins. Such formulations also require high energy levels for cure and involve up to several minutes of dwell time in the oven (e.g. 10 minutes at about 400° F. to 7 days at temperatures of 200° F.). These melamine and urea-formaldehyde cured alkyd systems also give off toxic formaldehyde.
In contrast, the present carbodiimide driers become totally a part of the alkyd resin and the systems of the present invention do not produce odors, fumes, or evolution of toxic or corrosive substances through the atmosphere, other than the natural evaporation of whatever solvent is chosen for use with the system of the invention.
The literature contains many teachings of preparation of carbodiimides and polycarbodiimides.
U.S. Pat. No. 3,755,242 to Reich (Class 524, subclass 437) teaches preparation of isocyanade-terminated high molecular weight polycarbodiimides.
U.S. Pat. No. 3,450,669 to Nolen (Class 524, subclass 133) teaches use of carbodiimides as a stabilizer for polyesters, polyethers and polymethanes.
U.S. Pat. No. 2,430,479 to Pratt et al (Class 154, subclass 140) teaches the use of polycarbodiimides as adhesives and adhesive modifiers.
It is known that many carbodiimides and polycarbodiimides moieties are formed in the production of copolymer foams utilizing the reaction of organic polyiscyanurates with polycarboxilic compounds.
U.S. Pat. No. 3,644,234 to Grieve (Class 260, subclass 2.5) and U.S. Pat. No. 3,723,364 to McLaughlin et al (Class 521, subclass 157) teach the above production of copolymer foams.
U.S. Pat. No. 4,118,536 to Beardsley et al (Class 427, subclass 385) teaches the use of carboxidiimides as primers and as ingredients in composite coatings.
West German DT-OS No. 2,655,836 now U.S. Pat. No. 4,060,664 (assigned 3M), class 156, subclass 331.1 discloses a novel adhesive composite coating wherein the intermediate layer is comprised of polymeric polycarbodiimides.
U.S. Pat. No. 3,556,829 to Gebura (CLass 106, subclass 288) discloses the use of carbodiimides to modify clays used in coating manufacturing.
U.S. Pat. No. 3,619,236 to Dappen et al (Class 430, subclass 621) teaches use of carbodiimides with gelatin and carboxyl-containing polymers as a support to provide photographic materials of improved dimensional stability.
All of the above references show the benefits of the carbodiimide moieties in coatings of many different types. However, none of these references teaches or suggests that the carbodiimides, polycarbodiimides or substituted carbodiimides are excellent driers for alkyd resins, polyesters, polyacrylate-type polymers or any of the resins or polymers that contain carboxylate groups having at least one active (labile) hydrogen molecule.
The driers of the present invention provide cross-linking for the alkyd type resins, polyesters, polyacrylates, modified vinyl-acrylics, epoxides, urethanes and polyurethanes, metal salts, e.g., Ca, Co, Cu, Pb, Mn, Ti, Zr, salts of acids and the melamines, urea-formaldehyde, aziridines and peroxides are the most conventional driers presently used. All of these conventional driers have some disadvantages; the metal salts in many cases cause slow drying, require heat or combination of long drying time plus heat to obtain thorough cure or drying. The melamine types all give off formaldehyde and most require relatively long curing periods at ambient temperatures. The aziridines are toxic and hydrolize easily in water systems and have relatively short shelf life or storage time. The organic peroxides are hazardous and require special handling and storage and only work for a free-radical polymerization. The urea formaldehyde types require high energy for cure and give off formaldehyde during cure.
In contrast, the carbodiimides, polycarbodiimides and substituted carbodiimides of the present invention avoid all of the above disadvantages.
From the above review of the art, it is apparent that the driers and cross-linking agents conventionally used today do not produce finished products with all the properties desired. Many attempts have been made to dry alkyd resins at ambient room temperature in relatively short periods of time. Those familiar with the art know that new driers are needed that will cause the alkyd resins to harden and present water resistance in a short time. The carbodiimides and related compounds described in this invention impart those desired properties to the alkyd polymers and copolymers.
SUMMARY
(1) General Statement of the Invention:
The present invention involves the discovery that carbodiimide driers, including polycarbodiimides and substituted carbodiimides provide fast drying coatings even at ambient temperatures and even using relatively long oil, alkyd resins high solids alkyd, polyester and acrylic resins and, further provide coatings which rapidly become firm, tough, hard and resistant to moisture and salt spray. Additionally, the driers of the present invention do not give off noxious or other by-products produced by the drying mechanism thus minimizing difficulties with pin-holing, corrosion of coated parts and apparatus, and holidays.
These driers are applicable for any class of polymers or compounds that have carboxylic groups containing at least one active hydrogen.
While not wishing to be held to any theory or mechanism of the present invention, the general reaction appears to follow the following: ##STR1## Where R and R 1 are hydrocarbon or hydrocarbon substituted with groups which do not interfere with the above reaction; preferably as described infra.
(2) The Utility of the Invention:
As mentioned above, the invention provides valuable coating formulations having excellent hardness, toughness, humidity and salt spray protection and good storage stability and capable of rapid drying at ambient temperatures without evolution of by products.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Starting Materials
Carbodiimides and Related Compounds:
As described above, the carbodiimides of the present invention can be carbodiimides, substituted carbodiimides, polycarbodiimides and substituted polycarbodiimides.
The preferred carbodiimides are those produced by the techniqures of U.S. Pat. Nos. 2,938,892 and 3,135,748. Suitable carbodiimides and related compounds are available from Union Carbide Corporation of Danbury, Conn. under the tradename "UNEL Cross-linking Agent" with preferred cross-linkers being designated by Union Carbide as "UNEL XL 20" and "UNEL XL 20E".
For water systems, the carbodiimides are preferably purchased or prepared as a water-based emulsion. For organic solvent based systems, the preferred form is the amyl acetate solution of the carbodiimide or mixed acetate solutions of lower flash points or the related compound. Both of these forms are available from the aforementioned Union Carbide Corporation.
The coating composition can contain about 0.1 to about 40% by weight of the carbodiimide or related compound, more preferably from about 0.5 to about 25% and most preferably from about 1 to 15% of the carbodiimide or related compound.
All percents given herein are percents by weight based on the dry weights of the materials excluding the weights of solvents unless otherwise expressly stated.
The carbodiimides of the invention are represented by the formula:
R--N═C═N--R'
Where R and R prime may be symmetrical or asymmetrical, alkyl or aryl, aliphatic or dialiphatic and the aryl and aliphatic groups may be substituted or unsubstituted with halogens, cyano, nitro, amino, alkylamine, alkoxy carbonyl or other substituents which do not interfere with the reactions of the invention e.g. by steric hindrance or causing competing side reactions. R and R' preferably contain from about 30 to 75, more preferably from about 55 to about 65 and most preferably from 45 to about 60 carbon atoms.
The carbodiimides of the present invention include, inter-alia, any of the compounds that are conveniently prepared by the techniques disclosed in U.S. Pat. No. 2,938,892 to Sheenan (Class 260, subclass 112) and U.S. Pat. No. 3,135,748 to Little (Class 544, subclass 164).
R and R' may alternatively be aromatic and hetrocyclic components substituted with any of the above stated classes of substituents.
Resins:
Suitable resins can be alkyds e.g. preferably those available from Cargill under the brand name "7472"; Spencer-Kellogg under the brand name "9706" or 3907GB74 under the brand name "KELSOL" polyesters including preferably those available from Reichold Chemicals Co. under the brand name "BECKOSOL" and particularly those available from Ashland Chemical Company of Columbus, Ohio under the designation ARAPOL; acrylics including preferably those available from ROHM & HAAS under the designation "Rhoplex"; epoxides including preferably those available from Cargill under the designation "Resin Code 1161, 1162, 1170, 1202-1206"; phenolics including preferably those available from Union Carbide under the designation "Ucars"; modified acrylics including preferably those available from Union Carbide under the designation "Ucars"; modified vinyls and urethanes including preferably those available from WITCO under the designation "Castomer". Other resins which can conventionally be substituted for the above resins will also be applicable to the formulations to the invention.
The resins must contain one or more carboxylate groups containing active hydrogen(s) and can be selected according to the criteria generally skilled in the art of coating compositions.
The carboxylate will preferably be present in at least the stoichiometric quantity required to react with the drying agent, including the carbodiimides and related compounds together with any other drying agent which might be add mixed to provide a special formulation. (It is a feature of the present invention that the carbodiimides do not interfere with the function of the conventional drying agents which may be useful with the formulation and maybe added to these drying agents.) Alternatively, in special formulations the carbodiimides or related compounds may be substituted for conventional drying agents.
The organic carboxylate resins will preferably be present in the formulation in an amount of about 1.0 to about 99.5% by weight (dry basis), more preferably from about 15 to about 60% and most preferably to about 2.0 to 20%.
Other Drying Agents:
As mentioned above, other conventional drying agents may be utilized in conjunction with the carbodiimides though they are not necessarliy required. Such drying agents can include all of those conventionally known to the art including metal driers such as the metal type driers mentioned under "Background of the Invention."
Resins-Polyol Esters
The esters useful for the present invention are preferably polyfunctional esters of carboxylic acids, preferably of fatty acids having 6 to 30 carbons. Mono-esters may find occasional use in special circumstances. Particularly preferred are the polyesters of naturally-derived fatty acids such as organic acid esters of glycerin, coconut oil, tall oil, soya oil acids, stearic acid, preferably, isostearic acid, oleic acid, linoleic acid and polyols, e.g. neopentylglycol, trimethylol propane and pentaerythrol. Most preferred is the dilanolinic acid ester of pentaerythritol.
Useful commercial polyol esters comprise: "Pentalan" from Croda Chemical Company of England, a tetrahydric lanolin alcohol; Degras manufactured by Emory Industries of Linden, N.J., and FAI manufactured by Azirona Chemical of New York City.
The quantity of esters employed with the present invention will not be narrowly critical and will depend to a substantial degree on the other ingredients and their amounts as selected for the particular formulation. Preferably the compositions will contain from about 5% to about 95%, more preferably from about 5% to about 10% and most preferably from about 8% to about 12% percent esters based on the total weight of the esters as compared to the total dry weight of the formulation. In most cases, the acid number of the polyester will be determined and from about 50 to 110% of stochiometric amount of carbodiimide (more preferably about 70 to 100 and most preferably 80 to 95%) will be added.
Surfactants (optional)
Surfactants useful with the present invention include natural surfactants such as salts of oleic acid, e.g. morpholine salts of oleic acid, or the similar salt or triethanolamine and entirely synthetic surfactants such as alkanol amide, e.g. Tamol 850 (Rohm & Haas, Philadelphia) or Igepals (GAF Corp. NYC) or WHC by Stephan Chemical Company of Chicago, Ill. (oleyl diethanol amide), sorbitan monooleates manufactured by ICI America of Wilmington, Del., isostearic acids salts, coconut oil salts, lauric acid salts and the like. Excess carboxylic acid, e.g. in wax components, can react with amines in situ to form salts which act as surfactants. The preferred range is about 2 to 8% carboxylic acid and about 1 to 5% amine. All or part of the surfactant can be organic sulfonates, e.g. alkyl lauryl sulfonate or alkyl benzene sulfonates.
Suitable surfactants comprise the reaction products of amines such as morpholine, thiethanolamine, ammonia, diethanolamine and ethanolamine with carboxylic acids such as those mentioned above. The compositions of the present invention will generally include surfactants in the amount of from about 0.1 to 15%, more preferably from about 0.5 to about 5% and most preferably from about 1 to 2 percent by weight based on the dry weight of the formulation. However, this will vary in response to the selection and quantities of the other ingredients employed.
Coupling Agents:
Coupling agents can be used with the invention. Preferred coupling agents comprise C 5 -C 30 liquid hydrocarbon components with C 2 -C 20 alcohol in a weight ratio of between 1:1 to 10:1.
Several types of coupling agents can be employed with the invention including mineral spirits, e.g. ethylene glycol ethers, preferably butyl and propyl ethers; hydroxy ethers (ether-alcohols), such as propyl cellosolve, (Ektasolve EP manufactured by Eastman Kodak of Rochester, N.Y.) diethylene glycol monoethyl ether, monopropyl ether of ethylene glycol, propyl cellosolve, ethyl cellosolve, and diethylene glycol monoethyl ether and other coupling agents which will be evident to those skilled in the art for use in specialized formulations according to the present invention. The coupling agent is selected by physical test; substituted alcohols or hydrocarbons and anything which does not interfere with the formulations of the present invention and which renders their ingredients mutually soluble in the water base will generally be acceptable.
Alcohol ether-esters may also be used e.g. ethylene glycol monoacetate, diethylene glycol monoproprionate, diethylene glycol monoacetate and propylene glycol monoacetate.
Alcohols, such as ethanol, isopropanol and isobutanol will generally be useful as coupling agents for the invention. Other commercial coupling agents which are useful with formulations of the present invention include: Ektasolve EP, manufactured by Eastman Kodak of New York, and Propasol P, manufactured by Union Carbide of Danbury, Conn.
The coupling agents of the present invention will generally be employed in quantities of from about 5 to about 35% or more, more preferably from about 8 to about 25% and most preferably from about 10 to about 20% based on the dry weight of the formulation. In addition to acting as a coupling compound, the coupling agent will usually be useful during the drying and curing process after application of the coatings composition of the present invention to substrates. For example, when carefully selected, the coupling agent will form an azeotrope with the water present in the formulation, thus increasing volatility, speeding cure, and providing a more permanent coating. Some coupling agents will assist the final coating in other ways, e.g. by providing leveling of the final coating, avoiding pinholes, and providing a more continuous, better quality dry film.
In organic-solvent based formulations, the coupling agent can serve as part or all of the solvent.
Water:
Deionized water will preferably be employed with the formulations of the present invention which are water based in order to prevent reaction of chlorine, calcium, magnesium or other components of tap water from interfering with the formulations of their curing. Distilled water could, of course, be employed but will general be avoided for economic reasons.
Solvents:
Conventional solvents, e.g. amyl or butyl acetates, ketones (MEK, etc.), acetone, alcohols mineral spirits and the like can be used with those formulations of the invention which are organic solvent based.
Those formulations of the present invention which are water-based will generally contain a minimum of about 8%, more preferably 10% and most preferably 50% or even more of water based on the total weight of the formulation. As the formulations of the present invention are generally classifiable as oil-in-water emulsions of special character, a quantity of water greater than about 92% may cause swelling and loss of wetting properties in most of the formulations of the present invention although specialized formulations utilizing carefully selected non-aqueous ingredients may tolerate water up to an amount of 97% by weight based on the weight of the total formulation.
pH:
The pH of this system will be preferably in the range of 7 to 10 with 8 to 9 being preferred. The nature of the system will depend heavily upon the amount of soap produced when the emulsifying agent (fatty acid) is neutralized with an alkaline material (e.g. amines, triethanolamine, morpholine). One should slightly overbase (make alkaline) the system to obtain maximum production by reacting any residual acids which may be left over at the normal end point of titration.
Techniques in Mixing:
Apparatus: The apparatus for the present invention will be that conventionally utilized in the preparation of coatings compositions, e.g. kettles and mixing tanks having flow metering or measuring devices and agitation means, e.g. pumps mounted on side-arms connecting with the main vessel, internal stirrers, contra-rotating shearing devices and any of the other available devices which are well known to the art.
Temperature: The temperature during mixing may be different during different stages in the formulation. In general the water will be at about room temperature, the non-aqueous ingredients will be transferred and mixed together at about room temperature. However, temperatures are not narrowly critical and will vary to provide faster mixing or better compatibility of ingredients according to observation of those skilled in the art. For example, pressure vessels may be utilized for the purpose of lowering ingredient melting and boiling points, where useful, in order to provide better dispersion of difficult-to-mix ingredients.
Mixing Procedure: While the formulations of the present invention may be manufactured continuously if desired, batch techniques will be more usually employed. For example, see Example No. 1. The carbodiimide or related compound wax, if any, esters, surfactants, coupling agents and any other non-aqueous ingredients are fed to the same vessel with the various non-aqueous ingredients being added slowly while the vessel is agitated with conventional mixer. In most cases, the esters will be added with the carboxylic acids; the neutralizing ingredient, e.g. morpholine, triethanolamine, will be added after the other ingredients have been thoroughly mixed. After neutralization, which is generally visually observable as a distinct increase in viscosity, the non-aqueous ingredients are allowed to mix for 15 to 30 minutes and transferred over to the aqueous phase, which is agitated during the addition of the non-aqueous phase. Generally, the carbodiimide or related compound is added last, as an oil-in-water emulsion (for water-based formulations) or as a organic solvent solution (for organic solvent-based formulations). The finished formulation is allowed to cool with preferably constant, agitation, after which the formulation is drawn off into shipping containers, e.g. tank cars, tank trucks, drums or smaller cans.
Quality Control:
The finished formulation, prior to packaging will generally be checked for pH, solids content, freeze-thaw stability, corrosion-protection under accelerated conditions and other tests utilizing techniques well known to the coatings industry.
Application:
The formulations of the present invention may be applied to substrates to be protected by conventional application techniques, such as spraying, brushing, roller-coating, dipping, flow-coating, electrostatic airless spraying, etc. Coating thickness can be varied by changing the formulation, the number of coats, or the amount applied per coat but in general will be in the range from about 0.5 mils to about 10 mils per coat after drying.
EXAMPLES
Example 1
(Reference B1346--1 to 3)
(Formulation according to the invention providing a good storage life and long term protective coating). 24.935 parts of deionized water are charged to a conventional mixing kettle of a high sheer disperser (type cowles dissolver). The water agitating at low to moderate speed add 0.598 parts of 28% ammonium hydroxide, 0.199 parts of anti-foam, 1.297 parts of anionic surfactant, 0.359 parts of non-ionic dispersant, 1.995 parts of ethylene glycol and 19.948 parts of "Kelsol" resin 3907-BG-74. Mix at low to moderate speeds at ambient temperatures until the mixture is uniform and a homogenous solution. To this agitating mixture is added 29.922 parts of an organic phosphate pigment, 9.974 parts of a zinc oxide pigment, 9.974 parts of a finely ground mica and 0.798 parts of a finely divided fungicide or mildiside. Disperse all of the components at high speed agitation long enough to make a dispersion that has a finesse of dispersion reading of 5-7 on a Hegman gauge. Due to the energy put into the system by the high speed agitation the temperature will probably rise to as much as 70° C. but should be controlled to assure that the temperature does not rise any more than a maximum of 70° C. The solids contact of this pigment dispersion is found to be about 66.2%.
The above referenced pigment dispersion is diluted with the following components using moderate agitation to produce a coating with good flexibility, solvent resistance and adhesion to cold rolled steel. 14.929 parts of the pigment dispersion B1346-1 was mixed with 17.627 parts of red oxide, 56.130 parts of acrylic latex, 5.051 parts of butyl cellesolve, 0.126 parts of anti-foam and 6.138 parts of UNEL XL-20 cross linking agent from Union Carbide, a corporation of Danbury, Conn. This paint is found to have a pH value of 7.8, a viscosity of 4,620 centapoises at 77° F. (determined using a Brookfield viscometer using spindle number 3 rotating at 10 rpm) and a calculated weigh solids of about 48.6%.
Cold rolled steel panels (O 2 -panels) are coated with the paint (using a conventional air spray gun for coatings) at a wet thickness of about 5 mils. The dry coating thickness is measured to be about 2 to 2.5 mils thickness. A part of the panels are air dried at ambient room temperatures and same dried at 200° F. for 5 minutes in a forced convection oven. The air dried panels after 16 hours are tested for methyl ethyl ketone (MEK) resistance by wetting a pad of clean cheese cloth with the MEK and with moderate pressure (about 5 pounds per square inch) rubbing it across the air dried coating and counting the number of double strokes (across the coating and back) required to expose the steel substrate. The following test results are obtained:
__________________________________________________________________________ MEKFilm Thickness Conditions UNEX XL-20 1/8" Resistance Tapein Mils Drying Cross Linked Mandrel Double Rubbs Adhesion__________________________________________________________________________2.1 2-2.5 Air Dry 16 Hrs. No Pass 5-12 100%2.2 2-2.5 Air Dry 16 Hrs. Yes Pass 52 100%2.3 2-2.5 200° F. 5 Min. No Pass 12-15 100%2.4 2-2.5 200° F. 5 Min. Yes Pass 300+ 100%__________________________________________________________________________
Example 2
(Reference: B1346--4, 5, & 7
A formulation is prepared using the same procedures and equipment as in Example I using 18.045 parts of deionized water, 1.113 parts of surfactant anionic, 0.361 parts 28% ammonium hydroxide, 18.045 parts of Kelsol 3907-BG-74 alkyd resin, 24.06 parts of molywhite 212 pigment, 6.015 parts of a zinc phosphate pigment, 3.008 parts of Mica, 12.030 parts of calcium carbonate, 6.015 parts of zinc oxide pigment, 0.301 parts of fungicide or mildewside, 3.008 parts of ethylene glycol, 0.120 parts of anti-foam and 7.880 parts of a carbon black dispersion, giving a calculated total solids of 67.34%. An aliquot of this concentrate is diluted to prepare a paint as follows: pigment dispersion 30.081 parts, thickening agent 14.476 parts, filming aid 3.909 parts, anti-foam agent 0.289 parts, modified acrylic polymer dispersion 43.529 parts and a drying agent 7.716 parts. Prepared samples on O 2 -panels as in Example I for testing are compared with the results with a similar coating that was cross-linked with a melamine type cross linking agent.
__________________________________________________________________________ Coating Corrosion Dry Film Cure Drier or MEK Salt FogNo. Thickness Conditions X-Linker Resistance Resistance__________________________________________________________________________1 2 mils 24 hr. ambient XL-20 52 --2 2 mils 72 hr. ambient XL-20 187 162 hrs. (5% rust)3 2 mils 180° F. 5 min. XL-20 300+ --4 2 mils 200° F. 5 min. XL-20 -- 260 hrs. (5% rust)5 2 mils 24 hrs. ambient melamine 23 --6 2 mils 180° F. 5 min. melamine 45 72 hrs. (5% rust)7 2 mils 72 hrs. ambient melamine 50 16 hrs. (50% rust)__________________________________________________________________________
Example 3
(Reference B1346--15)
A formulation is prepared using the same procedure and equipment as in example number I. 19.755 parts of a "Kelsol" resin (a Spencer Kellogg Division of Textroh Inc.), 1.534 parts of an amine, 25.566 parts of water, 25.566 parts of an acrylic copolymer dispersion, 23.725 parts of a lead containing pigment and 3.835 parts of a polycarbodiimide drier. This paint had a pH of 8.34, viscosity of 760 centepoises at 74° F. at 10 rpm using spindle no. 3 and a Brookfield viscometer model RVT, and a calculated total solids by weight of 54.45%.
Coatings prepared an O2-panels FM testing as in previous examples. Had to spray two coats to build a 2 mil dry film thickness.
______________________________________ 100% Coating MEK Relative 5% Curl Resis- Humidity Salt FogNo Conditions tance at 110° F. Resistance______________________________________1 Ambient Temp. 72 hrs. 36 2000 hrs. --2 Ambient Temp. 72 hrs. 10 -- -- Control Sample No. XL-203 Coating Without XL-20 15 -- -- Cured 5 min. at 200° F.4 Cured 5 min. at 200° F. 100 2000 hrs. 1700 hrs. (no rust)______________________________________
Example 4
(Reference B1346--16)
A formulation using the same procedure and equipment as in Example 1; 23.295 parts of an alkyd resin about 75% solids and produced by Spencer Kellogg Division of Textron, Inc. called "KELSOL" and having an acid number of about 40. 3.764 parts of triethylamine, 11.293 parts of an organic polyphosphate inhibiting pigment, 3.764 parts of a chromate containing pigment, 1.506 parts of carbon black, 41.861 parts of an acrylic copolymer dispersion and 14.516 parts of a poly carbodiimide drier. This produces a very thick smooth paste that dilutes readily with water to the viscosity needed for application. pH equals 8.7 and the calculated weight solids are 55.975%. Salt fog (5%) resistance=96 hours an O2 panels air dried at ambient temperatures. Panel is cured at 200° F. (5% NaCl) sort fog=1272 hours.
Example 5
(Reference B1346--19)
A formulation using the same equipment and procedures as in Example 1. This example is to be a comparison with other examples and uses conventional metal salt driers and no carbodiimide driers. 21.358 parts of Kelsol 3961 resin, 0.828 parts of HH4OH; 5.523 parts of a penn color black dispersion, 13.806 parts of a chromate pigment, 35.621 parts of an acrylic copolymer, 0.276 parts of anti-foam agent, 1.602 parts of a high boiling filming aid, 0.138 parts of a 12% active cobalt drier, 0.138 parts of a 6% zirconium drier, 13.806 parts of water and 6.903 parts of a medium boiling cosolvent. This produces a paint having a pigment to binder ratio of 1 to 2 and a calculated total solids by weight of 49.65%. Samples prepared for testing as in other examples an cold rolled steel (O2-pounds). All samples air dried at ambient temperatures seven (7) days and then cured 5 minutes at 200° F. in the oven. Samples put in 5% NaCl salt fog box and the 100% relative humidity cabinet at 110° F. Samples removed from salt fog cabinet after 96 hours exposure, coatings had blistered and rusted in 48 hours. Samples removed from the humidity cabinet after 1,104 hours exposure, no blistering or rusting evident on these panels.
Examples 6, 7 and 8
(Reference B1346--33A, B & C)
These are high solids systems that are formulated using a slow speed mixer that has high torque. These examples are to demonstrate and prove the reactivity of the polycarisodiimide driers in high solids alkyd, polyester systems and also the scope of the drying possibilities that have not before been possible with the alkyd coatings. Anyone skilled in the art of alkyd, polyester, acrylic or other polymers used for coatings containing carboxyl groups will readily recognize the many possibilities and advantages of the carbodiimide, polycarbodiimide and substituted carbodiimide driers or cross linking agents (6). A formulation containing 91.591 parts of a Cargil high solids alkyd number 5720, 0.814 parts of an alkynolamine, 0.680 parts of a cobalt salt drier, 0.769 parts of a Zirco drier, 2.661 parts of a calcium acid salt drier and 3.485 parts of a polycarbodiimide drier produced by Union Carbide Corporation under the name UNEL-XL20.
This gives a product that is 66.1% solids and a 3 mil film air dried to touch in 10 minutes. Pot life remains good after 7 months.
(7) A formulation containing 93.214 parts of Cargil resin number 5720, 0.829 parts of an alkanolamine, 0.692 parts of cobalt drier, 0.783 parts of Zirco drier, 2.708 parts of calcium drier and 1.775 parts of polycarbodiimide drier. This gives a system that is cobalt 67.3% weight solids the pot life or storage stability at ambient room temperature are good at 7 months. A 3 mil wet film cured to touch in 20 minutes at ambient room temperatures.
(8) A formulation containing 96.335 parts of Cargil resin number 5720 and 3.665 parts of a polycarbodiimide. This system is about 69.3% weight solids and jelled in 30 seconds. This film cured to touch in 60 seconds at ambient room temperatures.
Examples 9, 10 and 11
(Reference B1346--65 A, B and C)
These three examples demonstrate the advantages of using the polycarbodiimide driers in already commercial, water dilutable alkyd paint systems by the post addition of the polycarbodiimide driers. However, no commercial sales or public publications have been made to the inventors knowledge at the time of this patent memorandum accomplishment. These examples were prepared by taking a clear product similar to that produced according to Example 1 of co-pending U.S. Ser. No. 382,853 (a commercial product of Ashland Petroleum Company) and the corresponding black-pigmented product (a commercial product) and adding the polycarbodiimide at the proper levels to the coatings and recording the drying times and hardness levels of the coatings.
Example 9
Clear, (Batch No. 6E03332)
Films are prepared on O2-panels using a draw down bar with a 5 mil spacing.
______________________________________ PencilNo. Drying Conditions Tack to Touch Hardness______________________________________1 Ambient Room Temperatures 40 minutes tack 6B+ free2 Oven 245° F.-250° F. 4 minutes tack 4B free3 Oven 245° F.-250° F. 3 minutes tacky 6B+4 3 minutes at 250° F. and tack free F16 hours at ambienttemperature______________________________________
Example 10
Clear, Batch Number 6E03332
89.127 parts and polycarbodiimide 10.873 parts; test panels are prepared as in Example 9.
______________________________________ PencilNo. Drying Conditions Tack to Touch Hardness______________________________________1 Ambient Room Temperatures tack free 20 6B+ minutes2 oven at 245° F.-250° F. tack free 3 B minutes3 oven at 245° F.-250° F. three tack free 2Hminutes and 16 hours atambient temperature______________________________________
Example 11
Black, Batch Number 2E02790
100,000 parts as in Example 9.
______________________________________ PencilNo. Drying Conditions Tack to Touch Hardness______________________________________1 ambient room temperatures 50 minutes tack 6B+ free2 ambient room temperatures 16 hours tack free 5B3 oven at 245° F.-250° F. 3 minutes tack 5B free______________________________________
Examples 12, 13 and 14 continue the testing using the formulation of Example 1 pigmented with black and stanley red.
Example 12
Reference B1346-13 66D, E and F
Using the formulation of Example 1, pigmented with black, batch number 2E02790, 89.127 parts and 10.873 parts of polycarbodiimide; test panels are prepared as in Example 9.
______________________________________ PencilNo. Drying Conditions Tack to Touch Hardness______________________________________1 ambient room temperatures 20 minutes tack 6B free2 ambient room temperatures 16 hours tack free HB3 oven 245° F.-250° F. 3 minutes tack free B4 oven 345° F.-350° F. 1 minute tack free HB5 oven 345° F.-350° F. 2 minutes tack free 2H6 oven 345° F.-350° F. 10 minutes tack 3H free______________________________________
Example 13
Using the formulation of Example 1, pigmented with stanley red batch number 7-278C, 100.00 parts, test samples are prepared as in Example 9.
______________________________________ PencilNo. Drying Conditions Tack to Touch Hardness______________________________________1 ambient room temperatures 40 minutes tack 6B+ free2 oven 245° F.-250° F. 3 minutes tacky 6B+3 oven 245° F.-250° F. 5 minutes tack 5B free4 oven 245° F.-250° F. 3 minutes tack free Bplus 16 hours ambienttemperatures______________________________________
Example 15
Using the formulation of Example 1, pigmented with stanley red batch number 7-278C 89.127 parts and 10.873 parts polycarbodiimide, test samples are prepared as in Example 9.
______________________________________ PencilNo. Drying Conditions Tack to Touch Hardness______________________________________1 ambient room temperatures 15 minutes tack 4B2 oven 245° F.-250° F. 3 minutes tack free H3 oven 345° F.-350° F. 1 minute tack free 2H______________________________________
Examples 15-24
When additional formulations are made and tested according to the techniques of Example 1, formulations and test results are as set forth in Table I.
TABLE I__________________________________________________________________________ Ambient Test Results Percent of Thickness Air 270° F. Pencil HardnessExampleFormulation Total Wgt. Substrate Mils Wet Cure Cure ASTM__________________________________________________________________________ D3363-7415 Spencer Kellogg Alkyd #252-MA1-60 52.72 (CRS) 3 15 Min. -- 6B+ SoftDMEA 6.33 16 Hrs. -- FWater 31.64 -- 1 Min. 6B+Butyl Cellosolve 7.91 -- 2 Min. BCobolt Drier 0.79 -- 6 Min. HBActive 8 Driver 0.5916 SK Alkyd (95-110)* #252 MA160 42.15 CRS 3 12 Min. -- 6B+ SoftDMEA 6.32 16 Hrs. -- BWater 25.29 -- 1 Min. BButyl Cellosolve 6.32 -- 2 Min. BUNEL XL-20 (50%) 19.92 16 Hrs.+ 2 Min. H17 SK Alkyd (95-110)* #252 MA160 49.55 CRS 3 12 Min. -- 6B+ SoftDMEA 7.43 16 Hrs. -- BWater 29.73 -- 1 Min. BButyl Cellosolve 7.43 -- 2 Min. BUNEL XL-20 (50%) 5.85 16 Hrs.+ 2 Min. HB18 Cargill Alkyd XP-10511-222 (41.4)* 54.49 CRS 3 140 Min. -- 6B+ SoftDMEA 2.73 16 Hrs. -- 2BWater 33.07 -- 5 Min. 3BButyl Cellosolve 8.27 16 Hrs.+ 5 Min. 2BCobolt Drier 0.83Active 8 Driver 0.6219 Cargill Alkyd XP-10511-222 (41.4)* 49.44 CRS 3 37 Min. -- 6B+ SoftDMEA 3.38 2 Min. 4BWater 30.00 16 Hrs. 2 Min. 3BButyl Cellosolve 7.50UNEL XL-20 (50%) 9.6820 Cargill Alkyd XP-10511-222 (41.4)* 53.31 CRS 3 9 Hrs. -- 6B+ SoftDMEA 3.64 40 Min. 6B+ SoftWater 32.36 16 Hrs. 5BButyl Cellosolove 8.09UNEL XL-20 (50%) 2.6121 Cargill Alkyd XP-10511-221 (20.8)* 55.52 CRS 3 80 Min. -- 6B+ SoftDMEA 1.38 16 Hrs. -- FPropasol-P 41.64 -- 10 Min. 6B+ SoftCobolt Drier 0.83 20 Min. BActive 8 Drier 0.62 16 Hrs. F22 Cargill Alkyd XP-10511-221 (20.8)* 53.16 CRS 3 45 Min. -- 6B+ HardDMEA 1.79 16 Hrs. -- 3BPropasol-P 39.87 -- 10 Min. 6B HardUNEL XL-20 (50%) 5.1823 Aropol Polyester 8321 (31-37) 99.97 CRS 3 -- 5 Min. @ 260° F. B HardBenzoyl Peroxide 0.0324 Aropol Polyester 8321 (31-37) 82.07 CRS 3 -- 3 Min. @ 260° F. B HardBenzoyl Peroxide 0.02UNEL-XL20 17.91__________________________________________________________________________ *Acid Number CRS = Cold Rolled Steel
MODIFICATIONS
It will be understood by those skilled in the art that the invention is not to be restricted by the examples which merely illustrate the invention and that the invention is susceptible to a wide variety of modifications and variations without departing from the spirit thereof. For example, the formulations of the invention can be prepared as concentrates to which a substantial amount of water can be added in order to avoid shipping of water, particularly for international or other long distance shipment. The formulations may contain other useful ingredients such as biocides, anti-foam agents, pigments, dyes and leveling agents, well known to those skilled in coatings technology.
All references mentioned above and the references cited therein are hereby incorporated by reference.
Specific compositions, methods, or embodiments discussed are intended to be only illustrative of the invention disclosed by this Specification. Variation on these compositions, methods, or embodiments are readily apparent to a person of skill in the art based upon the teachings of this Specification and are therefore intended to be included as part of the inventions disclosed herein.
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New coating compositions having controllable drying time and capable of drying rapidly at ambient temperatures without substantial evolution of gaseous by-products caused by conventional driers such as melamines or urea formaldehyde comprising carbodiimides or homologies of carbodiimides together with organic carboxylates. These compositions are particularly useful in providing fast-drying long-oil alkyds which form coatings exhibiting excellent hardness, toughness and resistance to humidity and salt spray.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention is for an apparatus to stretch plastic dough having viscoelasticity, such as bread or confectionery dough, and more particularly for an apparatus to effectively stretch the dough by a simple and reliable mechanism.
2. Description of Prior Art
U.S. Pat. No. 3,973,895 teaches an apparatus to form dough pieces where a plurality of rollers are assembled into an oval circuit and is located above a plurality of conveyors.
Although dough fed between the rollers and the conveyors is smoothly stretched in the apparatus of this prior art, it requires a complex mechanism to transmit power to rotate the conveyors about their axes and along an endless roller path, and a large number of rollers are required.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide an apparatus by which the dough is effectively stretched without the use of a complex mechanism.
It is another object of this invention to provide such an apparatus that production costs are low and handling and maintenance is easier.
In accordance with the present invention, an apparatus for stretching dough is provided, which comprises a plurality of serial conveyors operable at different speeds, and a plurality of rollers above the conveyors, the rollers being freely rotatable about their axes and moving back and forth along the conveyance path of the conveyors, the lower portion of the rollers forming a straight portion spaced apart from and above the conveyors by a predetermined distance.
An apparatus of the present invention comprises a plurality of conveyors arranged in series and a plurality of rollers disposed above the conveyors. The conveyors are driven at different speeds, and preferably a downstream conveyor is driven at a speed higher than that of an upstream conveyor because of the effective stretching of the dough at a stage between the two conveyors. Each of the shafts of the rollers is connected to each slide member which is slidably mounted on a roller frame on each side of the apparatus. The roller frames are mounted on a frame on which the conveyors are also mounted.
Since each shaft is connected to a connecting arm which is connected to a crank arm, which crank arm is moved by a motor, the rollers can move back and forth together in unison. The speed of movement of the rollers is preferably substantially higher than that of any of the conveyors. The rollers can also rotate about the shafts by means of their frictional contact with the dough or by means of rolling friction from friction plates mounted to the roller frames, whereby the dough fed between the rollers and the conveyors is pressed, leveled, and rolled out into a less thick dough sheet.
Thus, according to the present invention, a simple but reliable stretching apparatus rolls out the dough with the same efficiency as that of a stretching apparatus having an endless roller mechanism requiring many rollers, gearings, sprockets, chains, and so forth.
In addition, changes in the distance between the rollers and the conveyors, and the angle of the straight portion of the rollers with the conveyors, can respond to various dough thicknesses and many kinds of dough with different rheological properties. As will be seen by the aformentioned explanation, whereas the apparatus according to the present invention is composed simply of a plurality of serially arranged conveyors and a plurality of rollers positioned above the conveyors, an excellent stretching effect can be achieved. Consequently, this apparatus is very applicable to industies treating various plastic and viscoelastic materials, in addition to food companies manufacturing dough and the like.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view of an embodiment of the present invention.
FIG. 2 is a plan view of the embodiment described in FIG. 1.
FIG. 3 is a fragmentary sectional view of a roller and a conveyor of the embodiment described in FIG. 1.
FIG. 4 diagrammatically illustrates an embodiment of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
An embodiment of the present invention will now be described with reference to the drawings. In FIG. 1, an upstream conveyor 1 and a downstream conveyor 2 are disposed in series on a frame 18. These conveyors are driven in a direction as shown by the arrows in the figure but are driven in the reverse direction if desired. The conveying speed of the downstream conveyor 2 is higher than that of the upstream conveyor 1. When these conveyors are driven reversely, the speed of conveyor 1 is higher than that of conveyor 2.
In FIGS. 1, 2, and 3, a plurality of rollers 3 are parallel. These rollers are on the same plane except for two rollers at the upstream and downstream ends, and the two rollers are located slightly above the plane, because, when larger mass of dough is stretched, it is easily fed between the roller and the conveyor, as shown in FIG. 4. Each roller is mounted on a shaft 4 about which it rotates. The shaft 4 extends beyond the roller at each end. Slide members 6 of a suitable shape, for instance, rectangular in cross-section, are fixed to each end of the shafts 4 and are adapted to be slidable within the recess of each of roller frames 7, 7, which are U-shaped in cross-section and mounted on the frame 18, on both sides of the rollers. The shafts 4 are fixedly connected to a pair of connecting arms 5, 5 in the vicinity of each end of the rollers 3. The connecting arm 5 is a plate horizontally disposed and with holes to receive the shafts 4. The connecting arms 5, 5 at both ends of the rollers are rotatably connected to one end of each of a pair of crank arms 9, 9. The other end of each of the crank arms 9, 9 is rotatalby connected by means of a pin 11 to a point near the circumference of one of a pair of discs 10, 10, which are mounted on both ends of a rotary shaft 12 supported by the frame of the apparatus. A sprocket 13 is mounted on the rotary shaft 12 and is connected to a sprocket 15 of a motor 14 with a chain. When the motor 14 rotates, the sprocket 15 then rotates and so causes the sprocket 13 to rotate. The rotation of the sprocket 13 causes the rotary shaft 12 and the discs 10, 10 to rotate. Since the pins 11, 11 are eccentrically connected to the discs 10, 10, the crank arms 9, 9 make a crank motion to cause a reciprocally linear motion of the connecting arms 5, 5.
The rollers 3 are adapted to freely rotate about the shafts 4. A pair of friction plates 8, 8 are mounted on the bottom of the frames 7, 7 to frictionally engage the rollers 3 as shown in FIG. 3. By the reciprocal motion of the roller frames 7, 7, the rollers 3 move back and forth and at the same time roll by means of rolling friction from the friction plates 8, 8, whereby dough 16, fed on the upstream conveyor 1, is initially leveled on the conveyor 1. The speed of the reciprocal motion of the connecting arms 5, 5 is preferably substantially higher than the conveying speed of any of the conveyors 1, 2, so that the reciprocal motion is repeated several times until the dough 16 is transferred onto the downstream conveyor 2. Since the conveying speed of the downstream conveyor 2 is higher than that of the upstream conveyor 1, an extension of the dough 16 can be smoothly carried out, resulting in dough of a desired thickness.
As described before, the dough can be fed from the other end of this apparatus if the conveying direction is reversed and the conveying speed of each of the conveyors is adjusted. Even if no friction plate is provided in this apparatus, the rollers 3 can still roll out the dough by means of the rolling friction, with the dough thereby achieving the object of the present invention. Although in the apparatus the roller frames 7, 7 and the conveyors 1 and 2 are described as being fixedly mounted on the frame 18, the addition of a height-adjusting mechanism to the roller frames or the conveyors can feed dough of various thicknesses onto the apparatus. The number of the rollers may be changed to enable the apparatus to more suitably stretch dough of different rheological features. Further, the roller frames 7, 7, and consequently, the rollers 3, are parallel with the conveying path, but the conveying path may be inclined relative to the rollers to easily receive the dough and to effectively stretch the dough. It will be seen from the above description that the apparatus of the present invention is simple in structure and easy to operate and still can attain the same result as that of the prior art apparatus.
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An apparatus for stretching plastic dough is provided. A plurality of conveyors arranged in series and a plurality of rollers disposed above the conveyors cooperatively act to stretch dough fed therebetween. The plurality of rollers are freely rotatable and the shafts thereof are fixed to connecting arms which can reciprocate above the conveyors to make the dough less thick.
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FIELD OF THE INVENTION
[0001] The present invention relates to a method for the assembly and cloning of polynucleotides comprising highly similar polynucleotidic modules, that is highly versatile, does not require intermediate amplification step and can be easily automated for high throughput production of customized polynucleotidic modules.
BACKGROUND OF THE INVENTION
[0002] Recent developments of methods for efficient gene targeting and site specific gene editing have unveiled exciting perspectives for gene therapies (Silva, Poirot et al. 2011). A key requirement of such methods is the ability to produce highly specific and active customized nuclease for unique genome target of interest. Since the past ten years, a lot of efforts have been made to develop customized nucleases with tailored DNA specificity (Carroll 2008; Silva, Poirot et al. 2011; Stoddard 2011; Urnov, Rebar et al. 2011). To date, the majority of customized nucleases used for genome editing are Meganucleases and Zinc finger nucleases. They have been successfully used in edition of numerous targets of interest (Silva, Poirot et al. 2011; Urnov, Rebar et al. 2011). Despite their great promise in the field of genome engineering, a more widespread adoption is still partly hampered by relatively long and/or costly engineering processes.
[0003] Engineering such molecule is not straightforward because of the strong context dependency affecting individual protein/base interaction patterns within the DNA binding interface of meganucleases (Grizot, Duclert et al.) and Zinc Finger Nucleases (Ramirez, Foley et al. 2008). Nevertheless, studies describing the making of tailored Zinc Finger proteins and Meganucleases with chosen specificities have been a major contribution to the field of protein engineering. In addition, the impact of these studies reaches far beyond the making of rare cutting endonucleases. Indeed, whereas Zinc Finger Nucleases result from the fusion of a Zinc Finger-based DNA binding domain with the catalytic domain of the bacterial FokI TypeIIS restriction enzyme (Kim, Cha et al. 1996; Smith, Berg et al. 1999; Smith, Bibikova et al. 2000), artificial Zinc Finger proteins have also been used in fusion with other effector domains: transcription activators or inhibitors have been tethered to Zinc Finger domains to activate or repress chosen genes (Choo, Sanchez-Garcia et al. 1994; Isalan, Klug et al. 2001; Pabo, Peisach et al. 2001), and fusions comprising recombinase (Gersbach, Gaj et al. 2010) or transposase domains (Feng, Bednarz et al. 2010) have also been described. With many meganucleases, and especially the meganucleases of the LAGLIDADG family (which have been the ones used in most genome engineering experiments), the catalytic core is embedded into the DNA binding domain (Stoddard 2005; Stoddard 2011). However, the catalytic activity can be inactivated with little impact on DNA binding (Chevalier, Sussman et al. 2004), and one can easily envision fusions between such catalytically inactive mutants and a new effector domain. Thus, developing faster processes to produce new DNA binding domains with chosen specificities (with a potential for automation and scale up) would benefit not only the potential users of rare cutting endonucleases, but also any application requiring to bring a chosen peptide next to a chosen DNA sequence in a living cell.
[0004] Transcription activator-like effectors (TALEs), a group of bacterial plant pathogen proteins have recently emerged as new engineerable scaffolds for the making of tailored DNA binding domains with chosen specificities (Boch, Scholze et al. 2009; Moscou and Bogdanove 2009; Boch and Bonas 2010; Christian, Cermak et al. 2010; Li, Huang et al. 2011; Li, Huang et al. 2011). TALE DNA binding domain is composed by a variable number of 33-35 aa repeat modules. These repeat modules are nearly identical to each other except for two variable amino acids located at positions 12 and 13 (Repeat Variable Di residues, RVD). The nature of residues 12 and 13 determines base preferences of individual repeat module. Moscou M. J and Bogdanove A. J and Boch et al. (Boch, Scholze et al. 2009; Moscou and Bogdanove 2009) described the preferential pairing between A, C, G, T and repeat modules harboring respectively NI, HD, NN, and NG at positions 12 and 13. This remarkable simple cipher, consisting in a one-repeat-to-one-base pair code, allowed for prediction of TAL effector binding site and more importantly for construction of custom TAL effector repeat domains that could be tailored to bind DNA sequence of interest. This unprecedented feature unmasked exciting perpectives to develop new molecular tools for targeted genome editing and required development of efficient assembly methods of TALE repeat modules. TALE-derived proteins have been used to specifically activate chosen genes (Morbitzer, Elsaesser et al. 2011; Zhang, Cong et al. 2011). In addition, TALE-based DNA binding domains can also be tethered to various effectors. TALENs (Transcription activator-like effector Nucleases) are formed by fusions of the cleavage domain of FokI and a TALE DNA binding domain (Christian, Cermak et al. 2010; Miller, Tan et al. 2010; Cermak, Doyle et al. 2011; Li, Huang et al. 2011; Li, Huang et al. 2011; Mahfouz, Li et al. 2011).
[0005] A major drawback for the large scale assembly of TALE DNA binding domains is that assembly of multiple highly similar repeats is challenging with classical molecular biology methods. In addition, chemical synthesis of such TALE DNA binding domain is prohibitive for large scale production. To tackle this issue, few different research groups have recently developed and reported assembly methods of TALE DNA binding domain (Miller, Tan et al. 2010; Cermak, Doyle et al. 2011; Geissler, Scholze et al. 2011; Li, Huang et al. 2011; Li, Huang et al. 2011; Morbitzer, Elsaesser et al. 2011; Weber, Engler et al. 2011; Zhang, Cong et al. 2011). Those methods all relied on the Golden gate cloning technology that is based on the ability of Type IIS restriction endonucleases to cleave outside of their recognition sequence and produce 4 bp 5′ overhang (Spear 2000; Engler, Kandzia et al. 2008). In these methods, TypeIIS recognition sites are placed at the 5′ and 3′ end of each DNA fragment in inverse orientation. This configuration allows for the seamless ligation of two DNA fragments that have compatible overhang sequences. In addition, as Type IIS restriction sites can be designed to have different overhang sequences, directional assembly of multiple DNA fragments is feasible. More importantly, as TypeIIS restriction sites are removed in the ligation process, restriction and ligation of multiple DNA fragments can be performed at the same time in a “one pot-one step reaction”, the hallmark of the Golden gate technology.
[0006] While these recently developed assembly methods are fast, inexpensive and clearly advantageous with respect to classical molecular biology techniques, their potential is limited when faced up with high throughput automated production of TALE DNA binding domains. Indeed, they all display different limitations. First, the “one pot-one step reaction” methods described so far are unable to efficiently assemble in one step, a functional DNA binding domains for TALE nuclease. Indeed, to assemble a TALE DNA binding domain, these methods requires mutiple pre-assemblies of TALE repeat subarrays. These TALE repeat subarrays are amplified either by PCR (Zhang, Cong et al. 2011) or by Ecoli transformation (Cermak, Doyle et al. 2011; Geissler, Scholze et al. 2011; Morbitzer, Elsaesser et al. 2011), then recovered and finally coupled together to form the functional TALE DNA binding domain. These amplification steps are prone to errors and/or hard to automate because they require numerous different steps such as plating, colony picking, PCR screening and DNA isolation. Second, the “one pot-one step reaction” leading to assembly of TALE repeats subarrays requires a large number of single repeat plasmid. Indeed, each of the four single TALE repeat (NI, HD, NN, NG and NK) has to be cloned into several flanking typeIIS cleavable sequences to allow for efficient directional assembly of multiple repeats at the same time. In addition, it also requires additional “receiver” plasmids for TALE repeat subarray subcloning, transformation and amplification. All together and depending on the method considered, a large number of plasmids have to be constructed to enable assembly of competent TALE DNA binding domains (Cermak, Doyle et al. 2011; Geissler, Scholze et al. 2011; Zhang, Cong et al. 2011). Third, the Golden Gate cloning plating efficiency (i.e the total amount of positive clones obtained after E. coli transformation and plating) decreases with increasing number of incorporated modules (Weber, Engler et al. 2011). Indeed, Weber & al reported that plating efficiency dramatically dropped from 30 000 to 150 positive colonies when the number of incorporated modules increased from 2 to 6 (Weber, Engler et al. 2011). This drawback hampers generation of high diversity libraries of TALE DNA binding domains.
[0007] Hence, to overcome the different drawbacks described above, we sought to develop a new method for assembly and cloning polynucleotides comprising highly similar polynucleotidic modules, such as TALE repeated modules. This assembly method is versatile, does not require intermediate amplification steps, and can be easily automated for high throughput production of customized polynucleotidic modules such as the repeated modules of TALE DNA binding domains. It consists in a sequential assembly of repeated modules on a solid phase supported by a 96 well plate format. In this method, a polynucleotide comprising the repeated module is linked to an organic moiety (biotin or digoxygenin) that binds specifically to the solid phase coated with streptavidin or digoxygenin-specific antibodies. Repeated modules are sequentially added via series of consecutive restriction and ligation steps using Type IIS restriction sites and enzymes. This new method displays several advantages with respect to the methods recently documented in the literature.
[0008] Anchoring a DNA fragment onto a solid phase allows for easy removal of excess reactants, byproducts and enzymes and thus theoretically increases the success rate of repeated modules recovery. This method doesn't require any intermediate amplification step such as E. coli transformation/DNA isolation (Cermak, Doyle et al. 2011; Geissler, Scholze et al. 2011; Morbitzer, Elsaesser et al. 2011) and PCR amplification of TALE repeated modules (Zhang, Cong et al. 2011) and it allows for assembly of flexible amounts of repeated modules. In addition, our method requires only one construction per repeat module and one “receiver plasmid”. Furthermore, this method can be used on a 96 well plate format and thus allows for simultaneous assembly of a large number of repeated modules. This feature makes it easy to automate with a 96 head pipetting robot.
[0009] Finally, this method has high success rates of products recovery and plating efficiency. The large number of positive colonies obtained could enable generation of high diversity libraries of polynucleotides repeated modules such as TALE DNA binding domains.
BRIEF SUMMARY OF THE INVENTION
[0010] The present invention relates to a method for the assembly and cloning of polynucleotides comprising highly similar polynucleotidic modules, that is highly versatile, does not require intermediate amplification step and can be easily automated for high throughput production of customized polynucleotides comprising an array of multiple polynucleotidic modules. The method of the present invention comprises a sequential assembly of polynucleotidic modules on a solid phase. The method of the present invention is particularly well-suited for assembly of Transcription Activator-Like Effector (TALE) DNA binding repeat modules. The method of the present invention allows to produce libraries of polynucleotides comprising highly similar polynucleotidic modules such as TALE DNA binding domains.
BRIEF DESCRIPTION OF THE FIGURES
[0011] In addition to the preceding features, the invention further comprises other features that will emerge from the description and appended drawings that follow. A more complete appreciation of the invention and many of the attendant advantages thereof will be readily obtained as the same becomes better understood by reference to the following figures in conjunction with the detailed description below.
[0012] FIG. 1 : Repeat polynucleotidic modules cloned into pAPG10 plasmid.
[0013] Binding sites BbvI, SfaNI and SfiI are indicated in red, cyan and green respectively. Overhangs generated by the three enzymes are displayed in dashed lines with the same color code. FIG. 1A : mono repeat module. FIG. 1B : terminal half repeat module.
[0014] FIG. 2 : Method to assemble two mono repeat polynucleotidic modules.
[0015] FIGS. 2A and 2B : extraction of polynucleotidic modules 1 and 2 from pAPG10 and digestion by SfaNI and BbvI. FIG. 2C : ligation of polynucleotidic modules 1 and 2 and sublconing into pAPG10.
[0016] FIG. 3 : Sequential assembly of 15.5 TALE repeats polynucleotidic modules using a sequential parallel process in solution and building blocks comprising di repeat polynucleotidic modules.
[0017] For the sake of clarity, TALE repeat polynucleotidic modules used in the process are displayed with overhangs that are free and ready to react. FIG. 3A : steps a-c of the process; FIG. 3B : steps e-g of the process; FIG. 3C : steps h-i of the process; FIG. 3D : steps k-l of the process.
[0018] FIG. 4 : Assembly of CAPT1.3 and CAPT1.4 TALE repeats polynucleotide modules in solution.
[0019] CAPT1.3 (SEQ ID NO: 1) and CAPT1.4 (SEQ ID NO: 2) targeted sequences and DNA spacer are displayed in green, cyan and red respectively. FIG. 4A : Assembly workflow; FIG. 4B : Colony PCR screen results of CAPT1.3 7.5 TALE repeats left polynucleotide assembly and 8 TALE repeats right polynucleotide assembly (steps a to g); FIG. 4C : Colony PCR screen results of CAPT1.3 15.5 TALE repeats polynucleotide assembly (steps k to 1). * Correspond to clones containing 8 or 7.5 TALE repeats polynucleotides.
[0020] FIG. 5 : Preparation of building blocks by PCR and BbvI or SfaNI Digestion.
[0021] Solid phase synthesis of TALE repeat stretch using sequential parallel process. For the sake of clarity, repeat polynucleotides modules used in the process are displayed with overhangs that are free and ready to react. FIG. 5A : steps a-b of the process; FIG. 5B : step c of the process; FIG. 5C : steps d-e of the process; FIG. 5D : steps h-i of the process.
[0022] FIG. 6 : Solid phase assembly of SADE2.3 TALE repeats polynucleotides using a sequential parallel process and building blocks comprising di repeat polynucleotidic modules.
[0023] SADE2.3 target sequences (SEQ ID NO: 3) and DNA spacer are displayed in green and red respectively. The first biotinylated building blocks of TALE repeats left and right are displayed as “RVD_bx-biot”. FIG. 6A : Assembly workflow; FIG. 6B , colony PCR screen results of SADE2.3 15.5 TALE repeats polynucleotide assembly performed with streptavidin coated magnetic beads as solid phase. * Correspond to clones containing 15.5 TALE repeats
[0024] FIG. 7 : Solid phase assembly of SADE2.3 TALE repeats polynucleotides using a sequential parallel process.
[0025] SADE2.3 target sequences (SEQ ID NO: 3) and DNA spacer are displayed in green and red respectively. The first biotinylated building block is marked as “RVD_b3-biot”. FIG. 7A , Assembly workflow; FIG. 7B , colony PCR screen results of SADE2.3 15.5 TALE repeats polynucleotide assembly performed with streptavidin coated magnetic beads as solid phase and building blocks comprising di repeats modules; FIG. 7C , colony PCR screen results of SADE2.3 15.5 TALE repeats polynucleotide assembly performed with streptavidin coated well as solid phase and building blocks comprising di repeats modules. * Correspond to clones containing 15.5 TALE repeats.
[0026] FIG. 8 : Solid phase assembly of AvrBS3 TALE repeats polynucleotides using a sequential parallel process.
[0027] AvrBS3 target sequence and DNA spacer are displayed in green and red respectively. The first biotinylated building block is displayed as “RVD_b2-biot”. FIG. 8A , Assembly workflow; FIG. 8B , colony PCR screen results of AvrBS3 17 TALE repeats polynucleotide assembly performed with streptavidin coated well as solid phase, biotinylated first building block comprising di repeats module and additional building blocks comprising tri repeats modules.* Correspond to clones containing 17 TALE repeats.
[0028] FIG. 9 : Method for improving TALE repeat polynucleotidic modules assembly success rate.
[0029] FIG. 10 : Solid phase assembly of TALE repeat polynucleotides using the reverse elongation method.
[0030] Workflow of steps 1-16 of the process.
[0031] FIG. 11 : Assembly of 14.5 TALE repeats polynucleotide modules with the reverse elongation method.
[0032] Colony PCR screens results of a 14.5 TALE repeats polynucleotide assembly. * Correspond to clones containing 14.5 repeats polynucleotides.
[0033] FIG. 12 : Solid phase assembly of TALE repeat polynucleotides using the reverse elongation method combined with the sequential linear synthesis.
[0034] Workflow of steps 1-16 of the reverse elongation process and steps 17-19 of sequential linear synthesis.
[0035] The above objects highlight certain aspects of the invention. Additional objects, aspects and embodiments of the invention are found in the following detailed description of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0036] Unless specifically defined herein, all technical and scientific terms used have the same meaning as commonly understood by a skilled artisan in the fields of gene therapy, biochemistry, genetics, and molecular biology.
[0037] All methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, with suitable methods and materials being described herein. All publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety. In case of conflict, the present specification, including definitions, will prevail. Further, the materials, methods, and examples are illustrative only and are not intended to be limiting, unless otherwise specified.
[0038] The practice of the present invention will employ, unless otherwise indicated, conventional techniques of cell biology, cell culture, molecular biology, transgenic biology, microbiology, recombinant DNA, and immunology, which are within the skill of the art. Such techniques are explained fully in the literature. See, for example, Current Protocols in Molecular Biology (Frederick M. AUSUBEL, 2000, Wiley and son Inc, Library of Congress, USA); Molecular Cloning: A Laboratory Manual, Third Edition, (Sambrook et al, 2001, Cold Spring Harbor, N.Y.: Cold Spring Harbor Laboratory Press); Oligonucleotide Synthesis (M. J. Gait ed., 1984); Mullis et al. U.S. Pat. No. 4,683,195; Nucleic Acid Hybridization (B. D. Harries & S. J. Higgins eds. 1984); Transcription And Translation (B. D. Hames & S. J. Higgins eds. 1984); Culture Of Animal Cells (R. I. Freshney, Alan R. Liss, Inc., 1987); Immobilized Cells And Enzymes (IRL Press, 1986); B. Perbal, A Practical Guide To Molecular Cloning (1984); the series, Methods In ENZYMOLOGY (J. Abelson and M. Simon, eds.-in-chief, Academic Press, Inc., New York), specifically, Vols. 154 and 155 (Wu et al. eds.) and Vol. 185, “Gene Expression Technology” (D. Goeddel, ed.); Gene Transfer Vectors For Mammalian Cells (J. H. Miller and M. P. Calos eds., 1987, Cold Spring Harbor Laboratory); Immunochemical Methods In Cell And Molecular Biology (Mayer and Walker, eds., Academic Press, London, 1987); Handbook Of Experimental Immunology, Volumes I-IV (D. M. Weir and C. C. Blackwell, eds., 1986); and Manipulating the Mouse Embryo, (Cold Spring Harbor Laboratory Press, Cold Spring Harbor, N.Y., 1986) and updated versions.
[0039] According to a first aspect of the present invention is a method of generating and assembling polynucleotides comprising arrays of at least two highly similar polynucleotidic modules comprising the steps of:
a) generating “n” polynucleotidic building blocks, with n≧1, each polynucleotidic building block comprising at least:
one polynucleotidic module; a single cleavage site for a first restriction enzyme A, placed on one side of the polynucleotidic module; a single cleavage site for a second restriction enzyme B; placed on the other side of the polynucleotidic module; wherein A and B can produce compatible cohesive ends; wherein cleavage of said polynucleotidic building blocks with restriction enzyme A results in a polynucleotide comprising a polynucleotidic module flanked on one side by a cohesive ends that can be re-ligated with a polynucleotide building block cleaved by restriction enzyme B without at least restoring a sequence cleavable by restriction enzyme B; wherein cleavage of said polynucleotidic building blocks with restriction enzyme B results in a polynucleotide comprising a polynucleotidic module flanked on one side by a cohesive ends that can be re-ligated with a polynucleotide building block cleaved by restriction enzyme A;
b) generating at least one polynucleotidic building block comprising a single cleavage site for a restriction enzyme A′, wherein A′ can generate cohesive ends compatible with the cohesive ends produced by B; c) generating at least one polynucleotide linked to a solid phase comprising:
one polynucleotidic module; one end linked to a solid phase; a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce at least a sequence cleavable by restriction enzyme B;
wherein said polynucleotide comprises no sequence cleavable by restriction enzyme B; d) cutting at least one polynucleotidic building block described in a) with restriction enzyme A; e) ligating the resulting polynucleotidic module with the free end of the polynucleotide immobilized on the solid phase, thereby producing a new immobilized polynucleotide; f) cutting the resulting new immobilized polynucleotide with restriction enzyme B, thus producing a new immobilized polynucleotide having a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A; g) repeating steps d-f n times, thus producing an immobilized polynucleotide having an array of n+1 polynucleotidic modules; h) cutting the polynucleotidic building block described in b) with restriction enzyme “A”; i) ligating the resulting polynucleotidic module with the free end of the polynucleotide immobilized on the solid phase, thereby producing a new immobilized polynucleotide comprising an array of polynucleotidic modules.
[0059] In a preferred embodiment, A and A′ are identical.
[0060] In another embodiment, at least one said polynucleotidic building block comprise a pre-assembly of more than one polynucleotidic module. In another embodiment, said polynucleotidic building blocks of the present invention comprise a pre-assembly of more than one polynucleotidic module. As non-limiting examples, said polynucleotidic building blocks of the present invention comprise a pre-assembly of 2, 3, 4, 5, 6, 7, 8, 9 or 10 polynucleotide modules. As other non-limiting examples, said polynucleotidic building blocks of the present invention comprise a pre-assembly of more than 10 polynucleotide modules, i.e., 11, 12, 13, 14, 15, 20, 30, 40, 50 or 100. In another embodiment more than 100 polynucleotides are pre-assembled in said building block according to the present invention.
[0061] In another embodiment, said polynucleotidic building blocks of the present invention can be partially or entirely generated by oligonucleotide synthesis from digital nucleic sequences of said polynucleotidic building blocks and subsequent annealing of the resultant polynucleotidic intermediate; said oligonucleotides being designed and synthesize to produce polynucleotidic building blocks with compatible cohesive ends with or without enzymatic reactions. In another embodiment, some of the building blocks used for the generation of polynucleotides comprising an array of polynucleotidic modules according to the present invention can be generated by oligonucleotide synthesis from digital nucleic sequences, said oligonucleotides being designed and synthesize to produce polynucleotidic building blocks with compatible cohesive ends with or without enzymatic reactions.
[0062] In another embodiment, said single cleavage sites respectively for restriction enzymes A and B are two different cleavage sites cleavable by restriction enzymes which produce compatible cohesive overhang ends and wherein said compatible cohesive overhangs remove respective recognition sites for said restriction enzymes A and B upon ligation. In other words, restriction enzymes A and B according to the present invention produce at their respective single cleavage site compatible overhang cohesive ends without restoring a sequence cleavable by restriction enzymes A and B after ligation. In another embodiment, said restriction enzymes A and B belong to subtypes of class II restriction enzymes such as subtypes A, B, C, H and S as listed for example at http://_rebase.neb.com. In another embodiment, said restriction enzymes A and B of the present invention belong to typeIIS restriction enzymes. In a preferred embodiment said restriction enzymes A and B of the present invention are BbvI and SfaNI.
[0063] In another embodiment, said single cleavage sites respectively for restriction enzymes A and B can be cleavage sites for other enzymes such as nick-creating enzymes (nickases as non-limiting examples) under appropriate use to generate compatible overhang cohesive ends.
[0064] In another embodiment, said polynucleotide of c) is the first polynucleotide (considering a 5′-3′ reading) comprising a polynucleotide module of the final polynucleotide comprising an array of polynucleotidic modules.
[0065] In another embodiment, said first polynucleotide of c) comprises a fragment of building block according to a).
[0066] In another embodiment, said polynucleotide of c) is the last polynucleotide (considering a 5′-3′ reading) comprising a polynucleotide module of the final polynucleotide comprising an array of polynucleotidic modules.
[0067] In another embodiment, said last polynucleotide of c) comprises:
A polynucleotide sequence not highly similar to a polynucleotide module according to a); A fragment of building block according to a).
[0070] In another embodiment, said first polypeptide of c) has been generated by:
c1) generating one polynucleotide linked to a solid phase comprising:
a polynucleotide sequence not highly similar to a polynucleotide module according to a); wherein said polynucleotide sequence does not comprise a cleavage site for restriction enzyme B; one end linked to a solid phase; a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce a sequence cleavable by restriction enzyme B;
c2) cutting a polynucleotidic building block described in a) with restriction enzyme A; c3) ligating the resulting polynucleotidic module with the free end of the polynucleotide immobilized on the solid phase; c4) cutting the resulting new immobilized polynucleotide with restriction enzyme B, thus producing a new immobilized polynucleotide comprising:
a polynucleotide sequence not highly similar to a polynucleotide module according to a); one polynucleotidic module; one end linked to a solid phase; a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce a sequence cleavable by restriction enzyme B;
[0082] In another embodiment, the present invention is a method of generating and assembling polynucleotides comprising arrays of at least two highly similar polynucleotidic modules comprising the steps of:
a) generating “n” polynucleotidic building blocks, with n≧1, each polynucleotidic building block comprising at least:
one polynucleotidic module; a single cleavage site for a first restriction enzyme A, placed on one side of the polynucleotidic module; a single cleavage site for a second restriction enzyme B; placed on the other side of the polynucleotidic module; wherein A and B can produce compatible cohesive ends; wherein cleavage of said polynucleotidic building blocks with restriction enzyme A results in a polynucleotide comprising a polynucleotidic module flanked on one side by a cohesive ends that can be re-ligated with a polynucleotide building block cleaved by restriction enzyme B; wherein cleavage of said polynucleotidic building blocks with restriction enzyme B results in a polynucleotide comprising a polynucleotidic module flanked on one side by a cohesive ends that can be re-ligated with a polynucleotide building block cleaved by restriction enzyme A, without restoring a sequence cleavable by restriction enzyme A;
b) generating at least one polynucleotidic building block comprising a single cleavage site for a restriction enzyme A′, generating cohesive ends compatible with the cohesive ends produced by A; c) generating at least one polynucleotide linked to a solid phase comprising:
one polynucleotidic module; one end linked to a solid phase; a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme B, and which ligation with a polynucleotidic building block cleaved by restriction enzyme B will not produce a sequence cleavable by restriction enzyme A;
wherein said polynucleotide comprises no sequence cleavable by restriction enzyme A; d) cutting a polynucleotidic building block described in a) with restriction enzyme B; e) ligating the resulting polynucleotidic module with the free end of the polynucleotide immobilized on the solid phase, thereby producing a new immobilized polynucleotide; f) cutting the resulting new immobilized polynucleotide with restriction enzyme A, thus producing a new immobilized polynucleotide having a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme B; g) repeating steps d-f n times, thus producing an immobilized polynucleotide having an array of n+1 polynucleotidic modules; h) cutting the polynucleotidic building block described in b) with restriction enzyme A′; i) ligating the resulting polynucleotidic module with the free end of the polynucleotide immobilized on the solid phase, thereby producing a new immobilized polynucleotide comprising an array of polynucleotidic modules.
[0102] In a preferred embodiment, A and B are identical.
[0103] In another embodiment, said polynucleotide sequence not highly similar to a polynucleotide module according to a) is linked to said solid phase. In another embodiment, said polynucleotide sequence not highly similar to a polynucleotide module according to a) encodes a N-terminal polypeptidic sequence of a TALE. In another embodiment, said polynucleotide sequence not highly similar to a polynucleotide module according to a) encodes a C-terminal polypeptidic sequence of a TALE. In another embodiment, said polynucleotide sequence not highly similar to a polynucleotide module according to a) encodes a C-terminal polypeptidic sequence of a TALE and a half Transcription Activator-like Effector (TALE) DNA binding repeat module. In another embodiment, said polynucleotide sequence not highly similar to a polynucleotide module according to a) encodes one protein domain able to process a nucleic acid target sequence adjacent to the nucleic acid sequence bound by a TALE DNA binding domain, thus producing a chimeric protein according to the method of the present invention comprising a set of repeated modules with RVDs to bind a nucleic acid sequence and one protein domain to process a nucleic acid target sequence adjacent to said bound nucleic acid sequence.
[0104] In another embodiment, said polynucleotidic building blocks according to the present invention can encode a polynucleotidic module that is not highly similar to the other polynucleotidic modules assembled according to the method of the present invention to produce polynucleotides comprising an array of polynucleotidic modules. As non-limiting example, said polynucleotidic building blocks according to the present invention can encode a protein domain able to process a nucleic acid target sequence adjacent to the nucleic acid sequence bound by the other polynucleotidic modules of the array. Position of said not highly similar module can be anywhere in the array. As a non-limiting example a polynucleotide comprising an array of polynucleotidic modules according to the present invention can comprise a succession of: 7,5 highly similar TALE repeat polynucleotidic modules—a not highly similar polynucleotidic module encoding a protein domain—7,5 highly similar TALE repeat polynucleotidic modules. In another embodiment, said polynucleotide comprising an array of polynucleotidic modules according to the present invention can comprise more than one not highly similar polynucleotidic module.
[0105] In another embodiment, the end of said polynucleotide of c) linked to a solid phase comprises a single cleavage site for a restriction enzyme C, wherein said cleavage of said site with restriction enzyme C allows to unlink said polynucleotide from the solid phase. In another embodiment of this aspect of the invention, said restriction enzyme C is SfiI. In another embodiment, said single cleavage site for a restriction enzyme C is cleavable by said restriction enzyme A or said restriction enzyme B and said final polynucleotide comprising an array of polynucleotidic modules comprises no sequence cleavable by restriction enzymes A or B.
[0106] In another embodiment, said method of the present invention further comprises the step of unlinking said final polynucleotide of step i) comprising an array of polynucleotidic modules, by unlinking it with in non enzymatic step such as chemical or ionic treatments well-known in the art.
[0107] In another embodiment, said method of the present invention further comprises the step of unlinking said final polynucleotide of step i) comprising an array of polynucleotidic modules, by cutting it with a restriction enzyme. In another embodiment, said restriction enzyme is a restriction enzyme C different than restriction enzymes A and B. In another embodiment, said restriction enzyme is A or B.
[0108] In another embodiment, each of said polynucleotidic modules to assemble according to the present invention encodes a Transcription Activator-like Effector (TALE) DNA binding repeat module. Said Transcription Activator-like Effector (TALE) DNA binding repeat module usually comprises between 8 and 30 repeated modules (or repeat modules), more frequently between 8 and 20 repeat modules, again more frequently 15 repeat modules. The assembly of said repeated modules produce a TALE binding domain. Said repeat modules usually encode for 30 to 42 amino acids, more preferably 33-35 amino acids wherein two critical amino acids of each repeat module located at positions 12 and 13 (Repeat Variable Diresidues, RVD), mediate the recognition of one nucleotide of the nucleic acid target sequence targeted by the entire Transcription Activator-like Effector (TALE) DNA binding domain; said polynucleotidic modules according to the present invention can encode for TALE repeat modules comprising equivalent two critical amino acids located at positions other than 12 and 13 specialy in repeat modules taller than 33-35 amino acids long. In another embodiment, said polynucleotidic repeat modules of the present invention can encode for repeat modules-like domains or RVDs-like domains. RVDs-like domains have a sequence different from naturally occurring polynucleotidic repeat modules comprising RVDs (RVDs domains) but have a similar function and/or global structure. As non-limiting examples, said RVDs-like domains are protein domains selected from the group consisting of Puf RNA binding protein or Ankyrin super-family. Non-limiting examples of such proteins from which RVDs-like domain can be derived are given by SEQ ID NO: 4 and SEQ ID NO: 5 respectively corresponding to proteins fem-3 and aRep. Depending on the structural context and binding constraints, said polynucleotidic modules to assemble according to the present invention encodes a Transcription Activator-like Effector (TALE) DNA binding domain that comprises a mix of naturally occurring RVDs structures and RVDs-like domains. In another embodiment, said polynucleotidic TALE repeat modules to assemble according to the present invention encodes a totally artificial Transcription Activator-like Effector (TALE) DNA binding domain i.e., without any repeated domains derived from naturally occurring TAL effectors.
[0109] In another embodiment, said polynucleotidic building block of b) encodes a half repeat module of a Transcription Activator-like Effector (TALE) DNA binding repeat module. Said half repeat module is equivalent to the truncated repeat module usually made of 20 amino acids that is located at the C-terminus of said Transcription Activator-like Effector (TALE) DNA binding repeat module. In this case, said Transcription Activator-like Effector (TALE) DNA binding repeat module comprises between 8.5 and 30.5 repeat modules, “0.5” referring to previously mentioned half repeat module (or terminal repeat module, or half-repeat). More frequently, said Transcription Activator-like Effector (TALE) DNA binding repeat module comprises between 8.5 and 20.5 repeat modules, again more frequently, 15.5 repeat modules.
[0110] In another embodiment, said polynucleotidic building block of b) encodes a half TALE repeat module and one TALE mono repeat module (i.e. one and half TALE repeat module). In another embodiment, said polynucleotidic building block of b) encodes a half Transcription Activator-like Effector (TALE) DNA binding repeat module and a C-terminal fragment of a TALE. In another embodiment, said building block of b) encodes a N-terminal fragment of a TALE.
[0111] In another embodiment, said polynucleotidic modules to assemble share at least 85% similarity. In another embodiment, said polynucleotidic modules to assemble share 86, 87, 88, 89 or 90% similarity. In another embodiment, said polynucleotidic modules to assemble share 91, 92, 93, 94, 95, 96, 97, 98, 99 or 100% similarity.
[0112] BLASTP may also be used to identify an amino acid sequence having at least 80%, 85%, 87.5%, 90%, 92.5%, 95%, 97.5%, 98%, 99% sequence similarity to a reference amino acid sequence using a similarity matrix such as BLOSUM45, BLOSUM62 or BLOSUM80. Unless otherwise indicated a similarity score will be based on use of BLOSUM62. When BLASTP is used, the percent similarity is based on the BLASTP positives score and the percent sequence identity is based on the BLASTP identities score. BLASTP “Identities” shows the number and fraction of total residues in the high scoring sequence pairs which are identical; and BLASTP “Positives” shows the number and fraction of residues for which the alignment scores have positive values and which are similar to each other. Amino acid sequences having these degrees of identity or similarity or any intermediate degree of identity of similarity to the amino acid sequences disclosed herein are contemplated and encompassed by this disclosure.
[0113] As previously mentioned, said polynucleotidic modules to assemble according to the present invention can encode Transcription Activator-like Effector (TALE) DNA binding repeat modules. The assembly of such polynucleotidic modules produces a TALE binding domain. Said Transcription Activator-like Effector (TALE) DNA binding domain usually comprises between 8 and 30 repeated modules (or repeat modules, or TALE repeat modules), more frequently between 8 and 20 repeat modules, again more frequently 15 repeat modules. Said repeat modules usually encode for 30 to 42 amino acids, more preferably 33-35 wherein two critical amino acids located at positions 12 and 13 (Repeat Variable Diresidues, RVD) mediate the recognition of one nucleotide of the nucleic acid target sequence targeted by the entire Transcription Activator-like Effector (TALE) DNA binding domain. Preferably, RVDs associated with recognition of the different nucleotides are HD for recognizing C, NG for recognizing T, NI for recognizing A, NN for recognizing G or A, NS for recognizing A, C, G or T, HG for recognizing T, IG for recognizing T, NK for recognizing G, HA for recognizing C, ND for recognizing C, HI for recognizing C, HN for recognizing G, NA for recognizing G, SN for recognizing G or A and YG for recognizing T. More preferably, RVDs associated with recognition of the nucleotides C, T, A, G/A and G respectively are selected from the group consisting of NN or NK for recognizing G, HD for recognizing C, NG for recognizing T and NI for recognizing A. In another embodiment, RVDs associated with recognition of the nucleotide C are selected from the group consisting of N* and RVDs associated with recognition of the nucleotide T are selected from the group consisting of N* and H*, where * denotes a gap in the repeat sequence that corresponds to a lack of amino acid residue at the second position of the RVDs. In another embodiment, critical amino acids 12 and 13 can be mutated towards other amino acid residues in order to modulate their specificity towards nucleotides A, T, C and G and in particular to enhance this specificity. By other amino acid residues is intended any of the twenty natural amino acid residues or unnatural amino acids derivatives.
[0114] In another aspect of the present invention is a method wherein said “n” polynucleotidic building blocks are part of a collection encoding polypeptidic repeated modules or polypeptidic repeat modules with Repeat Variable Dipeptide regions (RVDs) comprising a pair of amino acids responsible for recognizing one nucleotide selected from the group consisting of HD for recognizing C, NG for recognizing T, NI for recognizing A, NN for recognizing G or A, NS for recognizing A, C, G or T, HG for recognizing T, IG for recognizing T, NK for recognizing G, HA for recognizing C, ND for recognizing C, HI for recognizing C, HN for recognizing G, NA for recognizing G, SN for recognizing G or A and YG for recognizing T. In a preferred embodiment of this aspect of the invention, is a method wherein said “n” polynucleotidic building blocks are part of a collection encoding polypeptidic repeated modules with Repeat Variable Dipeptide regions (RVDs) comprising a pair of amino acids responsible for recognizing one nucleotide selected from the group consisting of HD for recognizing C, NG for recognizing T, NI for recognizing A, NN and NK for recognizing G.
[0115] In another embodiment is a method wherein said “n” polynucleotidic building blocks are part of a collection encoding two polypeptidic repeated modules with Repeat Variable Dipeptide regions (RVDs) for recognizing two nucleotides via two pairs of amino acids (TALE di repeat modules or di repeat modules) selected from the group listed in table 2 of example one below as non-limiting example.
[0116] In another embodiment is a method wherein said “n” polynucleotidic building blocks are part of a collection encoding three polypeptidic repeated modules with Repeat Variable Dipeptide regions (RVDs) for recognizing three nucleotides via three pairs of amino acids (TALE tri repeat modules or tri repeat modules) selected from the group listed in table 3 of example one as non-limiting example.
[0117] In another embodiment is a method wherein said “n” polynucleotidic building blocks are part of a library encoding “n” polypeptidic repeated modules with Repeat Variable Dipeptide regions (RVDs) for recognizing “n” nucleotides via “n” pairs of amino acids (TALE “n” repeat modules or “n” repeat modules). In another embodiment, “n” is comprised between 1 and 8. In another embodiment, “n” is 1, 2, 3, 4, 5, 6, 7 or 8.
[0118] In another embodiment, said polynucleotidic building block brought in previously described steps d) to g) of the method of the present invention is a unique molecular species comprising a precise sequence. In another embodiment, several polynucleotidic building blocks are brought in previously described steps d) to g) of the method of the present invention comprising each a precise sequence. In another embodiment, a library of polynucleotidic building blocks are brought in previously described steps d) to g) of the method of the present invention comprising a library of polynucleotidic modules. In another embodiment said library can be a random mutagenized library of polynucleotidic modules. In another embodiment, a library of polynucleotidic building blocks are used in previously described steps d) to g) of the method of the present invention comprising a library of polynucleotidic modules and encoding a library of TALE repeat polynucleotidic modules. Mutagenesis can concern the entire polynucleotidic module sequence. In another embodiment said library can be a random mutagenized library of TALE repeat polynucleotidic modules. Mutagenesis of said TALE repeat polynucleotidic modules library can focused on critical amino acids such as amino acids located at positions 12 and 13 as non-limiting examples. Mutagenesis of said TALE repeat polynucleotidic modules library can focused on other critical amino acids of said TALE repeat polynucleotidic modules. Mutagenesis of said TALE repeat polynucleotidic modules library may concern the entire TALE repeat module sequence. Said libraries of polynucleotidic modules constituting libraries of polynucleotidic building blocks can be used according to the method of the present invention to introduce diversity into polynucleotides comprising an array of polynucleotidic modules. As non-limiting example, the method according to the present invention is particularly well-suited to introduce diversity into TALE repeat polynucleotidic modules in order to produce high-diversity libraries of TALE DNA binding domains.
[0119] According to another aspect of the present invention is a method of generating and assembling polynucleotides comprising arrays of at least two highly similar polynucleotidic modules comprising the steps of:
a) generating at least one polynucleotidic building block comprising at least:
one polynucleotidic module; a single cleavage site for a first restriction enzyme A, placed on one side of the polynucleotidic module; a single cleavage site for a second restriction enzyme B, placed on the other side of the polynucleotidic module; wherein A and B can produce compatible cohesive ends; wherein cleavage of said polynucleotidic building blocks with restriction enzyme A results in a polynucleotide comprising a polynucleotidic module flanked on one side by a cohesive end that can be re-ligated with a polynucleotide building block cleaved by restriction enzyme B without restoring a sequence cleavable by restriction enzyme A and/or B; wherein cleavage of said polynucleotidic building blocks with restriction enzyme B results in a polynucleotide comprising a polynucleotidic module flanked on one side by a cohesive end that can be re-ligated with a polynucleotide building block cleaved by restriction enzyme A without restoring a sequence cleavable by restriction enzyme A and/or B;
b) generating “n” polynucleotides linked to a solid phase comprising at least:
one polynucleotidic module; one end linked to a solid phase; a single cleavage site for a first restriction enzyme A, placed on the side of the polynucleotidic module that is linked to a solid phase; a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce a sequence cleavable by restriction enzyme A and/or B;
c) generating one C-terminal polynucleotidic building block comprising at least:
one polynucleotidic module; a single cleavage site for a first restriction enzyme A, placed on one side of the polynucleotidic module; a single cleavage site for a second restriction enzyme B, placed on the other side of the polynucleotidic module; wherein cleavage of said polynucleotidic building block with restriction enzyme B results in a polynucleotide comprising a polynucleotide module flanked on one side by a cohesive end that cannot be re-ligated with a polynucleotide building block cleaved by restriction enzyme A and/or B;
d) cutting said one C-terminal polynucleotidic building block of c) with restriction enzyme A; e) ligating the resulting C-terminal polynucleotidic module with the free end of one polynucleotide of b) immobilized on a solid phase, thereby producing a new immobilized polynucleotide comprising one additional polynucleotidic module; f) cutting the resulting new immobilized polynucleotide with restriction enzyme A, thus producing a new polynucleotide having a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme B; g) ligating the new polynucleotide with the free end of one polynucleotide of b) immobilized on a solid phase thus producing a new immobilized polynucleotide comprising one additional polynucleotidic module;
[0140] In a preferred embodiment, steps e) and g) are respectively followed by washing steps such as three washes with an adapted volume of saline buffer such as PBS well known in the art.
[0141] In another embodiment, steps f) and g) are repeated N times to produce an immobilized polynucleotide having an array of n polynucleotidic modules wherein n=N+3.
[0142] In another embodiment, step g) is replaced by the following steps:
g′) cutting said at least one polynucleotidic building block of a) with restriction enzyme A; h) ligating the resulting polynucleotidic module with the free end of one polynucleotide of b) immobilized on a solid phase, thereby producing a new immobilized polynucleotide comprising one additional polynucleotidic module; i) cutting the resulting new immobilized polynucleotide with restriction enzyme B, thus producing a new immobilized polynucleotide having a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A; j) ligating on the new produced immobilized polynucleotide said new polynucleotide resulting from step f) thereby producing a new immobilized polynucleotide comprising “x” additional polynucleotidic modules wherein “x” is equal to the number of polynucleotidic modules present in said new polynucleotide resulting from step f);
[0147] In a preferred embodiment, “x” can be any number comprised between 1 and 50, preferably, between 1 and 20, more preferably, 19, 18, 17, 16, 15, 14, 13, 12, 11, 10, 9, 8, 7, 6, 5, 4, 3, 2, or 1.
[0148] In a preferred embodiment, steps h) and j) are respectively followed by washing steps such as three washes with an adapted volume of saline buffer such as PBS well known in the art.
[0149] In another embodiment, said method of this aspect of the present invention further comprises the steps:
a) Cutting the resulting new immobilized polynucleotide of step j) with restriction enzyme A, thus producing a new polynucleotide having a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme B; b) Ligating the new polynucleotide with the free end of one polynucleotide of b) immobilized on a solid phase thus producing a new immobilized polynucleotide comprising one additional polynucleotidic module;
[0152] In a preferred embodiment, step b) is respectively followed by washing steps such as three washes with an adapted volume of saline buffer such as PBS well known in the art.
[0153] In another embodiment, at least one said polynucleotidic building block of a) and/or at least one polynucleotide linked to a solid phase of b) and/or said polynucleotidic building block of c) comprise a pre-assembly of more than one polynucleotidic module.
[0154] In another embodiment, at least one said polynucleotidic building block of a) and/or at least one polynucleotide linked to a solid phase of b) and/or said polynucleotidic building block of c) comprise a fragment of building block. In another embodiment, said fragment of building block is a building block deleted at its 3′ end. In another embodiment, said fragment of building block is a building block deleted in its center. In another embodiment, said fragment of building block encodes at least a half Transcription Activator-like Effector (TALE) DNA binding repeat module.
[0155] In another embodiment, at least one said polynucleotidic building block of a) and/or at least one polynucleotide linked to a solid phase of b) and/or said polynucleotidic building block of c) comprise a building block variant.
[0156] In another embodiment, at least one said polynucleotidic building block of a) and/or at least one polynucleotide linked to a solid phase of b) and/or said polynucleotidic building block of c) comprise a polynucleotide sequence not highly similar to a polynucleotide module according to a).
[0157] In another embodiment, at least one said polynucleotidic building block of a) and/or at least one polynucleotide linked to a solid phase of b) and/or said polynucleotidic building block of c) further comprises a fragment of building block according to a).
[0158] In another embodiment, said one polynucleotide of b) has been generated by:
b1) generating one polynucleotide linked to a solid phase comprising:
one polynucleotidic module; one end linked to a solid phase;
a single cleavage site for a first restriction enzyme A, placed on the side of the polynucleotidic module that is linked to a solid phase; a single cleavage site for a second restriction enzyme B placed on the other side of the polynucleotide module;
b2) cutting said polynucleotide linked to a solid phase with restriction enzyme B thereby obtaining a polynucleotide with a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce a sequence cleavable by restriction enzyme A and/or B;
[0165] In another embodiment, said one polynucleotide of b) has been generated by:
b1) generating one polynucleotide linked to a solid phase comprising:
one end linked to a solid phase; a polynucleotide sequence not highly similar to a polynucleotide module according to a), wherein said polynucleotide sequence comprises a single cleavage site for a first restriction enzyme A, placed on the side of the polynucleotidic module that is linked to a solid phase; a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce a sequence cleavable by restriction enzyme A and/or B;
[0170] In another embodiment, said one polynucleotide of b) has been generated by:
b1) generating one polynucleotide linked to a solid phase comprising:
one end linked to a solid phase; a polynucleotide sequence not highly similar to a polynucleotide module according to a), wherein said polynucleotide sequence comprises a single cleavage site for a first restriction enzyme A, placed on the side of the polynucleotidic module that is linked to a solid phase and a single cleavage site for a second restriction enzyme B placed on the other side of the polynucleotide module;
b2) cutting said polynucleotide linked to a solid phase with restriction enzyme B thereby obtaining a polynucleotide with a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce a sequence cleavable by restriction enzyme A and/or B;
[0175] In another embodiment, said one polynucleotide of b) has been generated by:
b1) generating one polynucleotide linked to a solid phase comprising:
one end linked to a solid phase; a polynucleotide sequence not highly similar to a polynucleotide module according to a), wherein said polynucleotide sequence comprises a single cleavage site for a first restriction enzyme A, placed on the side of the polynucleotidic module that is linked to a solid phase; a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce a sequence cleavable by restriction enzyme A and/or B;
b2) cutting a polynucleotidic building block described in a) with restriction enzyme A; b3) ligating the resulting polynucleotidic module with the free end of the polynucleotide immobilized on the solid phase; b4) cutting the resulting new immobilized polynucleotide with restriction enzyme B, thus producing a new immobilized polynucleotide comprising:
one end linked to a solid phase; a polynucleotide sequence not highly similar to a polynucleotide module according to a); one polynucleotidic module; a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce a sequence cleavable by restriction enzymes A and/or B.
[0187] In another embodiment, at least one polynucleotide linked to a solid phase of b) has been generated by a gene synthesis technology wherein said free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A has been obtained by using restriction enzymes or specific annealing and wherein said polynucleotide ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce at least a sequence cleavable by restriction enzyme A and/or B.
[0188] In another embodiment, said at least one polynucleotide linked to a solid phase of b) has been generated by:
synthesis of a first oligonucleotide linked to a solid phase; synthesis of a second oligonucleotide complementary to the first one;
[0191] wherein annealing of both oligonucleotides in appropriate conditions generates, without using restriction enzymes, a double stranded polynucleotide with a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce a sequence cleavable by restriction enzyme A and/or B.
[0192] Parameters for reaching annealing appropriate conditions of oligonucleotides are well known in the art.
[0193] In another embodiment, said at least one polynucleotide linked to a solid phase of b) has been generated by:
synthesis of a first oligonucleotide linked to a solid phase; synthesis of a second oligonucleotide complementary to the first one;
[0196] wherein annealing of both oligonucleotides in appropriate conditions generates a double stranded polynucleotide with a single cleavage site for a second restriction enzyme B placed on the side of the polynucleotide that is not linked to a solid phase;
Cutting said polynucleotide linked to a solid phase with restriction enzyme B thereby obtaining a polynucleotide with a free end compatible with the cohesive ends resulting from cleavage with restriction enzyme A, and which ligation with a polynucleotidic building block cleaved by restriction enzyme A will not produce a sequence cleavable by restriction enzyme A and/or B;
[0198] In another embodiment, said polynucleotide sequence not highly similar to a polynucleotide module according to a) is linked to said solid phase.
[0199] In another embodiment, at least one said polynucleotide linked to a solid phase of b) comprises a sequence not highly similar to a polynucleotide module according to a) encoding a N-terminal polypeptidic sequence of a TALE.
[0200] In another embodiment, at least one said polynucleotidic building block of a) and/or said polynucleotidic building block of c) comprises a sequence not highly similar to a polynucleotide module according to a) encoding a C-terminal polypeptidic sequence of a TALE.
[0201] In another embodiment, at least one said polynucleotidic building block of a) and/or at least one polynucleotide linked to a solid phase of b) and/or said polynucleotidic building block of c) further comprises at least one cleavage site for a restriction enzyme C located outward compared to restriction enzymes A and/or B cleavage sites.
[0202] In another embodiment, the last polynucleotide of b) used comprises a single cleavage site for a restriction enzyme C placed on the side of the polynucleotide linked to a solid phase, located outward compared to restriction enzyme A cleavage site, wherein said cleavage with restriction enzyme C allows to unlink said polynucleotide from the solid phase.
[0203] In another embodiment of the invention is a method further comprising the step of unlinking said final polynucleotide comprising an array of polynucleotidic modules by cutting it with restriction enzyme C.
[0204] In another embodiment of the invention is a method further comprising the steps of:
unlinking said final polynucleotide comprising an array of polynucleotidic modules of step g) by cutting it with restriction enzyme C; subcloning said final polynucleotide comprising an array of polynucleotidic modules into a plasmidic vector.
[0207] In another embodiment, said method further comprises the step of subcloning said final polynucleotide comprising an array of polynucleotidic modules from a plasmidic vector into another plasmidic vector by cutting it with restriction enzymes A and B;
[0208] In another embodiment of the invention is a method further comprising the steps of:
unlinking said final polynucleotide comprising an array of polynucleotidic modules of step g) by cutting it with restriction enzymes A and/or B; subcloning said final polynucleotide comprising an array of polynucleotidic modules into a plasmidic vector.
[0211] In another embodiment of this aspect of the invention is a method wherein said polynucleotidic modules to assemble share at least 85% similarity.
[0212] In another embodiment of this aspect of the invention is a method wherein each polynucleotidic module encodes a Transcription Activator-like Effector (TALE) DNA binding repeat module.
[0213] In another embodiment of this aspect of the invention is a method wherein said polynucleotide sequence not highly similar to a polynucleotide module according to a) encodes a C-terminal fragment of a TALE and wherein said fragment of building block encodes at least a half Transcription Activator-like Effector (TALE) DNA binding repeat module.
[0214] In another embodiment of this aspect of the invention, said single cleavage sites respectively for restriction enzymes A and B are two different cleavage sites cleavable by restriction enzymes which produce compatible cohesive overhang ends and wherein said compatible cohesive overhangs remove respective recognition sites for said restriction enzymes A and B upon ligation. In other words, restriction enzymes A and B according to the present invention produce at their respective single cleavage site compatible overhang cohesive ends without restoring a sequence cleavable by restriction enzymes A and B after ligation. In another embodiment, said restriction enzymes A and B belong to subtypes of class II restriction enzymes such as subtypes A, B, C, H and S as listed for example at http://_rebase.neb.com. In another embodiment, said restriction enzymes A and B of the present invention belong to typeIIS restriction enzymes. In a preferred embodiment said restriction enzymes A and B of the present invention are BbvI and SfaNI.
[0215] In another embodiment, said single cleavage sites respectively for restriction enzymes A and B can be cleavage sites for other enzymes such as nick-creating enzymes (nickases as non-limiting examples) under appropriate use to generate compatible overhang cohesive ends.
[0216] In another embodiment of this aspect of the invention, said restriction enzyme C is SfiI.
[0217] In another embodiment of this aspect of the invention is a method wherein said at least one polynucleotidic building block of a) and/or said polynucleotides of b) linked to a solid phase and/or said polynucleotidic building block of c) are part of a collection encoding polypeptidic repeated modules with Repeat Variable Dipeptide regions (RVDs) comprising a pair of amino acids responsible for recognizing one nucleotide selected from the group consisting of HD for recognizing C, NG for recognizing T, NI for recognizing A, NN for recognizing G or A, NS for recognizing A, C, G or T, HG for recognizing T, IG for recognizing T, NK for recognizing G, HA for recognizing C, ND for recognizing C, HI for recognizing C, HN for recognizing G, NA for recognizing G, SN for recognizing G or A and YG for recognizing T.
[0218] In another embodiment of this aspect of the invention, is a method wherein said at least one polynucleotidic building block of a) and/or said polynucleotides of b) linked to a solid phase and/or said polynucleotidic building block of c) are part of a collection encoding polypeptidic repeated modules with Repeat Variable Dipeptide regions (RVDs) comprising a pair of amino acids responsible for recognizing one nucleotide selected from the group consisting of HD for recognizing C, NG for recognizing T, NI for recognizing A, NN and NK for recognizing G.
[0219] In another embodiment of this aspect of the invention, is a method wherein said at least one polynucleotidic building block of a) and/or said polynucleotides of b) linked to a solid phase and/or said polynucleotidic building block of c) are part of a collection encoding “y” polypeptidic repeated modules with Repeat Variable Dipeptide regions (RVDs) for recognizing “y” nucleotides via “y” pairs of amino acids wherein “y” is comprised between 1 and 8. In another embodiment, “y” equals 1, 2, 3, 4, 5, 6, 7 or 8.
[0220] In another embodiment of this aspect of the invention, is a method wherein said at least one polynucleotidic building block of a) and/or said polynucleotides of b) and/or said polynucleotidic building block of c) linked to a solid phase are part of a collection encoding two polypeptidic repeated modules with Repeat Variable Dipeptide regions (RVDs) for recognizing two nucleotides via two pairs of amino acids selected from the group listed in table 2.
[0221] In another embodiment of this aspect of the invention, is a method wherein said at least one polynucleotidic building block of a) and/or said polynucleotides of b) and/or said polynucleotidic building block of c) linked to a solid phase are part of a collection encoding three polypeptidic repeated modules with Repeat Variable Dipeptide regions (RVDs) for recognizing three nucleotides via three pairs of amino acids selected from the group listed in table 3.
[0222] In another embodiment of this aspect of the invention, is a method wherein said at least one polynucleotidic building block of a) and/or said polynucleotides of b) linked to a solid phase and/or said polynucleotidic building block of c) are part of a library of degenerated building blocks.
[0223] In another embodiment of this aspect of the invention, a library of polynucleotidic building blocks are processed in previously described steps d) to g), g′) and h) to j) of the method of the present invention comprising a library of polynucleotidic modules. In another embodiment said library can be a random mutagenized library of polynucleotidic modules. In another embodiment, a library of polynucleotidic building blocks are used in previously described steps d) to g), g′) and h) to j) of the method of the present invention comprising a library of polynucleotidic modules and encoding a library of TALE repeat polynucleotidic modules. Mutagenesis can concern the entire polynucleotidic module sequence. In another embodiment said library can be a random mutagenized library of TALE repeat polynucleotidic modules. Mutagenesis of said TALE repeat polynucleotidic modules library can focused on critical amino acids such as amino acids located at positions 12 and 13 as non-limiting examples. Mutagenesis of said TALE repeat polynucleotidic modules library can focused on other critical amino acids of said TALE repeat polynucleotidic modules. Mutagenesis of said TALE repeat polynucleotidic modules library may concern the entire TALE repeat module sequence. Said libraries of polynucleotidic modules constituting libraries of polynucleotidic building blocks can be used according to the method of the present invention to introduce diversity into polynucleotides comprising an array of polynucleotidic modules. As non-limiting example, the method according to the present invention is particularly well-suited to introduce diversity into TALE repeat polynucleotidic modules in order to produce high-diversity libraries of TALE DNA binding domains.
[0224] In another aspect of the present invention is a method of conducting a high throughput custom-designed platform of TALE DNA binding domains comprising:
a) receiving a DNA target sequence comprising “n” nucleotides, which TALE DNA binding domain has to bind; b) generating and assembling polynucleotidic repeated modules, each comprising a pair of amino acids for recognizing each one of the “n” nucleotides of said DNA target sequence according to the present invention, thus releasing a TALE DNA binding domain able to recognize said DNA target sequence; c) providing said custom-designed TALE DNA binding domains.
[0228] In another embodiment “n” is comprised between 1 and 50, preferably 45, more preferably 40, more preferably 35, more preferably 30, more preferably, 29, 28, 27, 26, 25, 24, 23, 22, 21, 20, 19, 18, 17, 16, 15, 14, 13, 12, 11, 10, 9, 8, 7, 6, 5, 4, 3, 2 or 1.
[0229] In another aspect of the present invention is a method of conducting a high throughput custom-designed platform of chimeric protein derived from a TALE comprising:
a) Receiving a DNA target sequence comprising “n” nucleotides, which a chimeric protein derived from a TALE has to process; b) Generating and assembling polynucleotidic repeated modules, each comprising a pair of amino acids for recognizing each one of the “n” nucleotides of said DNA target sequence according to the present invention, thus releasing a TALE DNA binding domain able to recognize said DNA target sequence; c) Fuse said DNA binding domain to a protein domain able to process said DNA target sequence; d) Providing said custom-designed chimeric protein derived from a TALE.
[0234] In another embodiment “n” is comprised between 1 and 50, preferably 45, more preferably 40, more preferably 35, more preferably 30, more preferably, 29, 28, 27, 26, 25, 24, 23, 22, 21, 20, 19, 18, 17, 16, 15, 14, 13, 12, 11, 10, 9, 8, 7, 6, 5, 4, 3, 2 or 1.
[0235] In another aspect of the present invention is a kit for generating and assembling polynucleotides comprising arrays of at least two highly similar polynucleotidic modules according to the present invention comprising at least a collection of “n” polynucleotidic building blocks encoding “n” polypeptidic repeated modules with Repeat Variable Dipeptide regions (RVDs) for recognizing “n” nucleotides via “n” pairs of amino acids (TALE “n” repeat modules or “n” repeat modules) and instructions to use it.
[0236] In another aspect of the present invention is a method for producing high diversity libraries of polynucleotides comprising arrays of polynucleotidic modules encoding TALE DNA binding domains comprising:
a) Generating a high diversity library of polynucleotidic building blocks; b) Assembling polynucleotidic building blocks according to the method of the present invention by using high diversity library of polynucleotidic building blocks of step a) for previously described steps d) to g).
DEFINITIONS
[0239] By “polynucleotidic building block(s)” or “building block(s)” is intended polynucleotidic entities or polynucleotides comprising polynucleotidic modules to assemble according to the present invention. Said building block(s) comprises one or several polynucleotidic modules and allows the assembly of several polynucleotidic modules. In addition to polynucleotidic module(s), said polynucleotidic building block(s) can comprise one single cleavage site for a restriction enzyme or two single cleavage sites for different restriction enzymes and wherein cleavage of said polynucleotidic building blocks with restriction enzyme(s) result in compatible cohesive ends which allow the assembly of several polynucleotidic modules. In addition, said polynucleotidic building block(s) can comprise other polynucleotidic sequences not highly similar to a polynucleotidic module according to the present invention. A “fragment of polynucleotidic building block(s)” or “a fragment of building blocks” can be used in the present invention to describe a building block according to the present invention comprising only one single cleavage site for a restriction enzyme A or B or lacking one single cleavage site for a restriction enzyme A or B. A “fragment of polynucleotidic building block” can be deleted at its 3′ end, at its 5′ end or in its center. More generally, the expression “fragment of polynucleotidic building block” is used to describe a truncated polynucleotide building block.
[0240] By “degenerated building block” is intended a polynucleotidic building block which contains one difference or several differences at specific locations in its sequence compared to a polynucleotidic building block of reference. This particularly applies when diversity has to be introduced in said polynucleotidic building block. Degenerated polynucleotidic building blocks with partial or total diversity introduced at one or several locations of its nucleotidic codon sequence can be used to screen the best interaction of a polynucleotidic building block toward a DNA target sequence; as a non-limiting example, a DNA target sequence of interest can be used as a bait to screen a library of “degenerated building blocks” wherein each “degenerated building block” comprises a similar and related sequence containing diversity at one or several nucleotidic codons (and amino acids encoded by these codons).
[0241] By “polynucleotidic module(s)” or “modules” is intended polynucleotidic entities or polynucleotides to assemble according to the present invention. Said polynucleotidic module(s) can be highly similar modules such as TALE repeat modules as a non-limiting example. Highly similar modules present in multiple copies can be described as “repeated modules”.
[0242] “Pre-assembly” means that a polynucleotidic building block used to elongate the polynucleotidic modules assembly process according to the present invention can comprise more than one polynucleotidic module. In this case, said polynucleotidic building block can be described as pre-assembled.
[0243] By a “TALE-nuclease” (TALEN) is intended a fusion protein consisting of a DNA-binding domain derived from a Transcription Activator Like Effector (TALE) and one nuclease catalytic domain to cleave a nucleic acid target sequence. First published TALEN are formed by fusion of the cleavage domain of FokI and a TALE DNA binding domain.
[0244] By “TALE DNA binding domain” is intended part of a Transcription Activator Like Effector (TALE) responsible of DNA binding and composed by a variable number of 33-35 amino acids “repeat modules” or “TALE repeat polynucleotidic modules” or “TALE repeat modules” or “RVDs domains”. The nature of residues 12 and 13 determines base preferences of individual repeat module.
[0245] By “chimeric protein” according to the present invention is meant any fusion protein comprising a set of repeated modules with RVDs (or with RVDs-like domains) to bind a nucleic acid sequence and one protein domain to process a nucleic acid target sequence adjacent to said bound nucleic acid sequence. Said chimeric protein according to the present invention can function as a dimer wherein each monomer constituting said chimeric dimeric protein comprises a set of repeated modules with RVDs (or with RVDs-like domains) to bind a nucleic acid sequence and one protein domain to process a nucleic acid target sequence adjacent to said bound nucleic acid sequence. “identity” refers to sequence identity between two nucleic acid molecules or polypeptides. Identity can be determined by comparing a position in each sequence which may be aligned for purposes of comparison. When a position in the compared sequence is occupied by the same base, then the molecules are identical at that position. A degree of “similarity” or identity between nucleic acid or amino acid sequences is a function of the number of identical or matching nucleotides or amino acids at positions shared by the nucleic acid or polypeptidic sequences. Various alignment algorithms and/or programs may be used to calculate the identity between two sequences, including FASTA, or BLAST which are available as a part of the GCG sequence analysis package (University of Wisconsin, Madison, Wis.), and can be used with, e.g., default setting. Common software tools used for general sequence alignments taskes include ClustalW for alignment and BLAST or FASTA for database searching.
[0246] In sequence alignments of proteins, the degree of similarity between aminoacids occupying a particular position in the sequence can be interpreted as a rough measure of how conserved a particular region or a sequence motif is among lineages. The absence of substitutions in a particular region or sequence or the presence of only very conservative substitutions by amino acids whose side chains have similar biochemical properties, suggest that this region has structural or functional importance.
[0247] “Percent identity” or “percent similarity” are used to quantify the similarity between biomolecule sequences. For two naturally occurring sequences, percent identity is a factual measurement, whereas similarity is a hypothesis supported by evidence.
[0248] Amino acid residues in a polypeptide sequence can be designated herein according to the one-letter or three-letter code, in which, for example, Q means Gln or Glutamine residue, R means Arg or Arginine residue and D means Asp or Aspartic acid residue.
[0249] Amino acid substitution means the replacement of one amino acid residue with another, for instance the replacement of an Arginine residue with a Glutamine residue in a peptide sequence is an amino acid substitution.
[0250] Nucleotides are designated as follows: one-letter code is used for designating the base of a nucleoside: a is adenine, t is thymine, c is cytosine, and g is guanine. For the degenerated nucleotides, r represents g or a (purine nucleotides), k represents g or t, s represents g or c, w represents a or t, m represents a or c, y represents t or c (pyrimidine nucleotides), d represents g, a or t, v represents g, a or c, b represents g, t or c, h represents a, t or c, and n represents g, a, t or c.
[0251] by “DNA target”, “DNA target sequence”, “target DNA sequence”, “nucleic acid target sequence”, “target sequence”, or “target” is intended a polynucleotide sequence that is recognized by the DNA binding domain of a protein. These terms refer to a specific DNA location, preferably a genomic location in a cell, but also a portion of genetic material that can exist independently to the main body of genetic material such as plasmids, episomes, virus, transposons or in organelles such as mitochondria or chloroplasts as non-limiting examples. The nucleic acid target sequence is defined by the 5′ to 3′ sequence of one strand of said target.
[0252] by “generating” a polynucleotide, a polynucleotidic building block or another polynucleotidic entity is meant to synthesize or to make synthesize this entity by one of the gene synthesis methods well-known in the art. It is also encompassed in this definition the generation of said polynucleotidic entity by Polymerase Chain Reaction using appropriate oligonucleotide primers, degenerated or not, linked to a non-polynucleotidic entity, such as Biotin as a non-limiting example, or not.
[0253] by “variant”, “polynucleotidic building block variant”, “building block variant”, “chimeric protein variant” is intended a molecule obtained by replacement of at least one nucleotide, or at least one amino acid residue compared to a polynucleotidic building block, a building block or a chimeric protein, respectively taken as a reference. According to this definition, a variant can result from a truncation, or a mutation or a sequence insertion. Said inserted sequence can possibly be one or several nucleotides, one or several amino acids, one protein motif or one reporter protein.
[0254] The above written description of the invention provides a manner and process of making and using it such that any person skilled in this art is enabled to make and use the same, this enablement being provided in particular for the subject matter of the appended claims, which make up a part of the original description.
[0255] As used above, the phrases “selected from the group consisting of,” “chosen from,” and the like include mixtures of the specified materials.
[0256] Where a numerical limit or range is stated herein, the endpoints are included. Also, all values and subranges within a numerical limit or range are specifically included as if explicitly written out.
[0257] The above description is presented to enable a person skilled in the art to make and use the invention, and is provided in the context of a particular application and its requirements. Various modifications to the preferred embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments and applications without departing from the spirit and scope of the invention. Thus, this invention is not intended to be limited to the embodiments shown, but is to be accorded the widest scope consistent with the principles and features disclosed herein.
[0258] Having generally described this invention, a further understanding can be obtained by reference to certain specific examples, which are provided herein for purposes of illustration only, and are not intended to be limiting unless otherwise specified.
EXAMPLES
Example 1
Sequential Assembly of Trancription Activator-Like Effector (TALE) Repeat Polynucleotidic Modules in Solution
[0259] 1a—Construction of Polynucleotidic Building Blocks Comprising TALE Repeat Polynucleotidic Modules
[0260] TALE repeat polynucleotidic modules or repeat modules or TALE repeat modules of AvrBS3 from Xanthomonas spp. plant pathogen, containing the RVDs NN, NK, NI, HD, NG and the terminal half repeat NG* are synthesized and cloned in the pAPG10 plasmid between restriction sites AscI and PacI (SEQ ID NO: 6-12, FIG. 1 ). Within the pAPG10 plasmid, mono repeats are flanked by a 5′ end region containing SfiI and BbvI sites and 3′ end region containing SfaNI and SfiI sites ( FIG. 1A ), i.e a polynucleotidic building block (SEQ ID NO: 13-18). BbvI and SfaNI restriction sites are designed to generate compatible overhangs that allow for coupling two repeat modules together in an oriented fashion. For that purpose, BbvI site is oriented to cut inward into the 5′ end of the repeat module sequence such that digestion leaves the appropriate overhang (GACC) to accept a SfaNI digested additional repeat module. Accordingly, SfaNI site was oriented to cut outward into the 3′ end flanking sequence of the repeat module such that digestion leaves an appropriate overhang (CTGG) to accept a BbvI digested repeat module. The terminal half RVD is synthesized and subcloned in pAPG10 according to the same strategy except that the SfaNI site is oriented to cut inward into the 3′ end sequence of the repeat module ( FIG. 1B ). Example of building block encoding a terminal half RVD is given by SEQ ID NO: 19. SfaNI digestion generates an overhang that is compatible with the one generated by BsmB1 in the final acceptor plasmid (pCLS7183, SEQ ID NO: 20) as will be described below. This design is intended to control the orientation of TALE repeat insertion within pCLS7183. pCLS7183 (SEQ ID NO: 20) is an expression vector comprising the N-terminal and C-terminal domains of the of AvrBs3 protein. A BsmB1 recognition site has been appropriately introduced between the 2 domains. The expression of the chimeric protein is driven by a CMV promoter and can comprise a protein domain able to process a nucleic target sequence adjacent to the nucleic acid sequence bound by the TALE DNA binding domain.
[0261] As an illustrative example, to prepare the building block encoding di repeat module 1-2, pAPG10 encoding the repeat modules 1 and 2 [building blocks encoding modules 1 and 2 (SEQ ID NO: 13 and 14)] are first digested by SfiI ( FIGS. 2A and 2B ). Extracted building blocks encoding repeat modules 1 and 2 are purified from agarose gel and then digested respectively by SfaNI and BbvI ( FIGS. 2A and 2B ) (SEQ ID NO: 21 and 22). Digested fragments are then ligated together to form the building block encoding di repeat module fragment 1-2 in a seamless manner ( FIG. 2C ) (SEQ ID NO: 23). Building block encoding di repeat module fragment is then purified on column, subcloned into the SfiI digested pAPG10 and transformed in DH5α competent E. coli ( FIG. 2C , lower part). Clones having building block encoding di repeat module are identified by colony PCR screening using appropriate primers (M13_Forward and M13_Reverse, SEQ ID NO: 24-25 respectively).
[0262] 1b—Sequential Assembly of TALE Repeat Polynucleotidic Modules
[0263] A method to assemble TALE repeat polynucleotidic modules comprised in polynucleotidic building blocks (or TALE building blocks) was designed according to the following protocol. It should be noted that TALE building blocks may contain multiple TALE repeat modules obtained from previous assemblies. As illustrated in FIG. 3 , below is described an example of 15.5 repeat fragment assembly using building blocks encoding TALE di repeat modules.
[0264] a—Choose a plasmid containing the first building block encoding the desired TALE di repeat module, extract it with SfiI and SfaNI restriction enzymes (polynucleotidic module A), and purify it on column (As an illustrating non-limiting example a TALE di repeat module HD_NI digested by SfiI and SfaNI is given by SEQ ID NO: 26);
[0265] b—Choose the plasmid containing the appropriate second building block encoding the desired second TALE di repeat module, extract it with SfiI and BbvI restriction enzymes (polynucleotidic module B), and purify it on column (As an illustrating non-limiting example a TALE di repeat module NG_NK digested by SfiI and SfaNI is given by SEQ ID NO: 27);
[0266] c—Ligate polynucleotidic modules A and B and purify the ligation product (polynucleotide AB) on column (Resulting TALE four repeat module HD_NI_NG_NK is given by SEQ ID NO: 28);
[0267] d—In parallel, repeat steps (a)-(c) using the appropriate plasmids in order to generate polynucleotide CD;
[0268] e—Digest polynucleotide AB with SfaNI and polynucleotide CD with BbvI and purify both of them on column;
[0269] f—Ligate polynucleotides AB with CD together with SfiI digested pAPG10 and transform it in DH5α E. coli;
[0270] g—PCR Screen for polynucleotides having the size of ABCD (8 TALE repeats polynucleotide);
[0271] h—Extract the 8 TALE repeats polynucleotide with SfiI and SfaNI restriction enzyme (polynucleotide ABCD) and purify it on column;
[0272] i—Repeat steps (a)-(g) using the appropriate plasmids to generate polynucleotide EFGH (with polynucleotide H encoding the last half RVD);
[0273] j—Extract the 7.5 TALE repeats polynucleotide with SfiI and BbvI restriction enzyme (polynucleotide EFGH) and purify it on column;
[0274] k—Ligate polynucleotides ABCD and EFGH together with SfiI digested pAPG10 and transform ligation products in DH5 a E. coli;
[0275] l—Colony PCR screen for polynucleotides having the size of ABCDEFGH (15.5 TALE repeats polynucleotide).
[0276] 1c—Materials and Methods
[0277] Preparation of TALE Repeat Polynucleotidic Modules
[0278] To prepare TALE repeat polynucleotidic modules for subsequent assembly, pAPG10 bearing TALE repeat polynucleotidic modules were first digested by SfiI. Digestion mixture consisted in 100 μL of a pAPG10 maxiprep containing the desired module (1 μg/μL), 5 μL SfiI (75 U, NEB), 12 μL NEB3 buffer (NEB), 1.2 μL BSA 100× and 1.8 μL H 2 0. Digestion was allowed to proceed for 1 hour at 50° C. Digestion products were separated on a 0.8% agarose gel and SfiI digested TALE repeat polynucleotides were extracted from the gel using Nucleospin extract II kit (Macherey-Nagel) and recovered in 35 μL H 2 0. 25 μL of extracted TALE repeat polynucleotides were then added to either SfaNI or BbvI digestion mixtures. SfaNI and BbvI digestion mixtures contained 2 μL of restriction enzymes (3U), 3 μL of NEB3 or NEB2 10× respectively and 5 μL H 2 0. Digestion was allowed to proceed for 1 hour at 37° C. Digested products were then column purified using Nucleospin extract II kit (Macherey-Nagel) and recovered in 35 L H 2 0. The overall process generated about 5 μg of digested TALE repeat polynucleotidic module ready for assembly.
[0279] Assembly of 15.5 TALE Repeats Polynucleotide
[0280] To assemble the 15.5 TALE repeats polynucleotide CAPT1.3 described in this example, the 8 first TALE repeats polynucleotide and the 7.5 last TALE repeats polynucleotide (named respectively 8 TALE repeats left and 7.5 TALE repeat right in FIG. 4 ) were first assembled separately and then coupled together according to the method described in FIG. 3 .
[0281] Assembly of 8 TALE Repeats Left and 7.5 TALE Repeats Right Polynucleotides
[0282] Concerning the assembly of the 8 TALE repeats left polynucleotide, 5 μL of SfaNI digested first TALE di repeat module Rvd_b1 (20 ng/μL), was first ligated with 5 μL of Bbv I digested Rvd_b16 (20 ng/μL) in the presence of 1 μL of T4 DNA ligase (3U, promega) and 10 μL of 2× rapid ligation buffer (Promega). Ligation was allowed to proceed for 1 hour at room temperature. Ligation product was then column purified using the Nucleospin extract II kit (Macherey-Nagel) and eluted in 35 μL H 2 0. 10 μL of the purified ligation product Rvd_b1-Rvd_b16 was then added to the SfaNI digestion mixture containing 1 μL SfaNI fast digest (Fermentas) and 10 μL fast digest buffer 2×(Fermentas). Digestion was allowed to proceed for 1 hour at 37° C. and the digestion product was then purified using Nucleospin extract II kit (Macherey-Nagel) and eluted in 35 μL H20. In parallel, the third and the fourth TALE di repeat polynucleotide Rvd_b15 and Rvd_b9 were ligated together and the ligation product was purified according to the same protocol. 10 μL of the purified ligation product Rvd_b15-Rvd_b9 was then added to the BbvI digestion mixture containing 1 μL BbvI (Fermentas) and 10 μL BbvI digestion buffer 2× (Fermentas). Digestion was allowed to proceed for 1 hour at 65° C. and the digestion product was purified using Nucleospin extract II kit (Macherey-Nagel) and eluted in 35 μL H 2 0.
[0283] To complete the assembly of 8 TALE repeats left polynucleotide, 5 μL of SfaNI digested Rvd_b1-Rvd_b16 was added to 5 μL of BbvI digested Rvd_b15-Rvd_b9 in the presence of 1 μL of T4 DNA ligase (3U, Promega) in a final volume of 20 μL of rapid ligation buffer 1× (Promega). Ligation was allowed to proceed for 45 min at room temperature. To subclone the 8 TALE repeats left polynucleotide into pAPG10, 5 μL of the ligation product was mixed with 1 μL of SfiI digested pAPG10 cut vector (20 ng/μL), 5 μL of Rapid ligation buffer and 1 μL of T4 DNA ligase (Promega). Ligation was allowed to proceed for 30 min at room temperature.
[0284] 5 μL of this ligation mixture was added to 30 μL of E. coli DH5α chimio competent cells (Invitrogen). Cells were transformed according to the manufacturer guidelines and plated on LB AGAR plates supplemented by ampiciline.
[0285] Transformants containing pAPG10 bearing the 8 TALE repeats left polynucleotide were identified by colony PCR screening using M13_F and M13_R as PCR primers (SEQ ID NO: 24-25).
[0286] The same procedure was used to generate and select the 7.5 TALE repeats left polynucleotide using Rvd_b1, Rvd_b12 and Rvd_T1
[0287] Coupling of 8 TALE Repeats Left and 7.5 TALE Repeats Right Polynucleotides
[0288] To generate the final 15.5 TALE repeats polynucleotide CAPT1.3, the 8 TALE repeats left and 7.5 TALE repeat right polynucleotides were first extracted from pAPG10 and then ligated together.
[0289] TALE repeats left and right polynucleotides were extracted from pAPG10 by SfiI digestion and gel purification. To do so, 20 μL of pAPG10 DNA preparation containing either TALE repeats left or right polynucleotides was added to a mixture containing 2 μL
[0290] SfiI (40U, NEB), 3 μL of BSA 10×, 3 μL, of NEB 4 buffer 10× (NEB), and 2 μL H 2 0. The digestion was allowed to proceed 1 hour at 50° C. Digestion products were run onto 0.8% agarose gel and extracted using Nucleospin extract II kit (Macherey-Nagel) and 35 μL H 2 0 for sample elution.
[0291] 10 μL of purified 8 TALE repeats left or 7.5 TALE repeat right polynucleotides were then added to digestion mixtures containing SfaNI or BbvI respectively. Digestion mixtures contained 1 μL of restriction enzyme (either SfaNI Fast digest or BbvI, Fermentas) in a final volume of 10 μL of SfaNI or BbvI digestion buffer 2× (Fermentas). Digestion was allowed to proceed for 1 hour. Digestion products were purified using Nucleospin extract II kit (Macherey-Nagel) and eluted in 35 μL H 2 O.
[0292] 5 μL of SfaNI digested 8 TALE repeats left polynucleotides were added to 5 μL of BbvI digested 7.5 TALE repeats right polynucleotides in the presence of 10 μL of Fast Ligase buffer 2× (Promega) and 1 μL of T4 DNA ligase (Promega). The ligation was allowed to proceed for 1 hour at room temperature. 1 μL of SfiI digested pAPG10 cut vector (20 ng/μL) was then added to the ligation mixture and the reaction was allowed to proceed for 30 min at room temperature. 3 μL of this ligation mixture was added to 30 μL of DH5α chimio competent cells (Invitrogen). Cells were transformed according to the manufacturer guidelines and plated on LB AGAR plates supplemented by ampiciline. Transformants containing pAPG10 bearing the 15.5 TALE repeats polynucleotide CAPT1.3 were identified by colony PCR screening using M13_F and M13_R as PCR primers (SEQ ID NO: 24-25).
[0293] 1d—Assembly of TALE Repeats Polynucleotides CAPT1.3 and CAPT1.4 (15.5 TALE Repeats Polynucleotides)
[0294] The method described above was used to generate 2 different 15.5 TALE repeats polynucleotide s that recognize the heterodimeric target CAPT1.1 (SEQ ID NO: 32) ( FIG. 4 , A). This target is located in the coding sequence of Calpain I small subunit, a protein known to be associated with myotonic dystrophy. CAPT1.1 target (SEQ ID NO: 32) is divided into 3 parts, the CAPT1.3 target (SEQ ID NO: 1), a 15 bp spacer (SEQ ID NO: 33) and the CAPT1.4 target (SEQ ID NO: 2) ( FIG. 4A , green, red and cyan respectively). To assemble both TALE repeat polynucleotides, CAPT1.3 (SEQ ID NO: 1) and CAPT1.4 (SEQ ID NO: 2) targets were first translated into RVD motif sequences then into polynucleotidic building blocks encoding polynucleotide modules with appropriate sequences. In this example, polynucleotidic building blocks comprises TALE di repeats modules that were obtained as intermediates of previous synthesis see below (section 1e). These building blocks sequences were separated into two parts named 8 TALE repeats left and 7.5 TALE repeats right. Building blocks were then assembled in parallel to generate left 8 TALE repeats polynucleotide and right 7.5 TALE repeats polynucleotide according to the method described above. Both left and right polynucleotides were subcloned into pAPG10 and transformed into E. coli . Transformation resulted in the growth of more than 1000 colonies on LB plate. Among 24 screened colonies, we obtained about 33% of left 8 TALE repeats polynucleotide or right 7.5 TALE repeats polynucleotide ( FIG. 4B ). The correct left 8 TALE repeats or right 7.5 TALE repeats polynucleotides were selected, extracted from pAPG10, ligated together and transformed into E. coli . Again, transformation resulted in the growth of more than 1000 colonies on LB plate and among 24 screened colonies, we obtained about 50% of 15.5 TALE repeats polynucleotides ( FIG. 4C ).
[0295] 1e—Generation of Libraries of TALE Di and Tri Repeat Modules
[0296] During assembly of TALE DNA binding domains, assembly intermediates containing TALE di or tri repeats were recovered and used to generate libraries of TALE-encoding building blocks. A complete set of pAPG10 plasmids encoding all the 20 possible TALE di repeat modules and all the 64 possible TALE tri repeat modules (including the last terminal half repeat module) was generated. These libraries of TALE-encoding building blocks were used to assemble custom TALE repeats according to the method described in this example and in examples 2 and 3.
[0297] Below in tables 1 to 3 are displayed libraries of mono, di and tri repeat modules.
[0000]
TABLE 1
Library of TALE mono repeat modules
TAL repeats name
RVD motif
Targeted Bases
rvd_m1
HD
C
rvd_m2
NG
T
rvd_m3
NI
A
rvd_m4
NN
G
rvd_m5
NK
G
rvd_mt
NG#
T
[0000]
TABLE 2
Library of TALE di repeat modules
TAL di repeats name
RVD motives
Targeted Bases
rvd_b1
HD-HD
CC
rvd_b2
HD-NG
CT
rvd_b3
HD-NI
CA
rvd_b4
HD-NN
CG
rvd_b5
NG-HD
TC
rvd_b6
NG-NG
TT
rvd_b7
NG-NI
TA
rvd_b8
NG-NN
TG
rvd_b9
NI-HD
AC
rvd_b10
NI-NG
AT
rvd_b11
NI-NI
AA
rvd_b12
NI-NN
AG
rvd_b13
NN-HD
GC
rvd_b14
NN-NG
GT
rvd_b15
NN-NI
GA
rvd_b16
NN-NN
GG
rvd_b17
NG-NK
TG
rvd_b18
HD-NK
CG
rvd_b19
NI-NK
AG
rvd_b20
NK-HD
GC
rvd_b21
NK-NI
GA
rvd_b22
NK-NK
GG
rvd_b23
NK-NG
GT
rvd_bt1
HD-NG#
CT
rvd_bt2
NG-NG#
TT
rvd_bt3
NI-NG#
AT
rvd_bt4
NN-NG#
GT
[0000]
TABLE 3
Library of TALE tri repeat modules
Targeted
TAL tri repeats name
RVD motives
Bases
rvd_t1
HD-HD-HD
CCC
rvd_t2
HD-HD-NG
CCT
rvd_t3
HD-HD-NI
CCA
rvd_t4
HD-HD-NN
CCG
rvd_t5
HD-NG-HD
CTC
rvd_t6
HD-NG-NG
CTT
rvd_t7
HD-NG-NI
CTA
rvd_t8
HD-NG-NN
CTG
rvd_t9
HD-NI-HD
CAC
rvd_t10
HD-NI-NG
CAT
rvd_t11
HD-NI-NI
CAA
rvd_t12
HD-NI-NN
CAG
rvd_t13
HD-NN-HD
CGC
rvd_t14
HD-NN-NG
CGT
rvd_t15
HD-NN-NI
CGA
rvd_t16
HD-NN-NN
CGG
rvd_t17
NG-HD-HD
TCC
rvd_t18
NG-HD-NG
TCT
rvd_t19
NG-HD-NI
TCA
rvd_t20
NG-HD-NN
TCG
rvd_t21
NG-NG-HD
TTC
rvd_t22
NG-NG-NG
TTT
rvd_t23
NG-NG-NI
TTA
rvd_t24
NG-NG-NN
TTG
rvd_t25
NG-NI-HD
TAC
rvd_t26
NG-NI-NG
TAT
rvd_t27
NG-NI-NI
TAA
rvd_t28
NG-NI-NN
TAG
rvd_t29
NG-NN-HD
TGC
rvd_t30
NG-NN-NG
TGT
rvd_t31
NG-NN-NI
TGA
rvd_t32
NG-NN-NN
TGG
rvd_t33
NI-HD-HD
ACC
rvd_t34
NI-HD-NG
ACT
rvd_t35
NI-HD-NI
ACA
rvd_t36
NI-HD-NN
ACG
rvd_t37
NI-NG-HD
ATC
rvd_t38
NI-NG-NG
ATT
rvd_t39
NI-NG-NI
ATA
rvd_t40
NI-NG-NN
ATG
rvd_t41
NI-NI-HD
AAC
rvd_t42
NI-NI-NG
AAT
rvd_t43
NI-NI-NI
AAA
rvd_t44
NI-NI-NN
AAG
rvd_t45
NI-NN-HD
AGC
rvd_t46
NI-NN-NG
AGT
rvd_t47
NI-NN-NI
AGA
rvd_t48
NI-NN-NN
AGG
rvd_t49
NN-HD-HD
GCC
rvd_t50
NN-HD-NG
GCT
rvd_t51
NN-HD-NI
GCA
rvd_t52
NN-HD-NN
GCG
rvd_t53
NN-NG-HD
GTC
rvd_t54
NN-NG-NG
GTT
rvd_t55
NN-NG-NI
GTA
rvd_t56
NN-NG-NN
GTG
rvd_t57
NN-NI-HD
GAC
rvd_t58
NN-NI-NG
GAT
rvd_t59
NN-NI-NI
GAA
rvd_t60
NN-NI-NN
GAG
rvd_t61
NN-NN-HD
GGC
rvd_t62
NN-NN-NG
GGT
rvd_t63
NN-NN-NI
GGA
rvd_t64
NN-NN-NN
GGG
rvd_tt1
HD-HD-NG#
CCT
rvd_tt2
HD-NG-NG#
CTT
rvd_tt3
HD-NI-NG#
CAT
rvd_tt4
HD-NN-NG#
CGT
rvd_tt5
NG-HD-NG#
TCT
rvd_tt6
NG-NG-NG#
TTT
rvd_tt7
NG-NI-NG#
TAT
rvd_tt8
NG-NN-NG#
TGT
rvd_tt9
NI-HD-NG#
ACT
rvd_tt10
NI-NG-NG#
ATT
rvd_tt11
NI-NI-NG#
AAT
rvd_tt12
NI-NN-NG#
AGT
rvd_tt13
NN-HD-NG#
GCT
rvd_tt14
NN-NG-NG#
GTT
rvd_tt15
NN-NI-NG#
GAT
rvd_tt16
NN-NN-NG#
GGT
Example 2
Solid Phase Assembly of TALE Repeat Polynucleotidic Modules Using a Parallel Sequential Process
[0298] 1a—Method for Parallel Sequential Assembly of TALE Repeat Polynucleotidic Modules Using a Streptavidin Coated Well and Streptavidin Coated Magnetic Beads as Solid Phases.
[0299] An efficient and highly versatile high throughput method for TALE DNA binding domains was implemented. It consists in a sequential assembly of TALE repeat polynucleotidic modules (constituting a TALE DNA binding domain) comprised in polynucleotidic building blocks on a streptavidin coated solid phase supported by a 96 well plate format. In this method, the first polynucleotidic building block of the TALE repeat polynucleotide to assemble is biotinylated on 5′. This first biotinylated polynucleotidic building block is immobilized onto a streptavidin-coated solid phase (either streptavidin-coated well or magnetic beads) and serves as an anchor for TALE repeat polynucleotidic modules assembly. TALE repeat polynucleotidic modules assembly proceeds through a sequential addition of TALE-encoding building blocks according to the method described in example 1.
[0300] 1a—Sequential and Parallel Assembly Process
[0301] We used two types of streptavidin coated solid phases:
streptavidin coated wells (Thermo fisher) streptavidin coated magnetic beads (Ademtech)
[0304] The handling of both solid phases is essentially the same. However, there are two main differences between the two, the reaction volume (100 μL for streptavidin coated wells and 50 μL for streptavidin coated magnetic beads), and the need of a magnet for streptavidin coated magnetic beads. As illustrated in FIG. 5 , below is described an example of 15.5 TALE repeats polynucleotide synthesis using building blocks encoding TALE di repeat modules.
[0305] This method includes the following steps:
a—Choose the shuttle plasmid containing the first building block encoding the desired TALE di repeat module (polynucleotidic module A), PCR amplify it with TAL_Shuttle_Bio_Forward primer and TAL_Shuttle_Reverse (SEQ ID NO: 29 and 30 respectively), digest it with SfaNI and purify it on column, leading to polynucleotidic module A; b—Choose the pAPG10 containing the appropriate second, third and fourth building blocks (respectively encoding TALE di repeat polynucleotidic modules B, C, D), extract them from pAPG10 using SfiI according to the method described in example 1 or alternatively, PCR amplify them with TAL_Shuttle_short_Forward primer and TAL_Shuttle_Reverse primer (SEQ ID NO: 31 and 30, FIG. 5A ) and purify them. Digest purified fragments with BbvI and purify them on column leading to polynucleotidic modules B, C and D; c—Immobilisation of the biotinylated first building block on a streptavidin coated magnetic beads ( FIG. 5B ); d—Ligation of polynucleotidic modules A and B followed by a washing step with a saline buffer to remove secondary reaction products, ligation buffer and enzymes ( FIG. 5C ); e—SfaNI digestion of polynucleotide AB followed by a washing step with a saline buffer to remove secondary reaction products, restriction buffer and enzymes ( FIG. 5C ); f—Repeat steps d to e with BbvI digested polynucleotidic modules C and D ( FIG. 5C ); g—In parallel, repeat steps a to f with polynucleotidic modules E, F, G, H ( FIG. 5C ); h—SfaNI digestion of ABCD polynucleotide and BbvI digestion of EFGH polynucleotide ( FIG. 5C ). i—Recovery of EFGH polynucleotide by column purification and ligation with polynucleotide ABCD still attached to the streptavidin coated solid phase ( FIG. 5C ). j—SfiI digestion, recovery and column purification of ABCDEFGH polynucleotide ( FIG. 5C ). k—Subcloning of ABCDEFGH polynucleotide into SfiI digested pAPG10 and transformation into DH5α E. coli ( FIG. 5C ). l—Colony PCR screen for polynucleotide having the size of an hexadeca TALE repeat polynucleotide ( FIG. 5C ).
[0318] 1b—Materials and Methods
[0319] PCR Amplification and Digestion of TALE Building Blocks
[0320] Respectively, the first TALE building blocks of left and right TALE repeat polynucleotides were amplified from pAPG10 using TAL_Shuttle_Bio_Forward and TAL_Shuttle_Reverse primers (SEQ ID NO: 29 and 30 respectively). TAL_Shuttle_Bio_Forward contained a biotinylated moiety that binds specifically to the streptavidin coated solid phase. TALE repeat polynucleotidic modules or TALE repeat polynucleotides used for subsequent assembly could be obtained via the method described in section 1a, and could be also obtained by PCR using TAL_Shuttle_short_Forward and TAL_Shuttle_Reverse primers (SEQ ID NO 31 and 30). Conditions for amplification were 5 ng of pAPG10 containing mono or multiple TALE repeat polynucleotidic modules, 250 μM dNTP mix, 200 nM of each oligonucleotide, 1 μL of Herculase II Fusion DNA Polymerase (Agilent) in a final volume of 50 μL of Herculase buffer 1×. PCR was initiated by a 5 min denaturation at 95° C. followed by 30 cycles of 30 sec denaturation at 95° C., 30 sec annealing at 48° C. and 20 sec elongation at 72° C. This was followed by a 3 min elongation at 72° C. PCR products were column-purified using nucleospin extract II kit (Macherey-Nalgen), recovered in 40 μL H 2 0 and digested by 10 U of either BbvI or SfaNI (NEB), in NEB 2 and 3 buffers, respectively, for 2 hours at 37° C. Digested PCR products were then column-purified using the nucleospin extract II kit (Macherey-Nalgen), recovered in 40 μL H 2 0 and quantified using a nanodrop device (Thermo scientific). 2 μg of purified digested PCR products were typically obtained with this process.
[0321] Immobilisation of TALE Polynucleotidic Building Blocks on Streptavidin Coated Solid Phase
[0322] Two types of streptavidin coated solid phases were used for TALE repeat polynucleotides assembly. These are streptavidin coated magnetic beads (Ademtech) and Streptavidin coated plates (Thermo Scientific). Below are described the methods to immobilize biotinylated DNA on both solid phases.
[0323] Streptavidin Coated Magnetic Beads
[0324] To prepare the streptavidin coated magnetic beads for TALE repeat polynucleotides assembly, 10 μL of streptavidin magnetic beads (Ademtech, Masterbeads streptavidin, 500 nm, ref #03150) were added to 90 μL PBS 1×, pH7.5 (buffer A) in a 1.5 mL tube (Eppendorff, low binding, DNAase and RNAase free). The mixture was washed 3 times with 100 μL buffer A using the magnet provided by the manufacturer (ref #20105). Beads were then resuspended by pipetting up and down 3 times (off magnet) with 50 μL of biotinylated SfaNI digested di repeat module (prediluted with buffer A to a suitable concentration, see below) and incubated for 30 min at room temperature. The mixture was then placed onto the magnet to remove the supernatant, beads were washed 2 times with 100 μL of PBS 1×, 1M NaCL, pH7.5 (buffer B) to remove nonspecific binding complexes, and then resuspended in 50 μL of buffer A. At this step, the first biotinylated di repeat module was bound to the beads and the system was ready for subsequent additions of TALE repeat modules.
[0325] Streptavidin Coated Plates
[0326] To prepare the streptavidin coated plate for TALE repeat polynucleotides assembly, each streptavidin coated well was washed 3 times with 150 μL of buffer A and then incubated 1 hour in the presence of 100 μL of the SfaNI digested biotinylated first polynucleotidic building block (prediluted to a suitable concentration, see below). Wells were then washed 2 times with 150 μL of buffer B to remove nonspecific binding complexes and finally equilibrated in 150 μL of buffer A. At this step, the first biotinylated polynucleotidic building block was bound to the wells and the system was ready for subsequent additions of TALE repeat polynucleotidic modules.
[0327] Assembly of TALE Repeats Polynucleotidic Modules Using a Series of Consecutive Digestion and Ligation Steps
[0328] Here, for the sake of clarity, we only described experimental conditions used with streptavidin coated magnetic beads. The experimental conditions used with streptavidin coated plate are essentially the same as the ones described below except for the reaction volume (100 μL instead of 50 μL).
[0329] To assemble the 15.5 TALE repeats polynucleotide described in this example (SADE2.3), the 8 first TALE repeats polynucleotide and the 7.5 last TALE repeats polynucleotide (named respectively 8 TALE repeats left, 7.5 TALE repeat right in the FIG. 6 ) were first assembled separately and then ligated together according to the method described in FIG. 6 . Concerning the assembly of the 8 TALE repeats left, 100 ng of biotinylated SfaNI digested first TALE di repeat module, Rvd_b3-biot, was first immobilized according to the protocol described above. Buffer A was discarded from the beads and ligation with the second TALE di repeat module, the Bbv I digested Rvd_b7, was performed by addition of the ligation mixture. This ligation mixture contained 100 ng of Rvd_b7, 1 μL of T4 DNA ligase (3U, Promega) in a final volume of 50 μL of Rapid ligation buffer 1× (Promega). Ligation was allowed to proceed for 1 hour at room temperature and was then stopped by pipetting the ligation mixture out of the beads. Beads were then washed 2 times with 150 μL of buffer B to remove byproducts and enzymes and finally reequilibrated with 150 μL of buffer A. Supernatant was then discarded from the beads and ligation product containing the TALE quadri repeats polynucleotide Rvd_b3-Rvd_b7 was digested by SfaNI. SfaNI digestion mixture contained 1 U SfaNI in a final volume of 50 μL of NEB 3 1×. Digestion was allowed to proceed for 1 hour at 37° C. and was then stopped by pipetting the digestion mixture out of the beads. Beads were then washed 2 times with 150 μL of buffer B to remove byproducts and enzymes and finally reequilibrated with 150 μL of buffer A. Two additional consecutive digestion and ligation steps were performed with Rvd_b11 to get the complete 8 TALE repeats left polynucleotide. The 7.5 TALE repeats right polynucleotide was assembled in parallel with the same overall protocol but with higher quantities of building blocks, restriction enzymes and ligase. Indeed we used 300 ng of biotinylated first TALE di repeats module, Rvd_b6-biot and 300 ng of TALE di repeats modules (Rvd_b7, Rvd_b12 and Rvd_T4) for the subsequent restriction/ligation steps. Building block quantities and enzyme units used for TALE repeat assembly are summarized in Table 4.
[0330] To obtain the 15.5 final TALE repeats polynucleotide, the 7.5 TALE repeats right polynucleotides were first stripped off the beads by BbvI digestion. BbvI digestion mixture contained 3U of BbvI in a final volume of 50 μL of NEB 2 1×. Digestion was allowed to proceed for 1 hour at 37° C. Supernatant was then recovered, column purified using nucleospin extract II kit (Macherey-Nalgen) and finally recovered in a final volume of 35 μL H 2 0. In parallel, the 8 TALE repeats left polynucleotides were digested by SfaNI according to the protocol described above. Beads containing the SfaNI digested 8 TALE repeats left polynucleotides were washed 2 times with 150 μL of buffer B to remove byproducts and enzymes and finally reequilibrated with 150 μL of buffer A. Supernatant was then discarded and a ligation mixture containing 30 μL of BbvI digested 7.5 TALE repeats right polynucleotides, 1 μL of T4 DNA Ligase (3U), in a final volume of 50 μL of Rapid ligation buffer 1× (Promega) was added to the beads. Ligation of TALE repeats Left and Right polynucleotides was allowed to proceed for 1 hour at room temperature and was then stopped by pipetting the ligation mixture out of the beads. Beads were then washed 2 times with 150 μL of buffer B to remove byproducts and enzymes and finally reequilibrated with 150 μL of buffer A. At this stage of the process, the 15.5 TALE repeats polynucleotides were assembled, but still attached to the streptavidin coated beads.
[0000]
TABLE 4
Building block quantities and enzyme
units used for TALE repeat assembly
8 TALE repeats left assembly
Di
repeat module name
Rvd_b3-biot
Rvd_b7
Rvd_b11
Rvd_b11
Quantity (ng)
100
100
100
100
Ligase (U)
3
3
3
—
SfaNI (U)
—
1
1
1
7.5 TALE repeats right assembly
Di
repeat module name
Rvd_b6-biot
Rvd_b7
Rvd_b12
Rvd_T4
Quantity (ng)
300
300
300
300
Ligase (U)
9
9
9
—
SfaNI (U)
—
3
3
—
BbvI
—
—
—
3
[0331] Recovery of TALE Repeats Fragment and Subcloning into pAPG10 Shuttle Vector
[0332] Recovery of the 15.5 TALE repeats polynucleotides was performed by SfiI digestion. SfiI digestion mixture containing 20 U SfiI and BSA 1× in a final volume of 100 μL of NEB buffer 4 1×, was added to the beads. The reaction was allowed to proceed for 1 hour at 50° C. Supernatant was recovered, column purified using nucleospin extract II kit (Macherey-Nalgen) and finally recovered in a final volume of 35 μL H 2 0. To subclone the 15.5 TALE repeats polynucleotides into pAPG10, 5 μL of the purified solution was added to 5 μL of Rapid ligation buffer 2× (Promega), 1 μL of SfiI digested pAPG10 cut vector (20 ng) and 1 μL of T4 DNA ligase (3U, Promega). Ligation was allowed to proceed for 1 hour at room temperature. 5 μL of ligated products were then used to transform 30 μL of DH5α chimio competent cells (Invitrogen) according to the manufacturer protocol.
[0333] 1d—Assembly of TALE Repeats Polynucleotide SADE2.3 (15.5 TALE Repeats Polynucleotide) Using Streptavidin Coated Magnetic Beads as Solid Phase.
[0334] The method described above was used to generate a 15.5 TALE repeats polynucleotide that binds to the SADE2.3 homodimeric target sequence (SEQ ID NO: 3) ( FIG. 6A ). SADE2.3 is divided into 3 parts, the SADE2.3 target (SEQ ID NO: 34), a 21 bp spacer (SEQ ID NO: 35) and a second SADE2.3 target (SEQ ID NO: 34) ( FIG. 6A , green, red and green respectively). To assemble the 15.5 TALE repeats polynucleotide, SADE2.3 target was first divided into two parts named 8 TALE repeats left and 7.5 TALE repeats right, translated into RVD motif sequences and then into TALE polynucleotidic building blocks comprising di repeats modules sequences. TALE Di repeats polynucleotidic modules were then assembled in parallel to generate 8 TALE repeats left and 7.5 TALE repeats right according to the method described above (see section 1a). The TALE repeats left and right were then digested by SfaNI and BbvI respectively and eventually coupled together to generate the final 15.5 TALE repeats polynucleotide. This final fragment was then stripped off the solid phase by SfiI digestion, recovered by column purification, subcloned into pAPG10 and transformed into E. coli . Transformation resulted in the growth of more than 1000 colonies on LB plate. Among 24 screened colonies, we obtained around 50% of 15.5 TALE repeats polynucleotides ( FIG. 6B ). This success rate was independent on the solid phase used for the assembly (data not shown).
Example 3
Solid Phase Assembly of TALE Repeat Polynucleotidic Modules Using a Linear Sequential Process
[0335] 1a—Method for Linear Sequential Assembly of TALE Repeat Polynucleotidic Modules Using a Streptavidin Coated Well and Streptavidin Coated Magnetic Beads as Solid Phases.
[0336] Below is described an example of 15.5 TALE repeats polynucleotide assembly using building blocks encoding TALE di repeats modules and streptavidin coated plates as a solid phase. This method includes the following steps:
a—Choose a shuttle plasmid containing the first building block encoding the desire TALE di repeat module (polynucleotidicmodule A), PCR amplify it with TAL_Shuttle_Bio_Forward primer and TAL_Shuttle_Reverse primer (SEQ ID NO: 29 and 30 respectively), SfaNI digestion of the PCR product and purification on column, leading to polynucleotide module A. b—Choose the shuttle containing the next building blocks needed for assembly (respectively encoding TALE di repeat polynucleotidic modules B, C, D, E, F, G), PCR amplify them with TAL_Shuttle_short_Forward primer and TAL_Shuttle_Reverse primer (SEQ ID NO 31 and 30 respectively), digest them with BbvI and purify them on column. Alternatively, these fragments can be extracted from pAPG10 using SfiI according to the method described in example 1. c—Immobilisation of the biotinylated first building block on a streptavidin coated well. d—Ligation of polynucleotidic modules A and B followed by a washing step with a saline buffer to remove secondary reaction products, ligation buffer and enzymes. e—SfaNI digestion of polynucleotide AB followed by a washing step with a saline buffer to remove secondary reaction products, restriction buffer and enzymes. f—Repeat steps d to e with BbvI digested polynucleotidic modules C, D, E, F, G and H g—SfiI digestion of ABCDEFGH polynucleotide. i—Recovery of ABCDEFGH polynucleotide by column purification, subcloning into SfiI digested pAPG10 and transformation into DH5α E. coli. l—Colony PCR screen for fragment having the size of an 15.5 TALE repeat polynucleotide.
[0346] 1b—Material and Methods
[0347] PCR Amplification and Digestion of TALE Building Blocks
[0348] The first TALE building block of TALE repeat polynucleotide was amplified from pAPG10 using TAL_Shuttle_Bio_Forward and TAL_Shuttle_Reverse primers (SEQ ID NO: 29 and 30 respectively). TAL_Shuttle_Bio_Forward contains a biotinylated moiety that binds specifically to the streptavidin coated solid phase. TALE repeat polynucleotidic modules or TALE repeat polynucleotides used for subsequent assembly could be obtained via the method described in section 1a, and could be also obtained by PCR using TAL_Shuttle_short_Forward and TAL_Shuttle_Reverse primers (SEQ ID NO 31 and 30). Conditions for amplification were 5 ng of pAPG10 containing mono or multiple TALE repeat polynucleotidic modules, 250 μM dNTP mix, 200 nM of each oligonucleotide, 1 μL of Herculase II Fusion DNA Polymerase (Agilent) in a final volume of 50 μL of Herculase buffer 1×. PCR was initiated by a 5 min denaturation at 95° C. followed by 30 cycles of 30 sec denaturation at 95° C., 30 sec annealing at 48° C. and 20 sec elongation at 72° C. This was followed by a 3 min elongation at 72° C. PCR products were column purified using nucleospin extract II kit (Macherey-Nalgen), recovered in 40 μL H 2 0 and digested by 10 U of either BbvI or SfaNI (NEB), in NEB 2 and 3 buffers respectively, for 2 hours at 37° C. Digested PCR products were then column purified using the nucleospin extract II kit (Macherey-Nalgen), recovered in 40 μl H 2 O and quantified using a nanodrop device (Thermo scientific). 2 μg of purified digested PCR products were typically obtained with this process.
[0349] Immobilisation of TALE Polynucleotidic Building Blocks on Streptavidin Coated Solid Phase
[0350] Two types of streptavidin coated solid phases were used for TALE repeat polynucleotides assembly. These are streptavidin coated magnetic beads (Ademtech) and Streptavidin coated plates (Thermo Scientific). Below are described the methods to immobilize biotinylated DNA on both solid phases.
[0351] Streptavidin Coated Magnetic Beads
[0352] To prepare the streptavidin coated magnetic beads for TALE repeat polynucleotides assembly, 10 μL of streptavidin magnetic beads (Ademtech, Masterbeads streptavidin, 500 nm, ref #03150) were added to 90 μL PBS 1×, pH7.5 (buffer A) in a 1.5 mL tube (Eppendorff, low binding, DNAase and RNAase free). The mixture was washed 3 times with 100 μL buffer A using the magnet provided by the manufacturer (ref #20105). Beads were then resuspended by pipetting up and down 3 times (off magnet) with 50 μL of biotinylated SfaNI digested di repeat module (prediluted with buffer A to a suitable concentration, see below) and incubated for 30 min at room temperature. The mixture was then placed onto the magnet to remove the supernatant, beads were washed 2 times with 100 μL of PBS 1×, 1M NaCL, pH7.5 (buffer B) to remove nonspecific binding complexes, and then resuspended in 50 μL of buffer A. At this step, the first biotinylated di repeat module was bound to the beads and the system was ready for subsequent additions of TALE repeat modules.
[0353] Streptavidin Coated Plates
[0354] To prepare the streptavidin coated plate for TALE repeat polynucleotides assembly, each streptavidin coated well was washed 3 times with 150 μL of buffer A and then incubated 1 hour in the presence of 100 μL of the SfaNI digested biotinylated first polynucleotidic building block (prediluted to a suitable concentration, see below). Wells were then washed 2 times with 150 μL of buffer B to remove nonspecific binding complexes and finally equilibrated in 150 μL of buffer A. At this step, the first biotinylated polynucleotidic building block encoding di repeat module was bound to the wells and the system was ready for subsequent additions of TALE repeat polynucleotidic modules.
[0355] Assembly of TALE Polynucleotidic Repeats Modules Using a Series of Consecutive Digestion and Ligation Steps
[0356] Here, we only described experimental conditions used with streptavidin coated magnetic beads. The experimental conditions used with streptavidin coated plate are essentially the same as the ones described below except for the reaction volume (100 μL instead of 50 μL).
[0357] The 15.5 TALE repeats polynucleotide described in this example (SADE2.3) was assembled sequentially in a linear fashion. To do so, 100 ng of biotinylated SfaNI digested first TALE di repeat module, Rvd_b3-biot, was first immobilized on magnetic beads according to the protocol described above. Buffer A was discarded from the beads and ligation with the second TALE di repeat module, the Bbv I digested Rvd_b7, was performed by addition of the ligation mixture. This ligation mixture contained 100 ng of Rvd_b7, 1 μL of T4 DNA ligase (3U, Promega) in a final volume of 50 μL of Rapid ligation buffer 1× (Promega). Ligation was allowed to proceed for 1 hour at room temperature and was then stopped by pipetting the ligation mixture out of the beads. Beads were then washed 2 times with 150 μL of buffer B to remove byproducts and enzymes and finally reequilibrated with 150 μL of buffer A. Supernatant was then discarded from the beads and ligation product containing the TALE quadri repeats polynucleotide Rvd_b3-Rvd_b7 was digested by SfaNI. SfaNI digestion mixture contained 1 U SfaNI in a final volume of 50 μL of NEB 3 1×. Digestion was allowed to proceed for 1 hour at 37° C. and was then stopped by pipetting the digestion mixture out of the beads. Beads were then washed 2 times with 150 μL of buffer B to remove byproducts and enzymes and finally reequilibrated with 150 μL of buffer A. Six additional digestion/ligation steps were performed with Rvd_b11, Rvd_b6, Rvd_b7, Rvd_b12, and Rvd_T4 to get the complete 15.5 TALE repeats polynucleotide. Building block quantities and enzyme units used for repeat assembly are summarized in Table 4.
[0358] At this stage of the process, the 15.5 TALE repeats polynucleotides were assembled, but still attached to the streptavidin coated beads.
[0359] Recovery of TALE Repeats Fragment and Subcloning into pAPG10 Shuttle Vector
[0360] Recovery of the 15.5 TALE repeats polynucleotides was performed by SfiI digestion. SfiI digestion mixture containing 20 U SfiI and BSA 1× in a final volume of 100 μL of NEB buffer 4 1×, was added to the beads. The reaction was allowed to proceed for 1 hour at 50° C. Supernatant was recovered, column purified using nucleospin extract II kit (Macherey-Nalgen) and finally recovered in a final volume of 35 μL H 2 0. To subclone the 15.5 TALE repeats polynucleotides into pAPG10, 5 μL of the purified solution was added to 5 μL of Rapid ligation buffer 2× (Promega), 1 μL of SfiI digested pAPG10 cut vector (20 ng) and 1 μL of T4 DNA ligase (3U, Promega). Ligation was allowed to proceed for 1 hour at room temperature. 5 μL of ligated products were then used to transform 30 μL of DH5α chimio competent cells (Invitrogen) according to the manufacturer protocol.
[0361] 1d—Assembly of TALE Repeats Polynucleotide SADE2.3 (15.5 TALE Repeats Polynucleotide) Using Streptavidin Coated Plates or Streptavidin Coated Magnetic Beads as a Solid Phase.
[0362] The method described above was used to generate a 15.5 TALE repeats TALE repeats polynucleotide that recognizes the homodimeric target SADE2.3 (SEQ ID NO: 3) ( FIG. 7A ). SADE2.3 is divided into 3 parts, the SADE2.3 target (SEQ ID NO: 34), a 21 bp spacer (SEQ ID NO: 35) and a second SADE2.3 target (SEQ ID NO: 34) ( FIG. 7A , green, red and green respectively). To assemble TALE repeats polynucleotide targeting SADE2.3, SADE2.3 target was first translated into a RVD motif sequence and then into TALE polynucleotidic building blocks comprising di repeats modules sequence. TALE di repeats polynucleotidic modules were then assembled sequentially to generate a 15.5 TALE repeats polynucleotide according to the method described in section 1a. The 15.5 TALE repeats polynucleotide was subcloned into pAPG10 and transformed into E. coli . Transformation resulted in the growth of more than 1000 colonies on LB plate. Variable success rates for the assembly of 15.5 TALE repeats polynucleotides were obtained depending on thesolid phase used for assembly (streptavidin coated well or streptavidin coated magnetic beads). Around 20% of 15.5 TALE repeats polynucleotides were obtained with streptavidin coated magnetic beads ( FIG. 7B ) and 50% of 15.5 TALE repeats polynucleotide were obtained with streptavidin coated well ( FIG. 7C )
[0363] 1e—Assembly of AvrBs3 TALE repeats polynucleotides variant (17 TALE repeats polynucleotide) using streptavidin coated plates as a solid phase.
[0364] The method described above (section 1a) was used to generate a 17 TALE repeats polynucleotide that recognizes the homodimeric target AvrBs3 (SEQ ID NO: 36) ( FIG. 8A ). AvrBs3 target is divided into 3 parts, the AvrBs3.3 target (SEQ ID NO: 37), a 15 bp spacer (SEQ ID NO: 38) and a second AvrBs3.3 target (SEQ ID NO: 37) ( FIG. 8A , green, red and green respectively). To assemble TALE repeats polynucleotides targeting AvrBs3, AvrBs3 target was first translated into a RVD motif sequence and then into TALE polynucleotidic building blocks comprising di and tri repeats modules sequence. TALE tri repeats polynucleotidic modules were then sequentially assembled to generate a 17 TALE repeats polynucleotide according to the method described in section 1a. The 17 TALE repeats polynucleotide was subcloned into pAPG10 and transformed into E. coli . Transformation resulted in the growth of more than 1000 colonies on LB plate. Among 20 PCR screened colonies, around 40% of AvrBs3 17 TALE repeats polynucleotides ( FIG. 8B ) were obtained.
Example 4
Improvement of TALE Repeat Polynucleotidic Modules Assembly Success Rate by Dual Immobilization Procedures
[0365] As illustrated in FIG. 9 , below is described a method to increase the success rate of TALE repeat polynucleotidic modules assembly. This method consists in a sequential assembly of TALE polynucleotidic modules comprised in polynucleotidic building blocks, assisted by two different solid phases. The first one is coated by streptavidin and is specific for biotinylated DNA fragments whereas the second one is coated by digoxigenin specific antibodies and is specific for digoxigeninylated DNA fragments. Using a combination of two different solid phases enables enrichment of the proper nascent TALE repeat polynucleotides and depletion of improper ones at each assembly step.
[0366] A method to assemble TALE polynucleotidic modules comprised in polynucleotidic building blocks was designed according to the following protocol. It should be noted that each TALE building block may contain multiple TALE repeat modules obtained from previous assemblies. Below is described an assembly example of 3 TALE polynucleotidic modules comprised in building blocks using the dual immobilization procedure. Complete assembly of a TALE DNA binding domain is not described here.
a—Immobilization of the first desired SfaNI digested biotinylated building block on a streptavidin coated well (building block A) b—Ligation of polynucleotide module A with a second BbvI digested digoxigeninylated building block c—Wash out the unbound polynucleotidic module B with a washing buffer d—BbvI digestion of polynucleotide AB, recovery of supernatant and immobilization of digested polynucleotide onto a new well coated by digoxigenin specific antibodies e—Ligation of BbvI digested polynucleotide AB with a third SfaNI biotinylated building block.
Example 5
Method for Assembly of Polynucleotidic Building Blocks by Reverse Elongation
Example 5a
Preparation of Building Blocks Repeat for Assembly by Reverse Elongation
[0372] Using reverse elongation on solid phases enables enrichment of the proper nascent TALE repeat polynucleotides and permit high throughput synthesis (HTS) of these molecules. A method to assemble TALE polynucleotidic modules comprised in polynucleotidic building blocks was designed according to the following protocol. Each TALE building block may contain multiple TALE repeat modules obtained from previous assemblies.
[0373] Below is described how to prepare TALE building blocks using a reverse elongation procedure.
[0374] A TALE building block of TALE repeat polynucleotide was amplified from pAPG10 using TAL_Shuttle_Bio_Forward and TAL_Shuttle_Reverse short primer (SEQ ID NO: 29 and 39, respectively). TAL_Shuttle_Bio_Forward contains a biotinylated moiety that binds specifically to the streptavidin coated solid phase. The last TALE repeat polynucleotidic modules or TALE repeat polynucleotides used for subsequent assembly could be obtained via the method described in example 1, section 1a, and could be also obtained by PCR using TAL_Shuttle_short_Forward and TAL_Shuttle_Reverse primers (SEQ ID NO 31 and 30). Conditions for amplification were 5 ng of pAPG10 containing mono or multiple TALE repeat polynucleotidic modules, 250 μM dNTP mix, 200 nM of each oligonucleotide, 1 μL of Herculase II Fusion DNA Polymerase (Agilent) in a final volume of 50 μL of Herculase buffer 1×. PCR was initiated by a 5 minutes denaturation at 95° C. followed by 30 cycles of 30 sec. denaturation at 95° C., 30 sec. annealing at 48° C. and 30-45 sec. elongation at 72° C. This was followed by a 3 min. elongation at 72° C. PCR products were column purified using nucleospin extract II kit (Macherey-Nalgen), recovered in 40 μL H 2 O and digested by 10 U of either BbvI or SfaNI (NEB), in Fast digest buffers for 1 hour at 37° C. Digested PCR products were then column purified using the nucleospin extract II kit (Macherey-Nalgen), recovered in 40 μL H 2 O and quantified using a nanodrop device (Thermo scientific). 1-2 μg of purified digested PCR products were typically obtained with this process by PCR.
Example 5b
TALE Repeat Polynucleotidic Modules Assembly by Reverse Elongation
[0375] As illustrated in FIG. 10 , below is described a method to assemble TALE repeat polynucleotidic modules. This method consists in a sequential assembly of TALE polynucleotidic modules comprised in polynucleotidic building blocks, assisted by a solid phase. The solid phase is coated by streptavidin and is specific for biotinylated DNA fragments prepared as described in examples 2 and 3. Below is described an assembly example of TALE DNA binding domain using a reverse elongation procedure.
[0376] The following example is given for the synthesis of a 13.5 blocks polynucleotidic module, using tri-modules (A, B, C, D) and a terminal di-module (1.5 RVDs) (E), but can be adapted to the synthesis of any repeat polynucleotides using various starting modules (Prior to any assembly of polynucleotidic modules, the solid surfaces (streptavidin-coated wells) are prepared by two washing steps with 200 μl of PBS 1×):
1—Immobilization of the desired SfaNI digested biotinylated building block on a streptavidin-coated well (building block D, 300 ng in PBS 1×, 100 μl final volume) 1 hour at room temperature. 2—Ligation of BbvI digested polynucleotide terminal module E (270 ng) in 1× ligation buffer containing 4 μl of T4 DNA ligase in a final volume of 100 μl. After 30 minutes incubation at room temperature, 0.5 mM final concentration of ATP was added and the reaction was set for an additional 30 minutes at room temperature. 3—Wash out the unligated polynucleotidic terminal module E with three times 150 μl PBS 1×, NaCl 1M, followed by two times 170 μl PBS 1×. 4—Release of nascent chain (DE) from the solid surface by addition of BbvI (0.5 μl Fast digest BbvI, fermentas #FD2074) in 1× Fast digestion buffer (Fermentas) in a final volume of 100 μl, followed by thermal inactivation (65° C., 20 minutes) of the restriction enzyme. The reaction was subsequently cooled down to room temperature. 5—Immobilization of the desired SfaNI digested biotinylated building block on a streptavidin coated well (building block C, 250 ng in PBS 1×, 100 μl final volume) 1 hour at room temperature. 6—Ligation of the nascent chain (DE) to the immobilized block C by addition of the reaction mixture (step 4) complemented with 1× ligation buffer and 4 μl of T4 DNA ligase to the immobilized block C (step 5). After 30 minutes incubation at room temperature, 0.5 mM final concentration of ATP was added and the reaction was set for an additional 30 minutes at room temperature. 7—Wash out the unligated polynucleotidic module DE with three times 150 μl PBS 1×, NaCl 1M, followed by two times 170 μl PBS 1×. 8—Release of nascent chain (CDE) from the solid surface by addition of BbvI (0.5 μl Fast digest BbvI, fermentas #FD2074) in 1× Fast digestion buffer (Fermentas) in a final volume of 100 μl, followed by thermal inactivation (65° C., 20 minutes) of the restriction enzyme. The reaction was subsequently cooled down to room temperature. 9—Immobilization of the desired SfaNI digested biotinylated building block on a streptavidin-coated well (building block B, 200 ng in PBS 1×, 100 μl final volume) 1 hour at room temperature. 10—Ligation of the nascent chain (CDE) to the immobilized block B by addition of the reaction mixture (step 8) complemented with 1× ligation buffer and 4 μl of T4 DNA ligase to the immobilized block B (step 9). After 30 minutes incubation at room temperature, 0.5 mM final concentration of ATP was added and the reaction was set for an additional 30 minutes at room temperature. 11—Wash out the unligated polynucleotidic module CDE with three times 150 μl PBS 1×, NaCl 1M, followed by two times 170 μl PBS 1× 12—Release of nascent chain (BCDE) from the solid surface by addition of BbvI (0.5 μl Fast digest BbvI, fermentas #FD2074) in 1× Fast digestion buffer (Fermentas) in a final volume of 100 followed by thermal inactivation (65° C., 20 minutes) of the restriction enzyme. The reaction was subsequently cooled down to room temperature. 13—Immobilization of the desired SfaNI digested biotinylated building block on a streptavidin coated well (building block A, 150 ng in PBS 1×, 100 μl final volume) 1 hour at room temperature. 14—Ligation of the nascent chain (BCDE) to the immobilized block A by addition of the reaction mixture (step 12) complemented with 1× ligation buffer and 4 μl of T4 DNA ligase to the immobilized block A (step 13). After 30 minutes incubation at room temperature, 0.5 mM final concentration of ATP was added and the reaction was set for an additional 30 minutes at room temperature. 15—Wash out the unligated polynucleotidic module BCDE with three times 150 μl PBS 1×, NaCl 1M, followed by two times 170 μl PBS 1×. 16—Release of the synthesized chain (ABCDE) with either SfiI to allow subcloning in the shuttle (pAPG10) plasmid or by sequential SfaNI, wash, BbvI digestions to allow subcloning in plasmids already containing a TALEN scaffold (e.g. pCLS7183, SEQ ID NO: 20) is followed by transformation in E. coli according to standard molecular biology procedures.
[0393] It is understood that washing steps can be done respectively after a given immobilization step of a polynucleotides modules or blocks, according to the state of the art; as a non-limiting example, three washing steps of an appropriate volume of saline buffer, such as PBS, can be added after a given immobilization step.
[0394] Analyses by PCR screening ( FIG. 11 ) reveal a frequency compatible with high throughput synthesis procedures.
[0395] In addition the following steps 17, 18 and 19 can be added after steps 1, 5, 9 and/or 13 to combine advantages of both, reverse elongation and direct linear sequential synthesis.
17—Ligation of any BbvI digested polynucleotide module X in 1× ligation buffer containing 4 μl of T4 DNA ligase in a final volume of 100 μl. After 30 minutes incubation at room temperature, 0.5 mM final concentration of ATP was added and the reaction was set for an additional 30 minutes at room temperature. 18—Digestion of the bound product using SfaNI (1 μl Fast digest BbvI, fermentas # FD2124) in 1× Fast digestion buffer (Fermentas) in a final volume of 100 μl. 19—Wash out the restriction enzyme and buffer with three times 150 μl PBS 1×, NaCl 1M, followed by two times 170 μl PBS 1×
[0399] The case where steps 17, 18 and 19 are added after steps 5 is represented in FIG. 12 .
Other Embodiments
[0400] It is to be understood that while the invention has been described in conjunction with the detailed description thereof, the foregoing description is intended to illustrate and not limit the scope of the invention, which is defined by the scope of the appended claims. Other aspects, advantages, and modifications are within the scope of the following claims.
LIST OF CITED REFERENCES
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[0418] (TALE) hybrid nuclease with novel DNA binding specificity creates double-strand breaks.” Proc Natl Acad Sci USA 108(6): 2623-8.
Miller, J. C., S. Tan, et al. (2010). “A TALE nuclease architecture for efficient genome editing.” Nat Biotechnol 29(2): 143-8. Morbitzer, R., J. Elsaesser, et al. (2011). “Assembly of custom TALE-type DNA binding domains by modular cloning.” Nucleic Acids Res. Moscou, M. J. and A. J. Bogdanove (2009). “A simple cipher governs DNA recognition by TAL effectors.” Science 326(5959): 1501. Pabo, C. O., E. Peisach, et al. (2001). “Design and selection of novel Cys2His2 zinc finger proteins.” Annu Rev Biochem 70: 313-40. Ramirez, C. L., J. E. Foley, et al. (2008). “Unexpected failure rates for modular assembly of engineered zinc fingers.” Nat Methods 5(5): 374-5. Silva, G., L. Poirot, et al. (2011). “Meganucleases and other tools for targeted genome engineering: perspectives and challenges for gene therapy.” Curr Gene Ther 11(1): 11-27. Smith, J., J. M. Berg, et al. (1999). “A detailed study of the substrate specificity of a chimeric restriction enzyme.” Nucleic Acids Res 27(2): 674-81. Smith, J., M. Bibikova, et al. (2000). “Requirements for double-strand cleavage by chimeric restriction enzymes with zinc finger DNA-recognition domains.” Nucleic Acids Res 28(17): 3361-9. Spear, M. A. (2000). “Efficient DNA subcloning through selective restriction endonuclease digestion.” Biotechniques 28(4): 660-2, 664, 666 passim. Stoddard, B. L. (2005). “Homing endonuclease structure and function.” Q Rev Biophys 38(1): 49-95. Stoddard, B. L. (2011). “Homing endonucleases: from microbial genetic invaders to reagents for targeted DNA modification.” Structure 19(1): 7-15. Urnov, F. D., E. J. Rebar, et al. (2011). “Genome editing with engineered zinc finger nucleases.” Nat Rev Genet. 11(9): 636-46. Weber, E., C. Engler, et al. (2011). “A modular cloning system for standardized assembly of multigene constructs.” PLoS One 6(2): e16765. Zhang, F., L. Cong, et al. (2011). “Efficient construction of sequence-specific TAL effectors for modulating mammalian transcription.” Nat Biotechnol 29(2): 149-53.
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The present invention relates to a method for the assembly and cloning of polynucleotides comprising highly similar polynucleotidic modules, that is highly versatile, does not require intermediate amplification step and can be easily automated for high throughput production of customized polynucleotidic modules.
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FIELD OF THE INVENTION
[0001] The invention relates to a yarn delivery device for delivering a yarn to a yarn consumer location, such as a knitting station of a knitting machine.
BACKGROUND OF THE INVENTION
[0002] Yarn delivery devices are used to draw off the yarn from a yarn supply, for example a bobbin, and to deliver it to a yarn-consuming arrangement, for example at a preset yarn speed, or at a preset yarn tension, or with other preconditions. Such yarn-consuming arrangements can be knitting stations of knitting machines, or other mechanical arrangements. Elastic yarns, inelastic yarns made of natural fibers or synthetic fibers, staple fiber yarns, other yarns or monofilaments are considered to be yarns. Often the yarn consumption location does not consume yarn at a constant rate. For example, such is the case when the yarn consumption location is switched on or off, for example in connection with loop or Jacquard machines. Friction feed wheel units are known for this, wherein the yarn is looped around a rotating drum, but is lifted off the drum at one or several locations. For example, U.S. Pat. No. 2,539,527 discloses a yarn delivery device whose yarn delivery wheel consists of a drum-shaped rod cage. Two hook-shaped spiral springs are arranged in the vicinity of the rod cage, which partially lift the single yarn winding looped around the drum off the rod cage. The looping characteristics of the rod cage change with different yarn tensions because of the deflection of the spiral springs.
[0003] Another yarn delivery device is known from French Patent 964 455. That yarn delivery device has a rotating yarn delivery drum. A yarn is looped several times around the drum. The individual yarn loops created in this way also loop around two pivotably seated pins, which extend next to the yarn delivery drum either parallel or at an acute angle relative to the drum, depending on the pivot position. This allows the pins to be pivoted away from the drum in order to increase the yarn reserve when the downstream located knitting station does not take on yarn. With this device, the looping characteristics also change because of the movement of the pins.
[0004] A yarn delivery device is also known from U.S. R Pat No. 785,168. This device has a rotating cylindrical yarn delivery drum and a yarn lifting element assigned to the drum. The yarn lifting element has a kinked yarn contact surface, with a first section that extends at an acute angle of 15° to 20° relative to the drum surface and a second section that extends parallel to the drum surface. The lower end of the yarn lifting element is forked, with a machine shut-off lever entering into the space between the tines of the fork. Because of the kink between the upper part and lower part of the contact surface, the individual windings looped around the lifting element and the drum have different lengths. Therefore, a strong or a weak yarn pull therefore is not easily propagated evenly through all windings.
[0005] There is often the desire to operate a yarn delivery device in different modes of operation. However, the above-mentioned prior art devices are arranged either as positive feed wheel units with a yarn supply, or as friction feed wheel units. It has also been noticed that the commercially available devices must be adapted to the yarn to be delivered. This is a considerable limitation, and the removal thereof is of primary importance.
OBJECTS AND BRIEF SUMMARY OF THE INVENTION
[0006] In view of the foregoing, it is an object of the invention to create a yarn delivery device which can be employed in as many ways as possible.
[0007] The yarn delivery device of the invention has at least one yarn contact surface in the vicinity of the yarn delivery wheel, over which the windings looping around the yarn delivery wheel can run. For example, a single yarn lifting element is provided for this. Alternatively, two yarn contact surfaces can be provided on two separate yarn lifting elements. However, the basic geometric design of the yarn contact surface(s) of the yarn lifting element and the design of the yarn delivery wheel is common to both yarn delivery devices. The yarn delivery device in accordance with the invention can be employed as a positive feed wheel unit, as well as a friction feed wheel unit.
[0008] The yarn delivery wheel has a yarn inlet area with a means which provides the wound yarn lap with a forward feed. For example, this is achieved by configuring the yarn inlet area as a very steep cone, which makes a continuous transition into the storage area, which in turn can be embodied as a cone with a slight taper. The yarn windings picked up by the rotating yarn delivery wheel are forced between the inlet area and the storage area and therefore displace the wound lap in the axial direction in order to provide space for the yarn windings. This is particularly important for the positive operation in which the yarn does not run over the yarn lifting element. For performing a friction operation, the yarn lifting element permits a limited fictional connection between the yarn and the yarn delivery wheel, so that the yarn delivery device can supply yarn amounts that fluctuate over time with a more or less constant number of revolutions of the yarn delivery wheel. The forward feed of the wound yarn lap on the yarn delivery wheel can be aided by the cone shape of the storage area. An acute angle between the yarn contact surface of the yarn lifting element and the side of the yarn delivery wheel remote from the yarn lifting element can also provide a forward feed of the lap.
[0009] The forward feeding mechanism provided in the inlet area which, as mentioned above, preferably is accomplished by the shaping of the yarn delivery wheel itself, can also be provided by other devices moving the wound yarn lap in the axial direction. For example, the forward feeding mechanism can be a disk arranged in the yarn delivery wheel, which has spokes extending outward through openings in the yarn delivery wheel. If the axis of rotation of the disk is slightly inclined relative to the axis of rotation of the yarn delivery wheel, the spokes of the disk push the wound lap axially forward on one side of the yarn delivery wheel. Moreover, the storage area can consist of two cages running inside each other at an acute angle and causing a forward feed of the yarn.
[0010] Independent of the actual embodiment of the forward feed mechanism, the yarn delivery device can be used with or without the yarn lifting element. If the yarn lifting element is not used, or even removed, the forward feed mechanism causes the formation of an ordered wound lap. The wound lap can have ten to twenty windings, without the windings being placed on top of each other. However, with friction operation at least several windings of the wound yarn lap are conducted over the yarn lifting element and its yarn contact surface. The required forward feed of the lap is provided here partially by the interaction between the yarn lifting element and the yarn delivery wheel. In this case, the axial forward feed force acts on each individual winding, so that a relatively large wound lap with ten to twenty windings (for example fifteen windings) can be placed on the yarn delivery wheel. A friction operation is made possible even with large wound laps of this type, and the placement of individual windings on top of each other (which would interfere with the operation) is prevented. The large wound yarn lap, one or all windings of which are conducted over the yarn lifting element, ensures that the end of a yarn does not run into the goods to be produced if a yarn is broken.
[0011] A run-in interrupter, which detects a yarn break, shuts off the downstream connected machine using the yarn. The yarn reserve on the yarn delivery wheel is sufficient to supply the machine with yarn as it runs down. This applies to the positive operation, as well as to the friction operation. Thus, it is possible to connect a new yarn to the existing yarn end, so that operational interruptions can be swiftly and simply fixed.
[0012] In a preferred configured of the invention, the yarn delivery wheel is embodied in such a way, and the yarn lifting element is arranged in such a way, that each relatively older winding in the wound lap being formed is slightly shorter than the adjoining newer winding. In this way, each individual winding is subjected to the forward feed effect. Depending on the type of yarn and yarn thickness, the reduction of the winding length can be matched by changing the inclined position of the yarn lifting element. In this way it is possible to regulate spacings possibly occurring between the windings.
[0013] The yarn contact surface is preferably designed to be straight, i.e. free of bends or kinks. The yarn cannot change the position of the yarn lifting element. This results in constant feed conditions. Moreover, the yarn lifting element(s) is/are preferably arranged in such a way that less than 240° of each yarn winding of the wound yarn lap is in contact with the yarn delivery wheel (contact angle), i.e. a section greater than 120° of each winding is lifted off the yarn delivery wheel. The entire wound lap rests against the yarn delivery wheel with less than ⅔ of the length of a (cylindrical) wound lap resting completely against the yarn delivery wheel. However, preferably the contact angle is greater than 180°.
[0014] It has been found that the straight contact surface (i.e. configured without kinks) of the yarn lifting element represents a good compromise for all yarns to be conveyed and delivered, in particular in connection with a yarn delivery wheel such as is used with purely positive feed wheel units. A drop in the yarn output tension can occur temporarily that progresses through all of the windings because of the kink free embodiment of the contact surfaces and results in slippage. During this, in case of low yarn tension (loose windings) yarn windings getting on top of each other is prevented.
[0015] It also has been shown that it is possible to process a particularly large spectrum of possible yarns if the distance between the two contact surfaces is approximately 10 mm to 30 mm, in particular 12 mm to 18 mm. This specifically applies in connection with yarn delivery wheels embodied as rod cages or corrugated drums. In this case the distance of the drum advantageously is in the range between 10 mm and 20 mm. The yarn lifting elements can be made of a ceramic material (wear resistance) or wire pins or wire loops (easy to produce). Moreover, the yarn lifting element can be consist of a bent sheet metal part. If the yarn lifting element is made of metal (wire or sheet metal), it is advantageous to provide a wear-reducing coating, for example of a ceramic material.
[0016] Except for the yarn delivery wheel, the yarn delivery device preferably does not have any other yarn conveying mechanisms, such as strips or the like resting against the yarn delivery wheel. Thus, the yarn delivery wheel has an unencumbered outer circumference. This permits controlled slippage between the yarn delivery wheel and the yarn.
[0017] The yarn delivery wheel has a yarn inlet section, which can be tapered. In this sense, tapered means that the diameter of the yarn delivery wheel changes in the area of the yarn inlet section as a function of the axial direction. In this case, the taper can have the shape of a steep circular taper or other curved shapes. The tapering shape enables the generation of a forward feed motion on the yarn delivery wheel by the running up yarn. In this case, the yarn inlet section is preferably configured as a closed surface area or as a rod cage.
[0018] In an advantageous embodiment, the yarn delivery wheel can be provided with a tapering yarn run-off edge. The yarn run-off edge can also be configured as a truncated cone or other tapering shape. The yarn run-off edge allows an oblique yarn draw-off, which is particularly advantageous with yarns causing deposits that contain dressings or sizing, or are very fuzzy.
[0019] A storage area is provided between the inlet section and the yarn run-off edge. The storage area preferably does not have a cylindrical configuration and has a diameter that is less than the diameter of the inlet section and the yarn run-off edge. In this case, the storage area can have a polygonal configuration, so that the yarn windings are only picked up by strip-shaped areas of the yarn delivery wheel. The yarn delivery wheel can be configured as a rod cage, or as a one-piece element, for example as a deep-drawn sheet metal element or as a ceramic element. The contact of the yarn windings in polygonal sections enable the positive delivery without slippage in a particularly effective manner, as well as the slippage-containing conveyance of the yarn. The exterior diameter of the storage area can slightly decrease in the direction of the yarn run-off edge.
[0020] The inlet yarn guidance arrangement of the yarn delivery device is preferably arranged above the storage area, so that the yarn is forced to run into the storage area over the inlet area of the yarn delivery wheel. In this case, the inlet yarn guidance arrangement is preferably rigidly seated, which provides defined yarn inlet conditions.
[0021] In an advantageous embodiment, the outlet yarn guidance arrangement is also rigidly seated and preferably arranged below the storage area. In this case, the outlet yarn guidance arrangement is preferably clearly offset in the axial and radial directions relative to the yarn delivery wheel, so that it is also located below the yarn run-off edge. By means of this, the outgoing yarn can slip over the run-off edge thereby keeping it clean. The rigid, possibly manually adjustable seating of the outlet yarn guidance arrangement provides defined yarn outlet conditions.
[0022] Preferably both yarn guidance arrangements are arranged on same level as the axis of rotation of the yarn delivery wheel. This provides symmetrical operating conditions, whereby the yarn delivery wheel can be driven counterclockwise or clockwise.
[0023] The yarn lifting element can be fixed on the yarn delivery device. However, the yarn lifting element preferably can be manually adjusted. An adjusting device can be provided for setting the inclination of the yarn lifting element relative to the longitudinal axis, or axis of rotation, of the yarn delivery wheel. In the course of this, fine adjustments can be performed for adapting the yarn delivery device to various yarn properties or applications.
[0024] The yarn lifting element additionally can be seated so it can be displaced on a circle, which is concentric relative to the yarn delivery wheel. This potential displacement provides improved handling capabilities without substantially affecting the yarn conveying properties. It can be helpful, particularly where space is limited (for example, if a number of identical yarn delivery devices are mounted on a machine circle of a circular knitting machine) to pivot a support carrying the lifting element laterally to the side of the yarn delivery device for manually placing the yarn on it. Once the yarn has been placed on it, the support can remain in this position, or the support can be pivoted by 90°, for example, so that the lifting element is located underneath the main body or main support of the yarn delivery device and therefore does not require more space. The position is mainly unimportant for the function of the yarn delivery device. This arrangement not only eases operation, but also helps prevent wrong settings.
[0025] The lifting element preferably extends above the storage area in the inlet area, as well as at the run-off edge, of the yarn delivery wheel. This ensures that the straight yarn contact surfaces extend over the entire storage area of the yarn delivery wheel.
[0026] The yarn lifting element is preferably releasably connected to the yarn delivery device. Because of this arrangement, the yarn delivery device can be operated purely as a positive feed wheel unit, if necessary. The yarn lifting element can be offered as an accessory or ancillary part.
[0027] With a yarn delivery device having two lifting elements, it can be advantageous to seat both lifting elements on different supports, which can be adjusted relative to each other. This has the useful advantage particularly in those cases where the lifting elements are set to different radii relative to the axis of rotation of the yarn delivery wheel. There is the option of placing both lifting elements one behind the other in the radial direction, so that only the one on the outside is operational.
[0028] A pulley can be used as the drive mechanism for the yarn delivery wheel. It is also possible to provide the yarn delivery device with an individual electric drive motor, which drives the yarn delivery wheel. For example, the drive motor can be operated corresponding to the yarn demand or controlled by the yarn tension.
BRIEF DESCRIPTION OF THE DRAWINGS
[0029] FIG. 1 , a perspective representation of the yarn delivery device,
[0030] FIG. 2 , a lateral view of the yarn delivery device in FIG. 1 ,
[0031] FIG. 3 , a front view of the yarn delivery device in FIG. 2 ,
[0032] FIG. 4 , a lateral view of a modified embodiment of the yarn delivery device,
[0033] FIG. 5 , a lateral view of a further modified embodiment of the yarn delivery device.
[0034] FIG. 6 , a lateral view of an embodiment of the yarn delivery device with an electrical drive mechanism,
[0035] FIG. 7 , a lateral view of an embodiment of the yarn delivery device with separate lifting elements,
[0036] FIG. 8 , a front view of a further embodiment of a yarn delivery device with separate lifting elements,
[0037] FIG. 9 , a view from above on a lifting element fastened on a support
[0038] FIG. 10 , a view from above on a modified embodiment of a lifting element,
[0039] FIG. 11 , a view from above on lifting elements maintained on separate supports,
[0040] FIG. 12 , the geometric relationships of the yarn delivery device in accordance with FIG. 1 , as well as of an alternative embodiment,
[0041] FIG. 13 , a yarn delivery device with two yarn lifting elements arranged diametrically opposite each other by means of the representation of the geometric relationships, and
[0042] FIG. 14 , the geometric relationships between the yarn delivery wheel and the yarn-lifting device.
DETAILED DESCRIPTION OF THE INVENTION
[0043] An exemplary yarn delivery device 1 according to the invention is illustrated in FIG. 1 The yarn delivery device is used for delivering a yarn 2 (shown in FIG. 2 ) to a knitting station of a knitting machine (not shown) or other yarn consumption station. The yarn delivery device 1 has an elongated base body 3 , for example made of a plastic material, which is equipped at one end with a clamp 4 for fastening the yarn delivery device 1 on a ring-shaped support (machine ring) of a knitting machine. On its opposite end, the base body 3 is provided with a yarn inlet arrangement 5 that includes an inlet eye 7 (made for example of a ceramic material), a knot catcher 8 , a yarn brake 9 and an inlet eye 12 that is immovably maintained on a rigid support 11 , which constitutes a yarn inlet guidance arrangement 13 .
[0044] A shaft is provided that supports one or more pulleys 14 , 15 on its upper end. The pulleys can be coupled, selectively fixed against relative rotation, with the shaft by means of an axially displaceable coupling ring 15 . The shaft is rotatably seated on or in the base body 3 between the yarn inlet guidance arrangement 13 and the clamp 4 . Below the base body 3 , the shaft is connected, fixed against relative rotation, to a yarn delivery wheel 17 , which therefore can be rotatingly driven by the pulleys 14 , 15 . The yarn delivery wheel 17 has an inlet area 18 , which is distinguished in that its diameter relative to the axial direction A of the yarn delivery wheel 17 becomes smaller as it extends from the top toward the bottom. As can be seen, the inlet area 18 consists of a first tapering section with a small opening angle that makes a curved transition into a second tapering section 18 b with a very large opening angle. The tapering section comprises a guide surface 18 a as a forward feed mechanism for the lap 26 . The shaft is substantially vertically oriented. During slippage-free operation (positive operation), a yarn that has not been removed can rotate, sagging toward the bottom, in the manner of a crank, without being wound up backward.
[0045] A storage area 21 , whose horizontal cross section preferably deviates from a circular shape, adjoins the inlet area 18 , which is configured as a closed surface without interruptions. In the illustrated embodiment, the yarn delivery wheel 17 is formed as a one-piece deep-drawn sheet metal element. In this instance, the storage area 21 comprises a cylindrical section 22 , from which ribs 23 protrude. Each of the ribs has a rounded back, against which the yarn 2 rests with individual windings 24 , 25 , as a lap 26 . The windings 24 , 25 lie freely between the individual ribs 23 . Yet looked at as a whole, the yarn delivery wheel 17 is free of openings. The storage area 21 is also closed. The storage area 21 can be slightly tapered toward the bottom.
[0046] Starting at the cylindrical section 22 , the diameter of the yarn delivery wheel increases again until it exceeds the outer diameter of the ribs 23 . A yarn run-off edge 27 starts there and widens in a conical manner. In this case, the yarn run-off edge forms a smooth, closed surface, into which the ribs 23 transition without any shoulders.
[0047] The yarn delivery wheel 17 rotates freely, i.e. it is only in contact with the yarn 2 . No further elements that would touch the yarn delivery wheel 17 or convey the yarn 2 exist.
[0048] A yarn lifting element 28 is arranged adjoining the yarn delivery wheel 17 , which, in accordance with FIGS. 1, 2 and 3 comprises a U-shaped hoop 29 . The hoop is preferably made of wire. The hoop 29 has two legs 31 , 32 , which are parallel to each other ( FIG. 1 ), and which are connected to each other at their lower free ends by means of a strip 23 . The sections of the legs 31 , 32 adjoining the storage area are configured straight, and they extend at an acute angle or parallel the axial direction A defined by the axis of rotation of the yarn delivery wheel 17 . In this way the legs 31 , 32 define yarn contact surfaces 34 , 25 ( FIG. 2 ), over which each winding 24 , 25 , 26 of the yarn 2 extends. The yarn contact surfaces 34 , 35 are arched (for example cylindrically arched), and each is straight in the longitudinal leg direction R over the entire height of the storage area 21 . The lower ends of the legs 31 , 32 are placed slightly radially outward, so that the strip 33 is angled away from the yarn delivery wheel 17 . The location of the bend lies below the storage area so as to prevent the yarn windings, which rest loosely on the yarn drum, from falling down. The legs 31 , 32 are bent or angled outward at their respective upper ends, preferably above the inlet area 18 ( FIG. 3 ). This arrangement entering yarn windings from getting too far toward the top. In this way yarn windings are also prevented from sliding over the upper drum edge and being wound up by the drum shaft. Thus, the upper shoulder of the pins 31 , 32 formed by the bend or angle increases the operational dependability.
[0049] The hoop 29 can be provided with a ceramic coating, in particular at its contact surfaces 34 , 35 .
[0050] The longitudinal leg direction R matches the axial direction of the yarn delivery wheel 17 , or forms an acute angle with it. Because of this, the length of all windings 24 , 25 , 26 is reduced winding by winding from the inlet side toward the outlet side. As illustrated in FIG. 14 , it is important that an acute angle alpha is formed between the yarn contact surface 34 and a generating line M of the storage area located on the opposite side relative to the yarn delivery wheel 17 . In place of the open space between the legs 31 , 32 , a closed surface can also be provided here.
[0051] The two upper ends of the legs 31 , 32 are maintained on a support 36 ( FIGS. 1 and 3 ), which is pivotally seated on the base body 3 of the yarn delivery device 1 , for example around the axis of rotation D extending in the axial direction Ax. The axis of rotation D is vertically arranged. The support 36 has a spring hinge 37 on its outer end, which connects it with the legs 31 , 32 . The spring hinge 37 maintains the legs 31 , 32 in the relaxed state at an acute angle relative to the axis of rotation D. As illustrated in FIG. 3 , an adjustment screw 38 is provided in the close vicinity of the spring hinge 37 . The adjustment screw 38 is supported on the support 36 and provides the option of setting the pivoted position of the hoop 29 in relation to the support 36 .
[0052] The adjustment screw is seated in a threaded bore of a base section 39 , which is connected via the spring hinge 37 with the support 36 , and which furthermore receives the upper ends of the legs 31 , 32 . Alternatively, the adjustment screw can be seated in a threaded bore of the support 36 and be supported on the base section 39 ( FIG. 1 ). The adjustability of the angle of inclination of the hoop 29 allows an adaptation of the forward yarn feed to varying yarn qualities.
[0053] The support 36 is designed in such a way that it maintains the hoop 29 , and therefore the legs 31 , 32 at a distance of approximately 10 mm to 15 mm from the outer circumference of the storage area 21 of the yarn delivery wheel 17 . This arrangement is illustrated in FIG. 12 . The pin distance A, i.e. the distance of the yarn contact surfaces 34 , 35 from each other ( FIG. 12 ) is preferably approximately 15 mm to 20 mm. This corresponds to a yarn delivery wheel diameter of approximately 45 mm and results in the desired angle of wrap, which is greater than 180°, but less than 240°. In any event, the radius of curvature r of the yarn contact surfaces 34 , 35 is less than the distance A.
[0054] An outlet yarn guidance arrangement 41 includes a hoop 41 , as shown in FIGS. 2 and 3 . The hoop 41 is arranged at the side next to the yarn delivery wheel 17 and has a lower horizontal section 43 that guides the yarn 2 and which is maintained laterally below the yarn delivery wheel 17 ( FIG. 3 ). This causes an oblique yarn draw-off. A further hoop 44 and a run-out interrupter 45 , which rests on the yarn 2 between the hoops 42 and 43 , are provided adjoining the outlet yarn guidance arrangement 41 . A run-in interrupter 46 , which monitors the yarn running toward the yarn delivery wheel 17 , can rest on the yarn between the yarn brake 9 and the inlet yarn guidance arrangement 13 .
[0055] The yarn guidance arrangement 41 , the inlet eye 12 , and the axis of rotation D are located on a common level or plane. As a result, the yarn delivery device 1 has no preferred direction of rotation, the yarn delivery wheel 17 can be operated in a clockwise, as well as in a counterclockwise direction.
[0056] The yarn delivery device 1 so far described operates as follows:
[0057] During operation, the yarn delivery wheel 17 is driven for rotation by a belt that runs over the pulley 14 . The yarn 2 is looped around the yarn delivery wheel 17 as shown in FIG. 2 . The windings 24 , 25 , 26 run over the yarn lifting element 28 . In this case, the number of revolutions of the yarn delivery wheel 17 is such that the circumferential speed of the yarn delivery wheel is slightly greater than the desired maximum yarn speed. The windings 24 , 25 , 26 loop around the yarn delivery wheel over a large portion of its circumference, but are raised off the yarn delivery wheel by the yarn lifting element 28 . This reduces the frictional action between the yarn 2 and the yarn delivery wheel 17 , with the friction still being strong enough so that in the normal case the yarn 2 is delivered with only slight slippage. In this case the yarn has a circumferential speed which is 10% less than the circumferential speed of the delivery wheel 17 .
[0058] If the yarn consumption station temporarily requires less yarn than is delivered by the yarn delivery device 1 , the required yarn speed clearly falls below the circumferential speed of the yarn delivery wheel 17 . In such a case, the yarn tension between the yarn delivery wheel 17 and the yarn consumption station is reduced. The lifting device 28 acts in a slightly braking manner on the yarn and prevents the yarn from being conveyed at full speed. The lap built up from the windings 24 , 25 , 26 is somewhat loosened, so that the conveying speed is reduced to such an extent that the yarn is delivered with slippage and in accordance with the requirements. The reduced frictional action allows the slippage of the windings 24 , 25 , 26 without a movement or adjustment of the yarn lifting element 28 , so that the yarn 2 generally trails the yarn delivery wheel 17 . The yarn runs clearly slower than would correspond to the circumferential speed of the yarn delivery wheel 17 . This is aided in particular by the ribbed structure of the surface of the storage area 21 .
[0059] The yarn lifting element 28 is rigidly seated by means of the structure of the displacement mechanism, represented in FIG. 3 and formed by the adjustment screw 38 and the spring hinge 37 . The adjustment screw 38 is supported between the yarn delivery wheel 17 and the hoop 29 is supported between the support 36 and the base section 39 , while the spring hinge 37 is located radially outward. Therefore, an increased yarn tension cannot cause the hoop 29 to pivot against the yarn delivery wheel 17 .
[0060] The support 36 is preferably configured to be removable. In such a case, the yarn delivery device can be operated purely as a positive feed wheel unit without slippage effect or, as described above, as a friction feed wheel unit, wherein the knitting station temporarily accepts less yarn in case of a reduced yarn tension. It is also possible to provide the support 36 with a hinge or a joint, for swiveling or pivoting the yarn lifting element 28 into a rest position where the yarn lifting element performs no function. Snap-in or other arresting mechanisms can be provided for maintaining the yarn lifting element either in the working position or the rest position.
[0061] It is also possible to employ the yarn delivery device 1 in both ways in that the windings 24 , 25 , 26 are selectively placed on or not placed on the yarn lifting element 28 . Moreover, the yarn lifting element 28 can be designed to be exchangeable, for example by making different hoops 29 available for different yarns. However, it has been found that all tested yarns within a wide spectrum can run over the same hoop 29 if the aforementioned geometric conditions are observed.
[0062] A modified embodiment of the yarn delivery device 1 is illustrated in FIG. 4 . Except for the yarn delivery wheel 17 , the FIG. 4 embodiment has the same elements as the above described yarn delivery device 1 (FIGS. 1 to 3 ), so that, based on the use of identical reference symbols, reference is made to the above description. In contrast to the above described yarn delivery wheel 17 , the yarn delivery wheel 17 in FIG. 4 has the basic structure of a rod cage. The rod cage is formed by a plurality of straight rods 48 , which replace the ribs 23 and together form a cylindrical cage, or a very slightly tapering cage. The rods 48 are inserted into an end disk 49 , whose tapering outer surface constitutes the yarn run-off edge 27 . Openings 51 are formed in the tapering outer surface, into which the rods 48 are inserted. The upper ends of the rods 48 furthermore are maintained in an upper end disk 52 , which forms the inlet area 18 .
[0063] A further embodiment of the yarn delivery device 1 is shown in FIG. 5 . The FIG. 5 embodiment mainly corresponds to the embodiment shown in FIGS. 1 to 3 and only differs therefrom in the design of the yarn run-off edge 27 of the yarn delivery wheel 17 . The yarn run-off edge 27 is designed as a straight truncated cone, i.e. the radius of the yarn run-off edge 27 increases linearly from top to bottom. Otherwise the description of its structure and function provided in connection with FIGS. 1 to 3 applies and identical reference symbols are used.
[0064] FIG. 6 illustrates a further embodiment of the yarn delivery device 1 , which is distinguished in that an electric motor is provided for driving the yarn delivery wheel 17 . The motor is seated in or projects from the base body 3 , as can be seen in FIG. 6 . It is also possible to place the electric motor 53 on top of the base body in place of the pulleys 14 , 15 . The yarn delivery wheel 17 can be designed in accordance with any of the above described versions. In this case, the lifting of the yarn from the yarn delivery wheel 17 enables a slippage of the yarn delivery wheel, without the interrupter reacting, when the yarn delivery and the yarn acceptance do not exactly agree, in particular in case of a minimum acceptance.
[0065] In all of the above described embodiments of the yarn delivery device 1 it is possible to use, instead of one yarn lifting element 28 with two legs 31 , 32 fixed relative to each other, the construction shown in FIG. 8 with two yarn lifting elements 28 a , 28 b . Both yarn lifting elements are maintained by their own supports 36 a , 36 b on their own base section 39 a , 39 b . Pins 54 , 55 , which have a straight configuration, are used as yarn lifting elements and are arranged, the same as the legs 31 , 32 , substantially parallel with or at an acute angle relative to the axis of rotation D. In this case the pins 54 , 55 are aligned parallel with each other and can, if necessary, be adjusted separately by means of their adjustment screws 38 a , 38 b . The two supports 36 a , 36 b can be pivoted independently of each other, so that the pins 54 , 55 can be set to different distances between each other. By means of this the contact angle at which the yarn 2 rests against the yarn delivery wheel 17 can be manually controlled, so that the yarn delivery device 1 can be adapted to installation requirements and/or yarn properties. This can be seen in FIG. 7 , for example, which illustrates the two supports 36 a , 36 b , which can be pivoted toward or away from each other. FIG. 7 moreover shows the parallel orientation of the pins 54 , 55 , which is maintained independently of the inclination relative to the axis of rotation D.
[0066] FIG. 9 illustrates a modified embodiment of the yarn lifting element 28 . In contrast to the embodiment illustrated in FIGS. 1 to 6 , wherein the yarn lifting element 29 a hoop 29 , the FIG. 9 yarn lifting element comprises a solid strip 56 , which has an elongated cross section with rounded flanks. The rounded flanks define the yarn contact surfaces 34 , 35 . The strip 56 can be made of, for example a hard alloy, a ceramic material, or another wear-resistant material. The strip can also be bent from sheet metal and provided with a coating of a hard material, for example a ceramic material. is the strip can be connected rigidly, or by means of an adjustment device and manually adjustable relative to the support 36 , which has a ring-shaped shoulder 57 for fastening on the base support 3 .
[0067] As shown in FIG. 10 , the strip 56 can have a groove 58 between its yarn contact surfaces 34 , 35 , which is spanned by the yarn 2 . An operation as described in connection with FIG. 13 can be achieved.
[0068] With the embodiments of the yarn lifting element 28 shown in FIG. 9 and FIG. 10 , the distance between the yarn contact surfaces 34 , 35 preferably lies in the range between 15 mm and 20 mm. In this way the strip 56 operates like and replaces the hoop 29 .
[0069] A modification of the embodiment in FIGS. 7 and 8 is also possible and is shown in FIG. 11 . The FIG. 7 embodiment is based on both pins 54 , 55 being arranged at the same distance from the yarn delivery wheel 17 . Therefore the supports 36 a , 36 b have the same length. In contrast, the embodiment in FIG. 11 provides supports 36 a , 36 b of different lengths, so that the two pins 54 , 55 are maintained at different distances from the axis of rotation D and the yarn delivery wheel 17 . This opens up the additional possibility of making the pin 55 inactive by pivoting it into the position 59 shown in dashed lines in FIG. 11 .
[0070] FIG. 12 illustrates an alternative arrangement in dashed lines. The legs 31 , 32 have been replaced by a single yarn lifting element 28 ′, which is arranged at a great distance from the yarn delivery wheel 17 . This angle is of such a size that the angle beta, which the yarn 2 running toward the leg 31 forms with the yarn 2 running away from the leg 32 remains unchanged.
[0071] FIG. 13 discloses a further exemplary embodiment of a yarn delivery device with two pins 54 , 55 . These are arranged with an angular spacing of approximately 180°. The pin 54 is fixed, while the pin 55 can be displaceable in the direction of the arrow 61 . With this arrangement, the pin 54 defines a liftoff zone of for example 70°, while the other lifting zone is variable. The loop angle gamma is the sum of both partial loop angles gamma 1 and gamma 2 .
[0072] A yarn lifting element 28 having straight yarn contact surfaces 34 , 35 is provided in a positive feed wheel unit. The position of the surfaces cannot be displaced by the yarn 2 enabling the yarn to slip relative to the yarn delivery wheel 17 if necessary. This permits the positive feed wheel unit to be used in applications which had previously been excluded because of the required synchronicity between the yarn delivery and yarn consumption.
[0000] List of Reference Symbols
[0000]
1 Yarn delivery device
2 Yarn
3 Base body
4 Clamp
5 Yarn inlet means
7 Inlet eye
8 Knot catcher
9 Yarn brake
11 Support
12 Inlet eye
13 Inlet yarn guidance arrangement
14 , 15 Pulleys
16 Coupling ring
17 Yarn delivery wheel
18 Inlet area
18 a , 18 b Sections
19 Yarn protection sleeve
21 Yarn conveying area
22 Cylindrical section
23 Ribs
24 , 25 , 26 Windings
27 Yarn run-off edge
28 Yarn lifting element
29 Hoop
31 , 32 Legs
33 Strip
34 , 35 Yarn contact surfaces
36 Support
37 Spring hinge
38 Adjustment screw
39 Base section
41 Outlet yarn guidance arrangement
42 Hoop
43 Strip
44 Hoop
45 Run-out interrupter
46 run-in interrupter
48 rod
49 end disk
51 openings
52 end disk
53 motor
54 , 55 pins
56 strip
57 shoulder
58 groove
59 position
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A yarn lifting element ( 28 ), which is provided on a positive thread regulating wheel, comprises straight yarn-bearing surfaces ( 34,35 ) whose position cannot be displaced by the yarn ( 2 ), enabling the yarn to slip in relation to the thread feeding wheel ( 17 ) when required. Said additional measure enables the positive thread regulating wheel to be used in areas which were previously excluded on account of the required synchronicity between the feeding of the thread and the consumption of the thread.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to an anisotropic conductive sheet which is incorporated into an information apparatus such as a mobile phone, a personal handyphone system (PHS), a personal digital assistant (PDA), or a notebook computer, or an AV apparatus such as a small audio player, and which is used for electrical connection between various components and members, for example, between circuit boards, between a circuit board and an electronic component, or between a conductive portion provided in an exterior component of an apparatus and a circuit board.
[0003] 2. Description of the Related Art
[0004] As shown in FIG. 20 , an anisotropic conductive sheet ( 1 ) has, within a base portion ( 2 ) formed of an insulating elastic sheet, conductive portions ( 3 ) continuously extending therethrough in the thickness direction thereof, and exhibits conductivity in the sheet thickness direction of the sheet but exhibits no conductivity in the planar direction of the sheet, that is, exhibiting anisotropy. Electrical connection can be easily effected solely by bringing conductive contacts ( 4 ), which are exposed portions of the conductive portions ( 3 ), into press contact with the contact portions (electrode portions) of components or members even without employing such means as soldering or mechanical bonding. Further, since the base portion ( 2 ) retaining the conductive portions ( 3 ) is formed of rubber-like elastic material, it is also possible to absorb vibrations and impact from the outside.
[0005] This anisotropic conductive sheet, however, has a problem in that even if positioning is effected between the contacts of the components or members (not shown) and the conductive contacts ( 4 ) of the anisotropic conductive sheet ( 1 ), positional deviation is liable to occur before the anisotropic conductive sheet ( 1 ) has been completely mounted. To solve this problem, there has been proposed, in JP 2000-82512 A, an anisotropic conductive sheet ( 1 a ) in which, as shown in FIG. 21 , an adhesive layer ( 5 ) is provided around the conductive portions ( 3 ). With this technique, due to the provision of the adhesive layer ( 5 ), when positioning is effected between the contacts of the circuit board and the anisotropic conductive sheet ( 1 a ), positional deviation does not easily occur even if some vibration or impact is applied to the anisotropic conductive sheet ( 1 a ). Further, even if the positioning is erroneously effected, the sheet can be easily peeled off, thus allowing re-positioning.
[0006] However, the anisotropic conductive sheet ( 1 a ) has a problem in that, when the sheet ( 1 a ) is pressurized at the time of mounting, some adhesive is caused to be squeezed out onto the conductive portions ( 3 ) to cover the conductive portions ( 3 ), resulting in an increase in conduction resistance.
SUMMARY OF THE INVENTION
[0007] The present invention has been made with a view toward solving the above-mentioned problems in the prior art. It is therefore an object of the present invention to provide an anisotropic conductive sheet which allows easy temporary fixation at the time of attachment of the anisotropic conductive sheet and which, if pressurized, causes no adhesive to be squeezed out onto the conductive contacts.
[0008] According to the present invention, there is provided an anisotropic conductive sheet including: an insulating base portion; and a plurality of conductive portions extending through the base portion in a thickness direction thereof, in which: the base portion has surfaces through which conductive portions are exposed to form conductive contacts; and at least one of the surfaces has an adhesive portion spaced apart from the conductive contacts.
[0009] Due to the provision of the adhesive portion that is out of contact with the conductive contacts on at least one surface of the base portion, in which the conductive contacts are formed through exposure of the conductive portions therefrom, there is no fear of the adhesive material being spread and squeezed out onto the conductive portions even if the sheet is pressurized after being mounted between a board, components, members, etc. where conduction is to be effected. Thus, there is involved no faulty conduction due to the covering of the conductive portions with the adhesive material.
[0010] In this anisotropic conductive sheet, the adhesive portion can be formed so as to be flush with the surfaces of the conductive contacts. By forming the adhesive portion such that the adhesive portion is flush with the surfaces of the conductive contacts, it is possible to bring the anisotropic conductive sheet into uniform contact with the board, components, and members, to which the anisotropic conductive sheet is to be attached. Thus, it is possible to secure sufficient conductivity and to effect the attachment by the adhesive material to a sufficient degree.
[0011] In forming the adhesive portion, it is possible to embed it in the base portion. By embedding the adhesive portion in the base portion, it is possible to prevent spreading of the adhesive material in the width direction of the anisotropic conductive sheet. Further, since the contact area between the adhesive material and the base portion increases and rubbing against the object of attachment does not easily occur, the adhesive material is not easily peeled off from the base portion and it is possible to suppress transfer of the adhesive material to the object of attachment, such as the board and electronic components, to which the anisotropic conductive sheet is to be attached.
[0012] Further, it is possible for the adhesive portion to be formed so as to protrude outwardly beyond the surfaces of the conductive contacts. By forming the adhesive portion such that the adhesive portion protrudes beyond the surfaces of the conductive contacts, it is possible to reliably effect the fixation of the anisotropic conductive sheet to the object of attachment. Further, even if the surface of the adhesive portion protrudes beyond the surfaces of the conductive contacts, the adhesive portion is spaced apart from the conductive contacts, so the adhesive material does not cover the conductive contacts even if the adhesive portion is spread as a result of pressurization.
[0013] The adhesive portion may be provided on a protrusion provided on the base portion and protruding in the thickness direction. Since the protrusion protruding in the thickness direction is provided on the base portion, and the adhesive portion is provided on the protrusion, it is possible to greatly deflect the protrusion by depression with low pressure. Thus, if the pressurization is weak, it is possible to attain a stable contact between the conductive contacts and the object of attachment. Further, if the adhesive material is spread as a result of pressurization, it only covers the protrusion, and does not cover the conductive contacts.
[0014] Further, it is possible to provide a conductive portion protruding in the thickness direction beyond the surface of the base portion, and to provide the adhesive portion on the surface of the base portion recessed from the surfaces of the conductive contacts. Due to the provision of the conductive portion protruding in the thickness direction beyond the surface of the base portion, and the provision of the adhesive portion on the surface of the base portion recessed from the surfaces of the conductive contacts, there is no fear of the adhesive material covering the conductive contacts even if it is spread as a result of pressurization.
[0015] The conductive portion may be formed by orienting conductive particles in the thickness direction of the anisotropic conductive sheet; by using magnetic particles, the conductive portion can be produced through solidification of the base portion after the formation of the conductive portion by magnetic force.
[0016] According to the anisotropic conductive sheet of the present invention, it is possible to secure stable conduction. Further, it is easy to mount, thus helping to improve workability.
[0017] The above description of the present invention should not be construed restrictively. The advantages, features, and uses of this invention will become more apparent from the following description given with reference to the accompanying drawings. Further, it should be understood that all appropriate modifications made without departing from the gist of this invention are to be covered by the scope of this invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] In the accompanying drawings:
[0019] FIGS. 1(A) through 1(C) show an anisotropic conductive sheet according to a first embodiment of the present invention, of which FIG. 1(A) is a sectional view taken along the line I(A)-I(A) of FIG. 1(B) , FIG. 1(B) is a plan view, and FIG. 1(C) is a sectional view taken along the line I(C)-I(C) of FIG. 1(B) ;
[0020] FIG. 2 is a sectional view of a die for manufacturing an anisotropic conductive sheet;
[0021] FIG. 3 is a sectional view of the die filled with liquid polymer in the anisotropic conductive sheet manufacturing process, showing the die in the state directly after filling with liquid polymer containing conductive particles;
[0022] FIG. 4 is a sectional view of the die filled with liquid polymer in the anistropic conductive polymer manufacturing process, showing how the conductive particles are oriented;
[0023] FIG. 5 is a perspective view of an anisotropic conductive sheet, illustrating how an adhesive material is applied in the anisotropic conductive sheet manufacturing process of the present invention;
[0024] FIGS. 6(A) through 6(C) show an anisotropic conductive sheet according a second embodiment of the present invention, of which FIG. 6(A) is a sectional view taken along the line VI(A)-VI(A) of FIG. 6(B) , FIG. 6(B) is a plan view, and FIG. 6(C) is a sectional view taken along the line VI(C)-VI(C) of FIG. 6(B) ;
[0025] FIGS. 7(A) through 7(C) show an anisotropic conductive sheet according to a first modification of the second embodiment of the present invention, of which FIG. 7(A) is a sectional view taken along the line VII(A)-VII(A) of FIG. 7(B) , FIG. 7(B) is a plan view, and FIG. 7(C) is a sectional view taken along the line VII(C)-VII(C) of FIG. 7(B) ;
[0026] FIGS. 8(A) through 8(C) show an anisotropic conductive sheet according to a second modification of the second embodiment of the present invention, of which FIG. 8(A) is a sectional view taken along the line VIII(A)-VIII(A) of FIG. 8(B) , FIG. 8(B) is a plan view, and FIG. 8(C) is a sectional view taken along the line VIII(C)-VIII(C) of FIG. 8(B) ;
[0027] FIGS. 9(A) through 9(C) show an anisotropic conductive sheet according to a third modification of the second embodiment of the present invention, of which FIG. 9(A) is a sectional view taken along the line IX(A)-IX(A) of FIG. 9(B) , FIG. 9(B) is a plan view, and FIG. 9(C) is a sectional view taken along the line IX(C)-IX(C) of FIG. 9(B) ;
[0028] FIGS. 10(A) and 10(B) show an anisotropic conductive sheet according to a third embodiment of the present invention, of which FIG. 10(A) is a sectional view taken along the line X(A)-X(A) of FIG. 10(B) , and FIG. 10(B) is a plan view;
[0029] FIGS. 11(A) and 11(B) show an anisotropic conductive sheet according to a fourth embodiment of the present invention, of which FIG. 11(A) is a sectional view taken along the line XI(A)-XI(A) of FIG. 11(B) , and FIG. 11(B) is a plan view;
[0030] FIGS. 12(A) and 12(B) show an anisotropic conductive sheet according to a first modification of the fourth embodiment of the present invention, of which FIG. 12(A) is a sectional view taken along the line XII(A)-XII(A) of FIG. 12(B) , and FIG. 12(B) is a plan view;
[0031] FIGS. 13(A) and 13(B) show an anisotropic conductive sheet according to a second modification of the fourth embodiment of the present invention, of which FIG. 13(A) is a sectional view taken along the line XIII(A)-XIII(A) of FIG. 13(B) , and FIG. 13(B) is a plan view;
[0032] FIGS. 14(A) and 14(B) show an anisotropic conductive sheet according to a third modification of the fourth embodiment of the present invention, of which FIG. 14 (A) is a sectional view taken along the line XIV(A)-XIV(A) of FIG. 14(B) , and FIG. 14(B) is a plan view;
[0033] FIGS. 15(A) and 15(B) show an anisotropic conductive sheet according to a fifth embodiment of the present invention, of which FIG. 15(A) is a sectional view taken along the line XV(A)-XV(A) of FIG. 15(B) , and FIG. 15(B) is a plan view;
[0034] FIG. 16 is a plan view of an anisotropic conductive sheet according to a modification of the present invention;
[0035] FIG. 17 is a plan view of an anisotropic conductive sheet according to another modification of the present invention;
[0036] FIG. 18 is a plan view of an anisotropic conductive sheet according to still another modification of the present invention;
[0037] FIGS. 19(A) through 19(C) show an anisotropic conductive sheet according to a modification of the first embodiment of the present invention, of which FIG. 19(A) is a sectional view taken along the line XIX(A)-XIX(A) of FIG. 19(B) , FIG. 19(B) is a plan view, and FIG. 19(C) is a sectional view taken along the line XIX(C)-XIX(C) of FIG. 19(B) ;
[0038] FIG. 20 is a sectional view of a conventional anisotropic conductive sheet; and
[0039] FIG. 21 is a sectional view of another conventional anisotropic conductive sheet.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0040] The present invention will be described in more detail with reference to the drawings. In the drawings, the reference numerals indicate portions and components. In the following, a redundant description of the materials and manufacturing method common to the various embodiments will be omitted.
[0041] First Embodiment ( FIG. 1 ): FIGS. 1(A) through 1(C) show an anisotropic conductive sheet ( 11 ) according to a first embodiment. FIG. 1(B) is a plan view (top view) of the anisotropic conductive sheet ( 11 ), FIG. 1(A) is a sectional view taken along the line I(A)-I(A) of FIG. 1(B) , and FIG. 1(C) is a sectional view taken along the line I(C)-I(C) of FIG. 1(B) . The anisotropic conductive sheet ( 11 ) has, in a base portion ( 12 ) formed of insulating silicone rubber, a plurality of (two in FIG. 1 ) conductive portions ( 13 ) composed of conductive particles connected together and extending therethrough in the thickness direction, with the portions of the conductive portions ( 13 ) exposed on the surfaces forming conductive contacts ( 14 ). Further, adhesive portions ( 15 ) are formed in a dotted fashion so as to be spaced apart from the conductive contacts ( 14 ) by the same distance. The adhesive portions ( 15 ) are formed by embedding an adhesive material in recesses ( 12 a ) provided in the surfaces ( 12 s ) in the thickness direction of the base portion ( 12 ), and the surfaces of the adhesive portions ( 15 ) are flush with the surfaces of the base portions ( 12 ) and the conductive contacts ( 14 ). The adhesive portions ( 15 ) are provided in both of the two surfaces ( 12 s ) in the thickness direction of the anisotropic conductive sheet ( 11 ).
[0042] FIGS. 2 through 5 schematically show the process of manufacturing the anisotropic conductive sheet ( 11 ). First, there are prepared a pair of upper and lower dies ( 17 a and 17 b ) in which pins ( 16 ) formed of magnetic material are embedded. In the dies ( 17 a and 17 b ), there are provided protrusions ( 17 c ) protruding into the cavity so as to form the recesses ( 12 a ) to be filled with adhesive material ( FIG. 2 ). A liquid polymer ( 19 ) containing conductive particles ( 18 ) is poured into the die ( 17 a , 17 b ) ( FIG. 3 ), and the liquid polymer ( 19 ) is cured while orienting the conductive particles ( 18 ) in the extensions of the pins ( 16 ) by the magnetic force thereof. In this way, there are formed the conductive portions ( 13 ) composed of the conductive particles ( 18 ) oriented in the insulating base portion ( 12 ) formed of the liquid polymer ( 19 ) ( FIG. 4 ). After releasing this molding from the die, an adhesive is applied to the recesses ( 12 a ) provided in the base portion ( 12 ) by means of a dispenser ( 20 ) or the like ( FIG. 5 ), and the polymer is cured. In this way, the adhesive portions ( 15 ) are formed in the recesses ( 12 a ) to thereby obtain the anisotropic conductive sheet ( 11 ) as shown in FIGS. 1(A) through 1(C) .
[0043] Of the die ( 17 a , 17 b ), the pins ( 16 ) are formed of a magnetic material, whereas the portion other than the pins ( 16 ) are produced by using a non-magnetic material, such as aluminum, copper, tungsten carbide, brass, or resin. It is desirable for the magnitude of the magnetic force of the magnetic material used for the pins ( 16 ) to be 0.1 T (tesla) to 2 T. If the magnitude of the magnetic force is less than 0.1 T, the orientation of the conductive particles is not effected to a sufficient degree, and no uniform conductive portions ( 13 ) can be generated. On the other hand, if the magnitude of the magnetic force is more than 2 T, while it is possible to form uniform conductive portions ( 13 ), no positive effect is to be expected since the saturation magnetic flux density of a ferromagnetic material such as iron, is less than 2 T.
[0044] For the liquid polymer ( 19 ), there is used a material which is electrically insulating and which exhibits a rubber-like elasticity after curing. Examples of the material that can be used include silicone rubber, natural rubber, isoprene rubber, butadiene rubber, acrylonitrile butadiene rubber, 1,2-polybutadiene, styrene-butadiene rubber, chloroprene rubber, nitrile rubber, butyl rubber, ethylene-propylene rubber, chlorosulfone rubber, polyethylene rubber, acrylic rubber, epichlorohydrin rubber, fluorine rubber, urethane rubber, styrene type thermoplastic elastomer, olefin type thermoplastic elastomer, ester type thermoplastic elastomer, urethane type thermoplastic elastomer, amide type thermoplastic elastomer, vinyl chloride type thermoplastic elastomer, fluoride type thermoplastic elastomer, and ion crosslinking elastomer. From the viewpoint of moldability, electrical insulation property, and weathering performance, it is desirable to employ silicone rubber; especially, it is still more desirable to employ liquid silicone rubber. It is necessary for the viscosity of the liquid polymer to be one imparting fluidity to the contained conductive particles ( 18 ) according to the magnetic field; preferably, it ranges from 1 Pa·s to 250 Pa·s, and more preferably, it ranges from 10 Pa·s to 100 Pa·s.
[0045] The conductive particles ( 18 ) contained in the liquid polymer ( 19 ) is made of a magnetic material of low electrical resistance forming the conductive portions ( 13 ) by magnetic force; examples of the materials to be preferably used include ferromagnetic metals such as iron, nickel, or cobalt, or an alloy thereof, a material obtained by plating a resin or ceramic with a magnetic conductor, and a material obtained by plating magnetic powder with a highly conductive metal. However, when the conductive portions ( 13 ) are formed by a method other than a method based on orientation with magnetic force, the material to be used is not particularly limited to a magnetic one; in this case, it is possible to employ a metal of a low electrical resistance of preferably 1Ω or less, ceramic, carbon, etc. Examples of the highly conductive metal other than that mentioned above include metals such as gold, silver, platinum, aluminum, copper, palladium, and chromium, and an alloy such as stainless steel. Further, it is also possible to employ a material obtained by plating thin wires of a resin, ceramic or the like with a highly conductive metal. When orienting the conductive particles ( 18 ) in the liquid polymer by magnetic force, a granular material is used; however, in the case in which the conductive material is previously formed into the configuration of the conductive portions ( 13 ), it is also possible to use a fibrous or thin-wire-like material.
[0046] When orienting the conductive particles ( 18 ) in the liquid polymer ( 19 ), it is desirable for the content of the conductive particles ( 18 ) to be 5 to 100 parts by weight with respect to 100 parts by weight of the liquid polymer. If the content is less than 5 parts by weight, there is a fear of the conductive particles ( 18 ) not being connected together to a sufficient degree to allow them to extend through the cured liquid polymer ( 19 ), involving portions where no conductive portions ( 13 ) are formed. If the content exceeds 100 parts by weight, the viscosity becomes too high, and there is the possibility of the conductive particles ( 18 ) not being oriented to a sufficient degree. It is desirable for the conductive particles ( 18 ) to be spherical ones of uniform grain size. If they do not exhibit a sharp grain size distribution, there is a fear of the conductive portions ( 13 ) of the resultant anisotropic conductive sheet ( 11 ) involving branching or the configuration of the conductive portions ( 13 ) being rather irregular. In view of this, it is desirable for the standard deviation of the grain size distribution to be 20% or less. It is desirable for the average grain size of the conductive particles to range from 10 nm to 200 μm. If the average grain size is less than 10 nm, the viscosity of the liquid polymer ( 19 ) containing the conductive particles ( 18 ) increases, and the contact resistance of the resultant anisotropic conductive sheet ( 11 ) increases. If the average grain size is larger than 200 μm, the conductive particles ( 18 ) are liable to settle in the liquid polymer ( 19 ), resulting in a deterioration in dispersion property.
[0047] The curing conditions for curing the liquid polymer ( 19 ), such as the curing temperature and time, are determined as appropriate according to the liquid polymer ( 19 ) selected; it is desirable for the curing to be effected after the conductive particles ( 18 ) have been oriented to a sufficient degree in the magnetic field. Further, the liquid polymer ( 19 ) containing the conductive particles ( 18 ) may also contain, apart from the liquid polymer ( 19 ) and the conductive particles ( 18 ), various additives such as crosslinking accelerator and dispersing agent as long as they do not adversely affect the orientation property of the conductive particles ( 18 ), the stability of the liquid polymer ( 19 ), conductivity of the resultant anisotropic conductive sheet ( 11 ), etc.
[0048] Examples of the material of the adhesive portions ( 15 ), which are formed through application of an adhesive material, include a silicone type resin, a urethane type resin, an acrylic resin, an epoxy type resin, an ethylene-vinyl-acetate copolymer, an ethylene-acrylate copolymer, a polyamide type resin, a polyester type resin, a polyolefin type resin, a fluorine type resin, an ionomer type resin, a polystyrene type resin, a polyimide type resin, other thermoplastic resins and thermosetting resins, and an adhesive material formed of a mixture of two or more kinds of the above-mentioned materials. Above all, a silicone type adhesive material is preferable from the viewpoint of heat resistance, durability, and vibration characteristic. Further, it is possible for those adhesive materials to contain, as needed, additives such as curing agent, vulcanizing agent, softening agent, coloring agent, and filler.
[0049] While the thickness of the anisotropic conductive sheet ( 11 ) allows various modifications, from the viewpoint of a demand for a reduction in the thickness and size of apparatuses, it usually ranges from approximately 0.1 mm to 10 mm, and more preferably, from 0.2 mm to 2 mm. If the thickness is less than 0.1 mm, the anisotropic conductive sheet ( 11 ) cannot be endowed with a sufficient level of strength, and there is a fear of breakage during use. On the other hand, if the thickness exceeds 5 mm, the magnetic force is weakened in the intermediate portion in the thickness direction, so it may occur that the orientation of the conductive particles ( 18 ) is not effected to a sufficient degree. Further, the thickness of the apparatus will increase. The thickness of the adhesive portions ( 15 ) varies according to the thickness of the anisotropic conductive sheet ( 11 ) as a whole; while it may be 1/10 to ½ of the thickness of the anisotropic conductive sheet ( 11 ), it is usually 10 μm to 500 μm, and more preferably, 25 μm to 50 μm. There are no particular limitations regarding the width of the anisotropic conductive sheet ( 11 ), and it may vary as appropriate according to the size of the conductive portions of the object of attachment; the diameter of one dot may range from 0.05 mm to 3.0 mm, and more preferably, from 0.2 mm to 1.0 mm.
[0050] The die ( 17 a , 17 b ) used for the production of the anisotropic conductive sheet ( 11 ) may employ, instead of the ferromagnetic pins ( 16 ), the paramagnetic pins ( 16 ), generating a magnetic field in the cavity inside the die ( 17 a , 17 b ) by an electromagnet installed outside the die ( 17 a , 17 b ). Pouring the liquid polymer ( 19 ) containing the conductive particles ( 18 ) into the die ( 17 a , 17 b ) to which magnetic force is imparted, is advantageous in that the orientation time for the conductive particles ( 18 ) is short. On the other hand, it must be cared so that a variation is not generated in the amount and density of the particles forming the conductive portions ( 13 ).
[0051] In the anisotropic conductive sheet ( 11 ) thus obtained, the adhesive portions ( 15 ) are provided at positions where they do not come into contact with the portions where the conductive contacts ( 14 ) are exposed and are spaced apart therefrom, so even when the anisotropic conductive sheet ( 11 ) is mounted and pressurized, there is no fear of the adhesive material being squeezed out to cover the conductive portions ( 13 ). Thus, no faulty conduction occurs. Further, since the surface of the conductive contacts ( 14 ) and the surfaces of the adhesive portions ( 15 ) are flush with each other, it is possible to bring the anisotropic conductive sheet ( 11 ) into uniform contact with the object of attachment.
[0052] Further, since the adhesive portions ( 15 ) are embedded in the base portion ( 12 ), it is possible to prevent the adhesive material from being spread even if pressurized. Further, the adhesive material is not easily separated from the base portion ( 12 ), making it possible to prevent transfer of the adhesive material to the object of attachment.
[0053] Second Embodiment ( FIG. 6 ): FIGS. 6(A) through 6(C) show an anisotropic conductive sheet ( 21 ) according to a second embodiment. As shown in FIG. 6(B) , the anisotropic conductive sheet ( 21 ) is the same as the anisotropic conductive sheet ( 11 ) of the first embodiment in that the adhesive portions ( 15 ) are formed in a dotted fashion. While in the anisotropic conductive sheet ( 11 ) the adhesive material is embedded in the recesses ( 12 a ) provided in the base portion ( 12 ), in this embodiment, no recesses are formed in the base portion ( 12 ) as shown in FIG. 6(C) ; instead, the adhesive portions ( 15 ) are formed through application to the flat surfaces ( 12 s ). Thus, the surfaces of the adhesive portions ( 15 ) protrude somewhat from the surfaces ( 12 s ) of the base portion ( 12 ). To produce the anisotropic conductive sheet ( 21 ), a die (not shown) having no protrusions for forming the recesses is used.
[0054] In the anisotropic conductive sheet ( 21 ), the adhesive portions ( 15 ) protrude beyond the conductive contacts ( 14 ), so the fixation to the object of attachment can be effected reliably. In forming the adhesive portions ( 15 ), it is desirable to adopt, apart from a dispenser, a printing method such as silk screen printing, pad printing, or metal block printing. It is also possible to previously provide on a base member a pattern formed of the adhesive material forming the adhesive portions ( 15 ), and to transfer the adhesive material onto the anisotropic conductive sheet ( 21 ), thereby providing the adhesive portions ( 15 ). In this embodiment, the adhesive portions ( 15 ) are provided on the flat surfaces ( 12 s ) of the base portion, so it is possible to adjust the thickness of the adhesive portions ( 15 ) as appropriate, with the thickness thereof being 5 μm to 1 mm.
[0055] First Modification of the Second Embodiment ( FIG. 7 ): FIGS. 7(A) through 7(C) show an anisotropic conductive sheet ( 21 a ) according to a first modification of the second embodiment. As compared with the anisotropic conductive sheet ( 21 ), in the anisotropic conductive sheet ( 21 a ), the conductive portions ( 13 ) and the portions of the base portion ( 12 ) around the same protrude somewhat and are swollen. Thus, the surfaces of the conductive contacts ( 14 ) protrude beyond the surfaces ( 12 s ) of the base portion ( 12 ). Thus, it is possible to reliably effect conduction between the anisotropic conductive sheet ( 21 a ) and the object of attachment. The conductive portions ( 15 ) are formed on the flat surfaces ( 12 s ) of the base portion ( 12 ). By adjusting the application amount of the adhesive material, it is possible to form the surfaces of the adhesive portions ( 15 ) so as to be flush with the surfaces of the conductive contacts ( 14 ); further, by increasing the application amount of the adhesive material, it is possible to form the surfaces of the adhesive portions ( 15 ) so as to protrude beyond the surfaces of the conductive contacts ( 14 ). In the anisotropic conductive sheet ( 21 a ) of the first modification, the surfaces of the conductive contacts ( 14 ) and the surfaces of the adhesive portions ( 15 ) are flush with each other, so it is possible to bring the anisotropic conductive sheet ( 21 a ) into uniform contact with the object of attachment. When the adhesive portions ( 15 ) protrude beyond the conductive contacts ( 14 ), it is possible to more reliably effect the fixation of the anisotropic conductive sheet to the object of attachment. In this way, even if the adhesive portions ( 15 ) protrude beyond the conductive contacts ( 14 ), since the adhesive material is soft, it is possible to sufficiently secure contact between the conductive contacts ( 14 ) and the object of attachment.
[0056] Further, the adhesive portions ( 15 ) are provided on the surfaces ( 12 s ) of the base portion ( 12 ) recessed from the surfaces of the conductive contacts ( 14 ), so if the adhesive material forming the adhesive portions ( 15 ) is pressed and spread through pressurization, it is not spread onto the conductive contacts ( 14 ), which are swollen high. Thus, it is possible to secure reliable conduction of the conductive contacts ( 14 ).
[0057] Second Modification of the Second Embodiment ( FIG. 8 ): FIGS. 8(A) through 8(C) show an anisotropic conductive sheet ( 21 b ) according to a second modification of the second embodiment, in which protrusions ( 12 b ) are provided on the base portion ( 12 ) so as to cover the difference in height between the swollen conductive contacts ( 14 ) and the flat base portion ( 12 ), and the adhesive portions ( 15 ) are provided on the protrusions ( 12 b ). That is, the height of the protrusions ( 12 b ) is substantially the same as the height of the conductive contacts ( 14 ). By providing the adhesive portions ( 15 ) on the protrusions ( 12 b ), the adhesive portions ( 15 ) become higher than the conductive contacts ( 14 ), and protrude outwardly, so the adhesive portions ( 15 ) are reliably brought into contact with the object of attachment. Thus, it is possible to temporarily fix the anisotropic conductive sheet ( 21 b ) to the object of attachment without pressurizing the anisotropic conductive sheet ( 21 b ). Further, since the base portion ( 12 ) has the protrusions ( 12 b ), the anisotropic conductive sheet ( 21 b ) can be deflected greatly with lower pressure, making it possible to stabilize the contact with the object of attachment even through pressurization with low pressure. While in FIG. 8 the protrusions ( 12 b ) have a truncated-cone-shaped configuration, they may also be formed in other configurations such as a columnar one.
[0058] Third Modification of the Second Embodiment ( FIG. 9 ): FIGS. 9(A) through 9(C) show an anisotropic conductive sheet ( 21 c ) according to a third modification of the second embodiment, which, while having, like the anisotropic conductive sheet ( 21 b ), the protrusions ( 12 b ), which are swollen portions of the base portion ( 12 ), has no swelling of the conductive contacts ( 14 ), with the surfaces ( 12 s ) of the base portion ( 12 ) being flush with the surfaces of the conductive contacts ( 14 ). In the anisotropic conductive sheet ( 21 c ), the adhesive portions ( 15 ) are provided on the protrusions ( 12 b ), whereby the adhesive portions ( 15 ) are higher than the conductive contacts ( 14 ) and protrude outwardly, so it is possible to reliably bring the adhesive portions ( 15 ) into contact with the object of attachment. Further, since the base portion ( 12 ) has the protrusions ( 12 b ), the anisotropic conductive sheet ( 21 c ) can be deflected greatly with low pressure, and the conductive contacts ( 14 ) can be brought into stable contact with the object of attachment even through pressurization with low pressure. While in FIGS. 9(A) through 9(C) the protrusions ( 12 b ) have a truncated-cone-shaped configuration, they may also be formed in some other configuration such as a columnar one. In this modification, the conductive portions ( 13 ) and the peripheral portions thereof do not protrude; however, if the adhesive material is pressed and spread through pressurization, the spread adhesive material covers the protrusions ( 12 b ) and does not reach the conductive contacts ( 14 ), so it is possible to secure stable conduction.
[0059] Third Embodiment ( FIG. 10 ): FIGS. 10(A) and 10(B) show an anisotropic conductive sheet ( 31 ) according to a third embodiment. FIG. 10(B) is a plan view (top view) of the anisotropic conductive sheet ( 31 ), and FIG. 10(A) is a sectional view taken along the line X(A)-X(A) of FIG. 10(B) . The anisotropic conductive sheet ( 31 ) has on its surfaces the adhesive portions ( 15 ) provided in a linear fashion. Unlike the anisotropic conductive sheet ( 11 ) formed in the dotted fashion of the first embodiment, the adhesive portions ( 15 ) are formed in a linear fashion. However, the anisotropic conductive sheet ( 31 ) of the third embodiment is the same as the anisotropic conductive sheet ( 11 ) of the first embodiment in that the recesses ( 12 a ) are formed in the base portion ( 12 ) and filled with the adhesive material. Thus, the surfaces of the adhesive portions ( 15 ) are formed so as to be flush with the surfaces of the conductive contacts ( 14 ).
[0060] In the anisotropic conductive sheet ( 31 ), the adhesive portions ( 15 ) are provided so as to be spaced apart from the conductive contacts ( 14 ), so even if it is pressurized at the time of mounting, there is no fear of the adhesive material being squeezed out to cover the conductive portions ( 13 ). Thus, no faulty conduction occurs. Further, since the surfaces of the conductive contacts ( 14 ) and the surfaces of the adhesive portions ( 15 ) are flush with each other, it is possible to bring the anisotropic conductive sheet ( 31 ) into uniform contact with the object of attachment. Further, since the adhesive portions ( 15 ) are embedded in the base portion ( 12 ), the adhesive material is not easily separated from the base portion ( 12 ), making it possible to prevent transfer of the adhesive material to the object of attachment.
[0061] Further, in the anisotropic conductive sheet ( 31 ), the adhesive portions ( 15 ) are provided continuously in a loop-like fashion around the conductive contacts ( 14 ), so it is possible to bring the anisotropic conductive sheet into stable contact with the object of attachment regardless of the configuration of the object of attachment. Since the loop-like adhesive portion ( 15 ) is held in contact with the object of attachment, the interior surrounded by the adhesive portion ( 15 ) is kept in a decompressed state, thereby making the anisotropic conductive sheet ( 31 ) still less subject to separation.
[0062] Fourth Embodiment ( FIG. 11 ): An anisotropic conductive sheet ( 41 ) according to this embodiment shown in FIGS. 11(A) and 11(B) is the same as the anisotropic conductive sheet ( 31 ) of the third embodiment in that the adhesive portion ( 15 ) is formed in a linear fashion. While in the anisotropic conductive sheet ( 31 ) of the third embodiment the adhesive material is embedded in the recesses ( 12 a ) formed in the base portion ( 12 ), in this embodiment, no recesses are formed in the base portion ( 12 ); the adhesive portions ( 15 ) are formed by applying the adhesive material to the flat surfaces ( 12 s ) of the base portion ( 12 ). Thus, the surfaces of the adhesive portions ( 15 ) protrude beyond the surfaces ( 12 s ) of the base portion ( 12 ) by the thickness of the adhesive portions ( 15 ).
[0063] In the anisotropic conductive sheet ( 41 ) of this embodiment, the adhesive portions ( 15 ) are provided so as to be spaced apart from the portions where the conductive contacts ( 14 ) are exposed, so even when the anisotropic conductive sheet ( 41 ) is mounted and pressurized, there is no fear of the adhesive material being squeezed out to cover the conductive portions ( 13 ). Thus, no faulty conduction occurs. Further, in the anisotropic conductive sheet ( 41 ), the adhesive portions ( 15 ) protrude beyond the conductive contacts ( 14 ), so the anisotropic conductive sheet can be reliably fixed to the object of attachment.
[0064] First Modification of the Fourth Embodiment ( FIG. 12 ): FIGS. 12(A) and 12(B) show an anisotropic conductive sheet ( 41 a ) according to a first modification of the fourth embodiment. As compared with the anisotropic conductive sheet ( 41 ), the anisotropic conductive sheet ( 41 a ) is configured such that the conductive portions ( 14 ) and the portions of the base ( 12 ) therearound are somewhat swollen. Thus, the surfaces of the conductive contacts ( 14 ) protrude beyond the surfaces ( 12 s ) of the base portion ( 12 ). Due to the protrusion of the conductive contacts ( 14 ), it is possible to achieve reliable conduction with the object of attachment. Further, the adhesive portions ( 15 ) of the anisotropic conductive sheet ( 41 a ) are formed on the flat surfaces ( 12 s ) of the base portion ( 12 ). By adjusting the application amount of the adhesive material, it is possible to form the surfaces of the adhesive portions ( 15 ) so as to be flush with the surfaces of the conductive contacts ( 14 ); further, by increasing the application amount of the adhesive material, it is possible to cause the surfaces of the adhesive portions ( 15 ) to protrude beyond the surfaces of the conductive contacts ( 14 ). In the anisotropic conductive sheet ( 41 a ) of the first modification, the surfaces of the conductive contacts ( 14 ) and the surfaces of the adhesive portions ( 15 ) are flush with each other, so it is possible to bring the anisotropic conductive sheet ( 41 a ) into uniform contact with the object of attachment. On the other hand, when the adhesive portions ( 15 ) protrude beyond the conductive contacts ( 14 ), it is possible to more reliably fix the conductive contacts ( 14 ) to the object of attachment. In this way, even if the adhesive portions ( 15 ) protrude beyond the conductive contacts ( 14 ), since the adhesive material is soft, it is possible to sufficiently secure contact between the conductive contacts ( 14 ) and the object of attachment.
[0065] Further, the adhesive portions ( 15 ) are provided on the surfaces ( 12 s ) of the base portion ( 12 ) recessed from the surfaces of the conductive contacts ( 14 ), so if the adhesive material forming the adhesive portions ( 15 ) is pressed and spread through pressurization, it is not spread onto the conductive contacts ( 14 ), which are swollen high. Thus, it is possible to secure reliable conduction for the conductive contacts ( 14 ).
[0066] Second Modification of the Fourth Embodiment ( FIG. 13 ): FIGS. 13(A) and 13(B) show an anisotropic conductive sheet ( 41 b ) according to a second modification of this embodiment, in which protrusions ( 12 b ) are provided on the base portion ( 12 ) so as to cover the difference in height between the swollen conductive contacts ( 14 ) and the flat base portion ( 12 ), and the adhesive portions ( 15 ) are provided on the protrusions ( 12 b ). That is, the height of the protrusions ( 12 b ) is substantially the same as the height of the conductive contacts ( 14 ). Due to the provision of the adhesive portions ( 15 ) on the protrusions ( 12 b ), the adhesive portions ( 15 ) are higher than the conductive contacts ( 14 ) and protrude outwardly, so the adhesive portions ( 15 ) are reliably brought into contact with the object of attachment. Thus, it is possible to temporarily fix the anisotropic conductive sheet ( 41 b ) to the object of attachment without having to pressurize the same. Further, since the base portion ( 12 ) has the protrusions ( 12 b ), it is possible to greatly deflect the anisotropic conductive sheet ( 41 b ) with low pressure, and the conductive contacts ( 14 ) can be brought into stable contact with the object of attachment through pressurization with low pressure. While the protrusions ( 12 b ) in FIG. 12(A) have a columnar configuration, they may also have some other configuration such as a truncated-cone-like one.
[0067] Third Modification of the Fourth Embodiment ( FIG. 14 ): FIGS. 14(A) and 14(B) show an anisotropic conductive sheet ( 41 c ) according to a third modification of this embodiment, which, while having the protrusions ( 12 b ) which are formed through swelling of the base portions ( 12 ) as in the case of the anisotropic conductive sheet ( 41 b ), has no swelling of the conductive contacts ( 14 ), and the surfaces ( 12 s ) of the base portion ( 12 ) and the surfaces of the conductive contacts ( 14 ) are flush with each other. In the anisotropic conductive sheet ( 41 c ), by providing the adhesive portions ( 15 ) on the protrusions ( 12 b ), the adhesive portions ( 15 ) are higher than the conductive contacts ( 14 ) by the sum of the height of the protrusions ( 12 b ) and the height of the adhesive portions ( 15 ), and protrude outwardly, so it is possible to reliably bring the contact portions ( 15 ) into contact with the object of attachment. Further, since the base portion ( 12 ) has the protrusions ( 12 b ), it is possible to greatly deflect the anisotropic conductive sheet ( 41 c ) with low pressure, and to achieve stable contact between the conductive contacts ( 14 ) and the object of attachment through pressurization with low pressure.
[0068] Further, the adhesive portions ( 15 ) of the anisotropic conductive sheet ( 41 c ) are swollen along the outer periphery of the anisotropic conductive sheet ( 41 c ), so nails or the like do not easily get between the object of attachment and the anisotropic conductive sheet ( 41 c ); thus, once mounted, the anisotropic conductive sheet is not easily separated.
[0069] Fifth Embodiment ( FIG. 5 ): FIGS. 15(A) and 15(B) show an anisotropic conductive sheet ( 51 ) according to a fifth embodiment. FIG. 15(B) is a plan view (top view) of the anisotropic conductive sheet ( 51 ), and FIG. 15(A) is a sectional view taken along the line XV(A)-XV(A) of FIG. 15(B) . The anisotropic conductive sheet ( 51 ) has, on the entire both surfaces in the thickness direction thereof, the adhesive portions ( 15 ) except for regions separating the contact electrodes ( 14 ) from the adhesive portions ( 15 ) by a fixed distance. The anisotropic conductive sheet ( 51 ) is the same as the anisotropic conductive sheet ( 11 ) and the anisotropic conductive sheet ( 31 ) in that the adhesive material fills the recesses ( 12 a ) provided in the base portion ( 12 ), and the surfaces of the adhesive portions ( 15 ) are flush with the surfaces of the conductive contacts ( 14 ).
[0070] In the anisotropic conductive sheet ( 51 ) of this embodiment, the adhesive portions ( 15 ) are formed over the entire surfaces except for the regions separating them from the conductive contacts ( 14 ) by a fixed distance, so it is possible for the anisotropic conductive sheet to be bonded to the object of attachment more firmly. Further, since the adhesive portions ( 15 ) extend to the outer periphery of the anisotropic conductive sheet ( 51 ), the mounting can be effected in a stable manner even if there are some protrusions and recesses in the boundary portion between the anisotropic conductive sheet ( 51 ) and the object of attachment.
[0071] Modifications of the Embodiments ( FIGS. 16 through 18 ): While in the anisotropic conductive sheet of each of the above-mentioned embodiments ( 11 , 21 , 21 a , 21 b , 21 c , 31 , 41 , 41 a , 41 b , 41 c , 51 ) two conductive portions ( 13 ) are formed, the number of the conductive portions ( 13 ) is not restricted to two. For example, it is also possible to form an anisotropic conductive sheet ( 61 ) as shown in FIG. 16 in which a large number of conductive portions ( 13 ) and adhesive portions ( 15 ) are formed, with a large number of conductive contacts ( 14 ) being exposed on the surfaces thereof (In FIG. 16 , the larger circles represent the conductive portions ( 13 ), and the smaller circles represent the adhesive portions ( 15 )). Further, it is also possible to cut off a part (region R of FIG. 16 ) of the anisotropic conductive sheet ( 61 ) to produce, for example, an anisotropic conductive sheet ( 11 ) with two conductive portions ( 13 ), or cut the anisotropic conductive sheet ( 61 ) in an appropriate size according to the use. By producing an anisotropic conductive sheet ( 61 a ) as shown in FIG. 17 , it is possible to cut off and produce anisotropic conductive sheets ( 11 ) efficiently without wasting any portion of the anisotropic conductive sheet ( 61 a ). Further, it is also possible to form an anisotropic conductive sheet ( 61 b ) as shown in FIG. 18 in which the adhesive portions ( 15 ) are formed in a linear fashion.
[0072] Further, while in the anisotropic conductive sheet of each of the above embodiments ( 11 , 21 , 21 a , 21 b , 21 c , 31 , 41 , 41 a , 41 b , 41 c , 51 , 61 , 61 a , 61 b ) the adhesive portions ( 15 ) are provided on both of the surfaces ( 12 s ) in the thickness direction of the base portion ( 12 ), it is also possible to provide the adhesive portions ( 15 ) on only one of the two surfaces. For example, FIGS. 19(A) through 19(C) show an anisotropic conductive sheet ( 11 a ) according to a modification of the anisotropic conductive sheet ( 11 ) of the first embodiment in which the adhesive portions ( 15 ) are provided on one side only.
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Disclosed is an anisotropic conductive sheet which is equipped with an insulating base portion and a plurality of conductive portions extending through the base portion in a thickness direction thereof, which easily allows temporary fixation at a time of attachment thereof, and which, if pressurized, causes no adhesive material to be squeezed out onto the conductive contacts. An anisotropic conductive sheet includes a base portion and conductive portions exposed therethrough to form conductive contacts, with at least one of surfaces of the base portion having an adhesive portion spaced apart from the conductive contacts. Thus, it is possible to secure stable conduction with a board and an electrode portion of an electronic component. Further, this anisotropic conductive sheet is easy to mount, thus helping to improve workability.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. patent application Ser. No. 12/809,477, filed Oct. 11, 2010, which is the National Stage of International Application No. PCT/IB2008/003566, filed Dec. 19, 2008, which claims priority to U.S. Provisional Patent Application No. 61/015,294, filed Dec. 20, 2007, all of which are hereby incorporated by reference as if fully set forth herein.
TECHNICAL FIELD
[0002] The present invention is related to assignment and handover in a radio communication network. (As used herein, references to the “present invention” or “invention” relate to exemplary embodiments and not necessarily to every embodiment encompassed by the appended claims.) More specifically, the present invention is related to assignment and handover in a radio communication network where a first resource indicator and a second resource indicator are offered together in a message for selection.
BACKGROUND
[0003] This section is intended to introduce the reader to various aspects of the art that may be related to various aspects of the present invention. The following discussion is intended to provide information to facilitate a better understanding of the present invention. Accordingly, it should be understood that statements in the following discussion are to be read in this light, and not as admissions of prior art.
[0004] The A-interface is defined in 3GPP as the terrestrial interface between the MSC node and the BSS radio network. Today TDM is the only defined bearer technology for user plane connection defined in the A-interface. The A-interface is defined in 3GPP technical specification 48.001 (3GPP TS 48.001 Base Station System—Mobile-services Switching Centre (BSS-MSC) interface; General aspects) and the references specified therein.
[0005] Handover procedures are defined in 3GPP technical specification 23.009 (3GPP TS 23.009 Handover Procedures). The technical specification assumes an A-interface as defined in the 3GPP standard (3GPP TS 48.001 Base Station System—Mobile-services Switching Centre (BSS-MSC) interface; General aspects).
[0006] FIG. 1 shows the procedure for an intra MSC, inter BSC, GSM to GSM handover procedure taken from 3GPP TS 23.009 Handover Procedures. This procedure is chosen as an example because it is used below to describe the concept of the new invention.
[0007] In regard to problems with existing solutions, currently the effort is taken to enhance the current standardized A-interface and to support the A-interface as well for IP used as bearer for the user plane. Although in the further disclosed, reference is made to IP technology as a further supported technology, the invention is not limited thereto but encompasses any differing bearer technology. It is assumed that during a network migration from the currently standardized A-interface (AoTDM) to the enhanced A-interface (AoIP) the two bearer technologies defined for the user plane are used in parallel. This may not be needed in all migration scenarios but it is seen as a likely scenario for many operators.
[0008] Applying the current 3GPP handover procedure (3GPP TS 23.009 Handover Procedures) in such a scenario—parallel use of TDM and IP as user plane bearer—results in the following issue: When the MSC request channel assignment from the target BSC then the MSC does not know if this BSC can establish the terrestrial interface using IP as bearer type. The BSC has the final decision on the bearer type because of the following rules:
[0009] In the BSC the decision for a specific bearer on the terrestrial interface may depend on the selected speech coder version for the A-interface.
[0010] The BSC has always the final decision regarding the radio codec and the same codec should be used on the terrestrial interface as on the radio link to avoid additional transcoding.
[0011] The MSC has to seize bearer resources for the A-interface user plane (terrestrial interface) before it sends BSSMAP Handover Request message to the target BSC. If the target BSC cannot support TDM bearer for the terrestrial interface then BSC has to reject the call. MSC could repeat the BSSMAP Handover Request message using in the new request IP bearer for the terrestrial interface. This handling would require additional signaling on the A-interface and would extend the handover time.
[0012] One simple solution to avoid the repetition of the handover request message would be to provide some configuration in MSC about the BSC capability. However, this solution has the following disadvantages:
[0013] It is static and cannot provide BSC capability for a specific call
[0014] It is error-prone due to manual interaction
[0015] Another sub-optimal solution would be that the BSC always accepts the bearer type offered from MSC in the handover request. If it cannot use the codec selected on the radio link on the terrestrial interface, then BSC should use another offered codec type. This solution has the following disadvantages:
[0016] The operator has to provide transcoder resources in the BSC to cover the described scenario
[0017] Inserting a transcoder in the BSC and using compressed speech codec on the terrestrial interface reduces speech quality and increases the delay in the speech path
BRIEF SUMMARY OF THE INVENTION
[0018] The present invention pertains to a method for using a network entity of a radio communication network. The method comprises the steps of seizing a first resource and a second resource for a terrestrial interface of the network, where the first resource is distinct and different from the second resource. There is the step of sending a handover request message identifying the first resource and the second resource.
[0019] The present invention pertains to a network entity for a radio communication network. The entity comprises a processing unit which causes a first resource and a second resource for a terrestrial interface of the radio network to be seized, where the first resource is distinct and different from the second resource. The entity comprises a network interface through which a handover request message identifying the first and the second resource is sent.
[0020] The present invention pertains to a method for using a network entity of a radio communication network. The method comprises the steps of seizing a first resource and a second resource for a terrestrial interface of the network, where the first resource is distinct and different from the second resource. There is the step of sending an assignment request message identifying the first resource and the second resource.
[0021] The present invention pertains to a network entity for a radio communication network. The entity comprises a processing unit which causes a first resource and a second resource for a terrestrial interface of the radio network to be seized, where the first resource is distinct and different from the second resource. The entity comprises a network interface through which an assignment request message identifying the first and the second resource is sent.
[0022] The present invention pertains to a network entity for a radio communication network. The entity comprises a network interface which receives a handover request message identifying a first resource and a second resource, the first resource distinct and different from the second resource. The entity comprises a processing unit that selects one of the first and second resources, allocates a radio channel associated with the handover, selects a bearer for a terrestrial interface and seizes resources for the interface.
[0023] The present invention pertains to a method for a network entity of a radio communication network. The method comprises the steps of receiving a handover request message identifying a first resource and a second resource, the first resource distinct and different from the second resource. There is the step of selecting one of the first and second resources. There is the step of allocating a radio channel associated with the handover. There is the step of selecting a bearer for a terrestrial interface. There is the step of seizing resources for the interface.
[0024] The present invention pertains to a network entity for a radio communication network. The entity comprises a network interface which receives an assignment request message identifying a first resource and a second resource, the first resource distinct and different from the second resource. The entity comprises a processing unit that selects one of the first and second resources, allocates a radio channel associated with the assignment, selects a bearer for a terrestrial interface and seizes resources for the interface.
[0025] The present invention pertains to a method for a network entity of a radio communication network. Any method comprises the steps of receiving an assignment request message identifying a first resource and a second resource, the first resource distinct and different from the second resource. There is the step of selecting one of the first and second resources. There is the step of allocating a radio channel associated with the assignment. There is the step of selecting a bearer for a terrestrial interface. There is the step of seizing resources for the interface.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] In the accompanying drawings, the preferred embodiment of the invention and preferred methods of practicing the invention are illustrated in which:
[0027] FIG. 1 shows an intra MSC, inter BSC, GSM to GSM handover procedure.
[0028] FIG. 2 shows inter BSC handover using AoTDM and AoIP of the present invention.
[0029] FIG. 3 shows improved inter BSC HO; BSC selects IP bearer for the terrestrial interface of the present invention.
[0030] FIG. 4 shows improved inter BSC HO; BSC selects TDM bearer for the terrestrial interface of the present invention.
[0031] FIG. 5 shows the selection of the IP bearer at call setup of the present invention.
[0032] FIG. 6 shows the selection of the TDM bearer at call setup of the present invention.
[0033] FIG. 7 is a block diagram of a network entity of the present invention.
DETAILED DESCRIPTION
[0034] Referring now to the drawings wherein like reference numerals refer to similar or identical parts throughout the several views, and more specifically to FIGS. 2 and 7 thereof, there is shown a network entity 10 , such as an MSC, for a radio communication network. The entity comprises a processing unit 12 which causes a first resource and a second resource for a terrestrial interface of the radio network to be seized, where the first resource is distinct and different from the second resource. The entity comprises a network interface 14 through which a handover request message identifying the first and the second resource is sent.
[0035] Preferably, the network interface 14 receives an acknowledgment of the handover. The processing unit 12 preferably detects that one of the first and second resources is selected for a bearer. Preferably, the processing unit 12 causes an unselected one of the first and second resources to be released.
[0036] The network interface 14 preferably sends the handover request message with a circuit identifier code of a selected time division multiplexing (TDM) circuit with respect to a TDM bearer, and with a transport address of a media gateway (MGw) that will terminate an IP connection with respect to an IP bearer.
[0037] The present invention pertains to a method for using a network entity 10 , such as an MSC, of a radio communication network. The method comprises the steps of seizing a first resource and a second resource for a terrestrial interface of the network, where the first resource is distinct and different from the second resource. There is the step of sending a handover request message identifying the first resource and the second resource.
[0038] Preferably, there is the step of receiving an acknowledgment of the handover. There is preferably the step of detecting that one of the first and second resources is selected for a bearer. Preferably, there is the step of releasing an unselected one of the first and second resources.
[0039] The sending step preferably includes the step of sending the handover request message with a circuit identifier code of a selected time division multiplexing (TDM) circuit with respect to a TDM bearer, and with a transport address of a media gateway (MGw) that will terminate an internet protocol (IP) connection with respect to an IP bearer. The transport address can include an IP address and a port number.
[0040] The present invention pertains to a method for using a network entity 10 , such as an MSC, of a radio communication network. The method comprises the steps of seizing a first resource and a second resource for a terrestrial interface of the network, where the first resource is distinct and different from the second resource. There is the step of sending an assignment request message identifying the first resource and the second resource.
[0041] Preferably, there is the step of receiving an assignment complete message that indicates a bearer shall be used on an A-interface user plane connection.
[0042] The present invention pertains to a network entity 10 for a radio communication network. The entity comprises a processing unit 12 which causes a first resource and a second resource for a terrestrial interface of the radio network to be seized, where the first resource is distinct and different from the second resource. The entity comprises a network interface 14 through which an assignment request message identifying the first and the second resource is sent.
[0043] The present invention pertains to a network entity 10 , such as a BSC, for a radio communication network. The entity comprises a network interface 14 which receives a handover request message identifying a first resource and a second resource, the first resource distinct and different from the second resource. The entity comprises a processing unit 12 that selects one of the first and second resources, allocates a radio channel associated with the handover, selects a bearer for a terrestrial interface and seizes resources for the interface.
[0044] Preferably, the network interface 14 sends an acknowledgment of the handover request. The acknowledgment request preferably includes information that identifies which bearer is used on the terrestrial interface.
[0045] Preferably, the handover request message is a BSSMAP handover request with a circuit identifier code of a selected time division multiplexing (TDM) circuit with respect to a TDM bearer, and with a transport address of a media gateway (MGw) that will terminate an IP connection with respect to an IP bearer.
[0046] The present invention pertains to a method for a network entity 10 , such as a BSC, of a radio communication network. The method comprises the steps of receiving a handover request message identifying a first resource and a second resource, the first resource distinct and different from the second resource. There is the step of selecting one of the first and second resources. There is the step of allocating a radio channel associated with the handover. There is the step of selecting a bearer for a terrestrial interface. There is the step of seizing resources for the interface.
[0047] Preferably, there is the step of sending an acknowledgment of the handover request. The acknowledgment preferably includes information that identifies which bearer is used on the terrestrial interface.
[0048] Preferably, the receiving step includes the step of receiving a BSSMAP handover request with a circuit identifier code of a selected time division multiplexing (TDM) circuit with respect to a TDM bearer, and with a transport address of a media gateway (MGw) that will terminate an IP connection with respect to an IP bearer.
[0049] The present invention pertains to a network entity 10 , such as a BSC, for a radio communication network. The entity comprises a network interface 14 which receives an assignment request message identifying a first resource and a second resource, the first resource distinct and different from the second resource. The entity comprises a processing unit 12 that selects one of the first and second resources, allocates a radio channel associated with the assignment, selects a bearer for a terrestrial interface and seizes resources for the interface.
[0050] The present invention pertains to a method for a network entity 10 , such as a BSC, of a radio communication network. The method comprises the steps of receiving an assignment request message identifying a first resource and a second resource, the first resource distinct and different from the second resource. There is the step of selecting one of the first and second resources. There is the step of allocating a radio channel associated with the assignment. There is the step of selecting a bearer for a terrestrial interface. There is the step of seizing resources for the interface.
[0051] There is preferably the step of selecting the bearer to be used on an A-interface user plane connection. Preferably, there is the step of sending an assignment complete message indicating the selected bearer.
[0052] Although this invention is explained with reference to 3GPP herein, the invention is not limited to 3GPP compliant networks but may encompass also other networks like the (W)iDEN compatible networks.
[0053] In the operation of the invention, to improve the inter BSC handover procedure for intra MSC or inter MSC handover scenarios, the handover can be either GSM to GSM handover or WCDMA to GSM handover or any other HO from any radio technology to GSM such as LTE to GSM.
[0054] MSC automatically detects if BSC can support IP on the terrestrial interface. Therefore, MSC monitors mobile originating and mobile terminating calls. As soon as BSC uses AoIP for any of those calls MSC marks the BSC as capable to support IP bearer. The call set-up procedure for AoIP supports that MSC and BSC are negotiating which bearer to use.
[0055] MSC seizes resources for the TDM bearer and the IP bearer before the handover request message is sent to BSC. Then BSC can choose any of the bearer types. In the BSSMAP Handover Request Acknowledge message the BSC informs the MSC about the selected bearer type. Finally MSC can release the seized resources from the not selected bearer type.
[0056] FIG. 2 shows the concept of the improved handover procedure. The numbers in the figure indicate the sequence of actions.
[0057] In a first step 1 , a BSC (source BSC) detects a handover condition and indicates in a second step 2 towards a MSC that a Handover is required. In a next step 3 , the MSC seizes TDM resources and resources for other bearer(s), e.g. IP for the terrestrial interface. Thereafter, in step 4 , a handover request is sent towards a further BSC (target BSC) including an indication about the seized resources. The further BSC (target BSC) selects a bearer for the terrestrial interface and sends an acknowledgement of said handover request in a further step 6 towards the MSC. Either within the acknowledgement or within any other appropriate message information which bearer is used on the terrestrial interface is provided towards the MSC. Finally, the MSC uses the provided information which bearer is used on the terrestrial interface in a step 7 to continue handover procedure, e.g. as defined in 3GPP. In addition, the MSC may also use provided information which bearer is used on the terrestrial interface to release the unused but seized resources for the other bearers.
[0058] The improvement for the inter BSC handover procedure is based on the following scenario:
[0059] Target BSC can support AoTDM and AoIP
[0060] Note: the MSC sending the handover request to the target MSC does not know in advance, which bearer BSC will select.
[0061] GSM to GSM or WCDMA to GSM handover is performed
[0062] MSC monitors the call set-up procedures for mobile originating and mobile terminating calls. Once BSC uses AoIP for any of those calls the MSC marks that BSC is capable using IP on the user plane.
[0063] The information whether a BSC supports AoIP may also be provided towards the MSC in a different manner, e.g. it might be administered via an O&M (Operations & Maintenance) tool.
[0064] During handover procedure, one MSC sends the BSSMAP Handover Request to the target BSC. This can be either the anchor MSC (intra MSC HO procedure or sub-sequent inter MSC HO back to anchor MSC), or in the non-anchor MSC (intra MSC in non-anchor MSC, inter MSC handover or sub-sequent inter MSC handover to another non-anchor MSC).
[0065] FIG. 3 shows a possible message flow that can be used for the proposed handover procedure. In this example the BSC selects IP bearer for the terrestrial interface.
[0066] The following steps are shown in FIG. 3 :
[0067] First the MSC detects a condition to request channel assignment from source BSC (step 1 ). This could be for example the reception of BSSMAP Handover Required message from BSC (intra MSC HO) or the reception of MAP Prepare Handover Request message (inter MSC HO).
[0068] Then MSC seizes a TDM circuit and IP resources for the terrestrial interface towards the target BSC. This involves MSC internal processes and in case of layered network architecture the MSC-S has to request MGw to seize a TDM termination and an IP termination (steps 2 - 5 ).
[0069] Then MSC sends the BSSMAP Handover Request message to the target BSC (step 6 ). This message includes the circuit identify code (CIC)—in case MSC allocates the CIC and a container (AoIP Container) used to transport IP address information from the MGW to the BSC.
[0070] BSC allocates the radio channel, selects the bearer for the terrestrial interface and seizes resources for this interface (step 7 ). Here, the BSC decides to use IP bearer.
[0071] In the acknowledgment message the BSC provides its user plane address information within the AoIP Container (step 8 ). MSC identifies that IP is selected for the bearer because it receives the AoIP Container.
[0072] MSC is passing the contents of the AoIP Container to the MGW (steps 9 , 10 ).
[0073] MSC releases the seized TDM resources. In layered architecture MSC request MGW to release the TDM termination (steps 11 , 12 ).
[0074] FIG. 5 shows the selection of the IP bearer at call setup (assignment).
[0075] FIG. 4 shows a second example for a possible message flow that can be used for the proposed handover procedure. In this example the BSC selects TDM as bearer for the terrestrial interface.
[0076] The steps 1 - 6 are equal to the case before, where BSC selected IP bearer for the terrestrial interface. The following steps are different:
[0077] BSC allocates the radio channel, selects the bearer for the terrestrial interface and seizes resources for this interface (step 7 ). In opposite to the previous example, here, the BSC decides to use TDM bearer.
[0078] BSC sends the acknowledgement message as defined in 3GPP for AoTDM (step 8 ). MSC identifies that TDM is selected for the bearer because it does not receive the AoIP Container.
[0079] MSC releases the seized IP resources. In layered architecture MSC request MGW to release the IP termination (steps 9 , 10 ).
[0080] Note, that in case BSC is responsible to allocate the CIC the following changes have to be applied to the examples above:
[0081] MSC does not provide a CIC in the Handover Request message (both examples).
[0082] If BSC select TDM bearer for the terrestrial interface it provides a CIC in the Handover Request Acknowledge message (first example).
[0083] FIG. 6 shows the selection of the TDM bearer at call setup (assignment).
[0084] Handover (HO) and assignment request are two independent functions. Assignment request is at call setup. It is mandatory to establish the radio connection (mobile terminal to antenna and further to the BSC node) and to connect that part with the core network.
[0085] Handover is a process that is performed during the call when the terminal is moving around. Different handover types can be distinguished: while moving the terminal may reach the area of a new antenna, a new radio coverage cell, an area that is controlled by another BSC or even an area that is controlled by another MSC. Further intersystem handover is possible, that means a calling subscriber starts a call in the 2G network and changes to the 3G network.
[0086] With respect to the invention herein, the relevant handover process is the inter BSC intra MSC (the BSC is changed, and both BSC nodes are controlled by the one MSC).
[0087] Not shown (but still possible) is inter BSC inter MSC HO. In this case BSC and MSC are changed. Not shown but still possible is the inter system handover where the target system is a GSM system. The source system can be any technology for example WCDMA or LTE.
[0088] With reference to FIGS. 5 and 6 , the following are the steps for Assignment.
[0089] 1. MSC detects a condition to perform call setup.
[0090] 2. MSC seizes a TDM termination to be used in case BSC selects the TDM bearer for the A-interface user plane connection later. In the ADD Request MSC specifies the TDM termination identifier to be seized (not shown). The TDM termination identifier can be mapped uniquely to the CIC used in this call.
[0091] 3. MGw replies on the ADD Request.
[0092] 4. MSC seizes an IP termination to be used in case BSC selects the IP bearer for the A-interface user plane connection later.
[0093] 5. MGw replies on the ADD Request.
[0094] 6. MSC sends BSSMAP Assignment Request message to trigger the channel assignment in the target BSC. MSC provides the CIC and the AoIP Container, where one of them is to be used for the call.
[0095] 7. BSC establishes the radio channel. Further BSC selects the bearer to be used on the A-interface user plane connection. In this example ( FIG. 5 ) BSC decided to use the TDM bearer.
[0096] 8. BSC sends Assignment Complete message back to MSC as specified in standard.
[0097] 9. From the received Assignment Complete message MSC deducts that TDM bearer (see FIG. 6 ). shall be used on A-interface user plane connection. MSC requests MGw to remove the previously seized IP termination.
[0098] 10. MGw confirms the SUB Request.
[0099] The present invention includes, but is not limited to, the following inventive steps:
[0100] MSC detects BSS capability to support IP on the terrestrial interface
[0101] MSC seizes a TDM and IP bearer before it request channel assignment from the target BSC
[0102] MSC releases unused resources after BSC selected a bearer and informed MSC about the decision
[0103] The invention has the following advantages:
[0104] MSC automatically detects if BSC is capable to support IP bearer for the terrestrial interface
[0105] The BSSMAP message defined for the 3GPP handover procedure and assignment procedure can be reused.
[0106] BSC has full freedom to select the bearer for the terrestrial interface.
[0107] No configuration in MSC or BSC is required
[0108] The procedure is only applicable for the case that AoIP and AoTDM are used in parallel.
[0109] The procedure can be removed and does not have any additional impact in case BSC supports on AoIP (proposed target solution for future networks).
[0110] The procedure supports CIC selection in MSC and CIC selection in BSC (for AoTDM)
[0111] Abbreviations:
[0112] (W)iDEN (Wideband) Integrated Digital Enhanced Network
[0113] 3GPP 3 rd generation Partnership Project
[0114] AoIP A-Interface (user plane) over IP
[0115] AoTDM A-Interface (user plane) over TDM
[0116] BSC Base Station Controller
[0117] BSS Base Station Subsystem
[0118] BSSMAP Base Station System Management Application Part
[0119] CIC Circuit Identity Code
[0120] GSM Global System for Mobile communications
[0121] HO Handover
[0122] iDEN Integrated Digital Enhanced Network
[0123] IP Internet Protocol
[0124] LTE Long Term Evolution
[0125] MGw Media Gateway
[0126] MSC Mobile Switching Center
[0127] MSC-S Mobile Switching Center Server
[0128] TDM Time-division Multiplexing
[0129] WCDMA Wideband Code Division Multiple Access
[0130] Although the invention has been described in detail in the foregoing embodiments for the purpose of illustration, it is to be understood that such detail is solely for that purpose and that variations can be made therein by those skilled in the art without departing from the scope of the invention except as it may be described by the following claims.
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Systems and methods related to performing an assignment and a handover in a radio communication network are provided. In one exemplary embodiment, a method performed by a Mobile Switching Center (MSC) of a radio communication network may include seizing resources for a Time Division Multiplexed (TDM) bearer and an Internet Protocol (IP) bearer for use on a terrestrial A-interface of the radio communication network for an activity to be performed by a target Base Station Controller (BSC) of the radio communication network. Further, the method may include sending, to the target BSC, an indication that requests the activity be performed by the target BSC and that also identifies the seized resources for the TDM bearer and the IP bearer for use on the terrestrial A-interface for the activity
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to an apparatus and method for measuring the resistance of superconductors. Structures of this type, generally, allow the resistance of the superconductor to be accurately measured in a non-destructive manner by using a bifilar coil which includes an integrated loop/switch formed from the bifilar coil.
2. Description of the Related Art
The use of superconductors for production devices has a problem in that the resistance (or absence thereof) of a long length of material cannot be easily measured nondestructively, i.e. without actually building the device and measuring its field accurately over time. The reason for this is that in producing the desired field, the current in the conductor also produces large forces on the conductor which require the conductor to be potted in a hard material, such as epoxy to avoid motion and consequent quenching of the superconductor.
One way to address this issue is to wind a bifilar coil, wherein two conductors are wound adjacent to one another so that current will flow in opposite directions when the winding is excited. The field thus produced is very low and the coil can typically be wound "dry" without concern about the forces, the resultant motion and quenching. This facilitates unwinding after a successful test and subsequent rewinding into the desired field-producing coil configuration. The bifilar coil can then be excited from its end leads and the voltage across the leads measured at a given current to infer the resistance of the conductor.
The measurement which is desired from such a screening test is one of the overall resistance of the length of superconductor together with any joints which may be present in it. Unfortunately, the resistance which is required for a persistent current device such as an MR magnet is very low, and therefore difficult to detect by voltage measurements. An estimate of the resistance level which must be attained for a given device can be made from an equation governing the behavior of a circuit with a series resistance (R) and inductance (L) (FIG. 1). For a given initial current I o at time 0, the current at time t is given by
I=I.sub.o e.sup.-tR/L (Eq. 1).
For example, the specification for field drift rate for an MR magnet is typically 0.1 ppm/hr. Solving Equation 1 for R/L with this desired current drift rate (the current and field are linearly related) yields R/L=2.8e -11 Ω/H. For a magnet with an inductance of 20 Henries, the overall coil resistance must be no greater than 5.6e -10 Ω. At a current of 150 A, the voltage generated by such a resistance is 83e -9 V. Because of thermally induced voltages in the sensing leads and at junctions, as well as, other effects, the accurate measurement of such a low voltage is very difficult-a typical limitation on accurate voltage measurement is perhaps 100e -9 V. Therefore, inference of resistance of the sample of superconductor from the measured voltage can lead to results which are not of the required accuracy.
Resistance tests of superconductors have been made in the past by measuring the voltage at a given current for long (up to 70,000 feet) and short (4-12 inches) lengths of conductor. Resistance has been measured from drift tests on individual loops of conductor, but this qualifies only that short length of material and is not useful for qualifying lengths which are required to wind a complete magnet. Therefore, a more advantageous system, then would be presented if the resistance of long lengths of superconductor could be measured in a non-destructive manner.
It is apparent from the above that there exists a need in the art for a system which measures the resistance of a superconductor, and which at least equals the voltage measurement accuracy of the known measurement systems, but which at the same time is capable of measuring long lengths of superconductor. It is a purpose of this invention to fulfill this and other needs in the art in a manner more apparent to the skilled artisan once given the following disclosure.
SUMMARY OF THE INVENTION
Generally speaking, this invention fulfills these needs by providing an apparatus for measuring the resistance of a superconductor, comprising a bifilar coil having a loop formed substantially integrally with said coil and a field measuring means located substantially adjacent to said loop.
In certain preferred embodiments, the bifilar coil is wound with paired conductors which carry current in opposite directions to minimize the field, and the forces created in the coil. The coil includes a loop which is formed from the radially outboard of the two paired conductors in the last (outboard) layer. The loop performs two functions with a heater attached. The loop acts as a switch to allow the bifilar coil to be ramped up to a desired current level, and the loop also acts as a field generator which can be used to infer the current in the conductor. The drift rate of the current, coupled with the known (calculated or measured) inductance of the bifilar coil, allows an accurate computation of the overall resistance of the coil and any joints therein.
A direct extension of the proposed concept performs the resistance measurement in a background magnetic field. The advantage of this method is that it allows exploration of the resistance of the tested conductor in the actual operating regime which it will see the when the conductor is wound into a magnet. This magnetic field may be imposed on the coil by a solenoidal or other suitable winding which is powered by a highly stable power supply, or which is separately rendered persistent with a superconducting switch. Background magnetic field effects on the desired field measurement are minimized by ensuring that the background field is orthogonal to the field of the loop and by using field measurement techniques which integrate the field around a loop which contains no part of the field coil.
In another further preferred embodiment, the resistance of the superconductor can be accurately measured in a non-destructive manner.
The preferred superconductor measurement system, according to this invention, offers the following advantages: ease of use; excellent resistance measurements characteristics; excellent economy; good stability; and high strength for safety. In fact, in many of the preferred embodiments, these factors of use, resistance measurement characteristics, and economy are optimized to an extent that is considerably higher than heretofore achieved in prior, known superconductor measurement systems.
BRIEF DESCRIPTION OF THE INVENTION
The above and other features of the present invention which will become more apparent as the description proceeds are best understood by considering the following detailed description in conjunction with the accompanying drawings wherein like characters represent like parts throughout the several views and in which:
FIG. 1 is a R-L circuit diagram for a superconducting coil, according to the prior art;
FIG. 2 is a circuit diagram for the switch/coil, according to the present invention;
FIG. 3 is a schematic illustration of the loop/switch for a bifilar winding, according to the present invention;
FIG. 4 is a second embodiment of the loop/switch for a bifilar winding;
FIG. 5 is a third embodiment of the loop/switch for a bifilar winding;
FIG. 6a is a schematic illustration of a apparatus for placing a background magnet field on a bifilar coil, according to the present invention;
FIG. 6b is a second embodiment of an apparatus for placing a background magnetic field on a bifilar coil; and
FIG. 6c is a third embodiment of an apparatus for placing a background magnetic field on a bifilar and a loop/switch for the bifilar coil.
DETAILED DESCRIPTION OF THE INVENTION
As discussed earlier, FIG. 1 is a prior art diagram for a R-L circuit 2 for a conventional superconducting coil. Circuit 2 includes power source (V) 4, resistor (R) 6 and inductor (L) 8.
As disclosed by the present invention, a more accurate measurement of the resistance of a length of conductor than is obtainable from voltage measurements can be obtained by connecting the conductor with superconducting joints in a closed loop circuit, inducing a current into it, and reading the field created by its current over a long time. Since the field varies linearly with the current, this amounts to measuring the current drift. The resistance of a length of conductor with an inductance L over a time interval Δt is given by
R=(0.05)L/Δt (Eq. 2).
A reasonable time interval over which to measure the field is one day, or 86,400 s. A bifilar coil typically wound of 70,000 feet of tape superconductor (enough to make a 0.5T MR magnet) has an inductance of about 1200 μH. This value is independent of the diameter and length of the coil, as it involves only the spacing between and the length of the two conductors. It may be derived as the inductance of a pair of parallel conductors carrying oppositely directed currents from Gauss' Law in the form: ##EQU1## where λ is the inductance in Henries/meter, g and w are the gap between and width of the conductors, respectively, and μ o is the magnetic permeability of free space. Alternatively, the inductance may be experimentally derived from measurement of the voltage required to create a given rate of current change in the coil. Such a measurement should be carried out over a region of no appreciable flux penetration into the superconductor, or preferably in the normal state but at low temperature so the resistive effects are minimized. Using the 1200 μH calculated value of inductance, from Eq. 3, the resistance from Eq. 2 corresponding to a 4% field drop over one day is 5.6e-10Ω. This is equal to the resistance value which must be measured. The 4% field measurement accuracy is well within the range of a Hall sensor.
This preferred test can be accomplished with a superconductor by attaching the current leads to form a parallel circuit having as one leg a short length of conductor (called a switch) which may be driven above its transition temperature with a small heater and as the other the bulk of the coil (see FIG. 2). In particular, FIG. 2 illustrates circuit 10 including power source 12, switch resistor 14 and coil resistor 16.
With respect to FIG. 3, the simplest embodiment of switch assembly 20 is formed by wrapping along the direction of arrow A a portion of the radially outermost turn of one conductor 24 of the paired bifilar conductors 22 around a mandrel 26 of the desired diameter in the opposite direction to that of the plural turn coil winding 21 formed by said bifilar conductors which is being wrapped in the direction of arrow B for a single turn to form switch 28 on mandrel 26 before it rejoins the radially outermost turn of the other conductor 30 to complete the final turn of the bifilar coil with a pigtail-type joint 32. In order to induce the desired current in coil winding 21, switch 28 is turned normal by powering a conventional heater 34 attached to switch 28 by conventional fasteners, energizing power leads 36, and allowing the current to stabilize. The currents flowing in the coil (I c ) and the switch (I s ) are determined from the resistances of the two sides of the circuit and the power supply current I p by the equations ##EQU2## which can be rearranged as ##EQU3##
The switch resistance which can be generated by heating a length of tape superconductor is governed by the resistivity of the copper stabilizer in the tape, which has a resistivity ratio of about 75 which indicates a low temperature (4-20K) resistivity of about 2.27e-8Ω/cm. The copper, preferably, is 0.015 cm thick and 0.3 cm wide, so the resistance per unit length is 5μΩ/cm. Therefore, a conventional 1 inch heater will produce a resistance of about 13μΩ. Note that the tape temperature is below the transition temperature very close to the boundary of the heater because of the excellent thermal conductivity of the copper in the tape, so the length of the normal region in the switch is essentially equal to the length of the heater. Since the coil resistance is unknown, the fraction of the current which circulates in the coil will also be unknown. However, a desirable coil resistance is in the nΩ range. Using 13 nΩ as a working value, the coil current will be 0.999I p . Should the resistance of the coil be significantly higher then 13nΩ, it will not affect the ability of the apparatus to yield an accurate resistance measurement. This is determined solely from field drift rate and inductance. But the current at which the resistance is measured will be a smaller fraction of the power supply current. Even at a coil resistance of 1.3 μΩ, the coil current will still be about 0.91I p . This is not seen as a significant drawback to this testing method.
The placement of the field sensor is an important part of the proposed testing technique, because there are fields generated by means other than the transport current in the superconductor. These means include circulating currents which are driven by changes in magnetic flux in the region of the conductor and Meissner effect currents. Fortunately, these fields drop off as a higher power of the distance from the coil than does that produced by the transport current. In order to ensure that the effects of the fields from circulating currents are minimal, the field sensor must be placed sufficiently far from the coil that the transport current field dominates the reading. For instance, while the center of the switch loop is an attractive place to position the sensor, the field from circulating currents in the main coil at that position may be substantial. Since the bifilar coil actually produces a finite field at a distance away from the coil where the circulating current field is small, the field of the loop is not required for the measurement. In fact, a location distinct from the center of the loop is preferred.
Thus far the geometry has been presented in which the loop extension from the coil is in a plane perpendicular to the axis of the bifilar coil. While this is the easiest winding geometry, especially for tape conductor, it presents a difficulty because the principal fields of the bifilar coil and the loop extension are in the same direction. With respect to FIG. 4, in order to minimize the effects of the field of the bifilar coil, the loop extension or switch 28 may be aligned with its plane perpendicular to the direction of arrow C along the azimuthal (circumferential) direction (the direction of arrow B of the bifilar coil winding 21). Since the bifilar coil field has only radial and axial components, Hall sensor 38 measures only the field of the loop extension or switch 28, which is preferred. Three other preferences for the loop extension 28 location relative to the coil 21 are:
1. radially far from the coil winding 21 (provided a large radius dewar is available);
2. axially far from the coil winding 21 (provided a large height dewar is available);
3. reaching to a location which allows placement of Hall sensor 38 on the bifilar coil winding axis.
With respect to FIG. 5, the measured field contributions from Meissner effect circulating currents in the tape superconductor comprising the loop extension or switch 28 can be eliminated by coupling a ring 52, preferably, made of ferrite, mild steel, or other suitable ferromagnetic material to the loop extension or switch 28. Ring 52 has a gap 56 in which a Hall sensor 38 could be placed to measure the flux circulating in the ring, without being affected by the field of the bifilar coil winding 21 or the circulating currents in the loop extension or switch 28. The current sensitivity expression for the loop extension is: ##EQU4## where I is the transport current in the loop, dl the differential length along the iron ring, B the flux density in the ring, μ rel the relative permeability of the ring, and μ o is the magnetic permeability of free space. The calibration of ring 52 is achieved by winding a coil 54 on the ring 52 in a toroidal fashion such that any magnetic flux change in ring 52 will induce a current in the toroidal coil 54. Coil 54, preferably, is constructed of copper. Note that the toroidal or calibration coil 54 need not be a complete toroid, but may be only cover part of the circumference of the ring 52. In the linear range of a conventional B-H curve for the ferrite or soft iron ring 52, the toroidal current is linearly dependent on the current in the loop extension 28.
The same toroidal calibration coil 54 can be used to null out the field of the loop extension or switch 28 for the purpose of improving the accuracy of measuring the deviation from that null. In this configuration, the temporal stability of Hall sensor 38 can be enhanced by reducing the contribution of loop extension or switch 28 and by using a conventional highly stable calibrated current source, such as, is used in the powering Hall sensor 38 itself. A temporal stability of about 10 ppm has been achieved in this manner.
With respect to FIGS. 6a-6c, an improvement in the measurement and the information which may be derived therefrom can be realized by operating all or part of the bifilar coil winding 21 in a background magnetic field 104 of background field assembly 100. Since the conductor under test will eventually be wound into a field-producing coil, it will operate in a field. The characteristics of a superconductor vary depending on the field, so it is best to measure the resistance of the test length of conductor in a background field 104 which approximates that in which it will operate. Several alternatives for producing such a field with a solenoidal coil 102 are described here:
1. Place solenoid 102, which is small relative to the bifilar coil, winding 21 against the side flange of the bifilar coil winding 21, thus exposing part of the bifilar coil winding 21 to field 104 (FIG. 6a);
2. Insert the bifilar coil winding 21 in the bore of a large solenoid 102 (FIG. 6b);
3. Insert the bifilar coil winding 21 in the radial gap between two solenoids 102a and 102b which produce fields 104a and 104b, respectively, in the same direction in the gap (FIG. 6c). This option allows a fairly low field 104a and 104b to be generated in the central region of the interior field coil, where very convenient measurements free of background field can be made that include all features of the Hall sensor 38, loop extensions or switch 28 and rings 52.
The stabilizing of the background field coil current can be accomplished by using a commercially available highly stable power supply (available to stability levels of 10 ppm or better) or a superconducting switch. In fact, an acceptable level of insensitivity to field fluctuations can be achieved with a standard power supply (100 ppm or so) because the mutual inductance between the background field solenoid 102 and the bifilar coil 21 is reduced by the ratio of the volume of the bifilar winding to the cylindrical volume enclosed by the bifilar coil 21. This ratio is about 4%, so a 100 ppm stability in the power supply for the background field coil 102 translates into a 4 ppm stability of the bifilar persistent current loop. This value is much better than the resolution of the Hall sensor measuring device and the ferrite coil coupling.
Once given the above disclosure, many other features, modifications and improvements will become apparent to the skilled artisan. Such features, modifications and improvements are, therefore, considered to be part of this invention, the scope of which is to be determined by the following claims.
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This invention relates to an apparatus and method for measuring the resistance of superconductors. Structures of this type, generally, allow the resistance of the superconductor to be accurately measured in a non-destructive manner by using a bifilar coil which includes an integrated loop/switch formed from the bifilar coil.
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FIELD OF THE INVENTION
This invention relates to the production of wood I-beams and more particularly it relates to the machinery and process for assembly and securing the flanges and web together to produce I-beams.
BACKGROUND OF THE INVENTION
Overhead support beams used for building structures have long been made of wood as well as steel. Whereas steel beams are typically in the form of what are referred to as I-beams, having upper and lower flanges connected by a web and thus resembling the letter I, wood beams have historically been made in the form of rectangles, i.e., 4"×6", 4"×8", etc. A restriction on the use of rectangular wood beam supports is the size of a beam that can be produced from available tree sizes which over the years have become smaller and smaller.
A process of producing wood I-beams has been developed which does not rely on tree or log size. Flanges are produced by the process referred to as LVL or laminated veneer layers and the web between the flanges is produced by the process referred to as OSB or oriented strand board. The LVL process stacks sheets of veneer that are typically 4' wide and 8' long and, e.g., 0.1" thick. The ends of the sheets are scarfed and end spliced together (glued) to extend the length as desired. The spliced ends of overlying sheets are staggered to produce a consistent strength throughout the length and the elongated stacks are cut into strips, e.g., having a thickness of 11/2" to 31/2", a width of 4" and a length of 28' to 65'.
The OSB process involves first reducing a wood material to strands which are then oriented in a common direction to produce strand layers. Alternating overlying layers have the strands oriented 90° from the underlying layers and the layers are added as desired to achieve the desired thickness. Again the boards produced from the strands are cut into strips to achieve the thickness, e.g., 3/8" and width, e.g., 71/2" as desired for the web of the I-beam. The webs are not continuous and, e.g., 4' or 8' lengths are end butted between the flanges to produce the desired lengths of the I-beams.
The challenge then is to assemble the web strips (webs) and flange strips (flanges) together as an I-beam. In a known process, the web segments are provided with tapered side edges of a precise configuration and the flanges are provided with mated grooves. Glue is applied to the tapered sides and/or grooves and as the components are conveyed along a path, the flanges are guided onto the tapered side edges at each side of the web and the assembly of the center web and side flanges is compressed between rollers to squeeze the tapered side edges of the web into the grooves of the flanges. The compression rollers insure that the overall dimension between the outside faces of the flanges conforms to an established dimension, i.e., the dimension intended with the side edges of the web properly seated in the grooves of the flanges.
The above process has at least three deficiencies to which the present invention is directed. As the flanges and web are brought together and compressed, any variation in the groove size, tapered side edges, glue deposited or even surface imperfections (within the groove or on the tapered edges) will cause one side of the web to be more resistive to being seated in the groove than the other side. The result may be that one side is inserted to a greater depth than the other which produces bowing or skewing of the beam and can even produce cracking of a flange.
The process is continuous, e.g., producing repeated 28' to 65' I-beams with the flanges following one after the other as they are guided into the assembly process. The LVL board lengths (from which the flange strips are generated) are typically not precisely the same lengths (e.g., there can be 1/4" variance in a 30' to 65' length), and accordingly as the flanges from one board follow another board, there can be a slight disparity between the lengths of the flanges from one side of the I-beam to the other. Whereas a slight disparity can be tolerated, a series of mismatches compounds the difference and produces an unacceptable disparity. This requires periodic resetting of the stream of flanges and on occasion generates a rejected I-beam which is too short for that run of I-beams and will have to be cut down to a shorter standardized length. This is a costly waste of production and undesirable.
The third deficiency is the required shut down for resetting of the machinery when a change to a different I-beam size is required. There are numerous machines involved and all or most require adjustment relative to the conveyor when the I-beam depth or flange size is varied. This shut down is extremely expensive and reducing the shut down time is highly desirable.
BRIEF SUMMARY OF THE INVENTION
The process of the present invention departs from the manner by which the flanges are fit to the web, i.e., the prior process being to force the two flanges onto the web at a pre-set width determined from the outside face of one flange to the outside face of the other flange. (The reader will understand that the term "width" is used to measure the lateral dimension during processing. When installed during construction, the I-beam is rotated 90 degrees and the width dimension as used here then becomes the height dimension.)
In the present invention, the desired web path is established and the web is fixed in that path by a clamping action of the conveyor. In the preferred embodiment, the web is conveyed using upper and lower conveyors (one being a sharp chain conveyor) to clamp and hold the web in the centered position. The desired half width, i.e., as between the center of the web and the outer side (outside face) of the flange is determined. The flanges are guided and urged into the seated position for each side of the web and the pressure rollers that urge the flanges onto the web sides are prevented from applying excessive pressure. Thus, each of the flanges are urged to a prescribed fixed position measured from the fixed center line of the web. If one side is more resistive to assembly, that resistance will not be transferred to the other side. In the event that one side cannot be properly assembled onto the web, the pressure rollers will release and sensors will signal the existence of a flawed section in the I-beam. The accepted I-beams will not have one flange more deeply seated than the other to which can happen in the prior process.
As concerns the problem of accumulating a length disparity as between the flanges, the first improvement is the feeding of flanges to the conveyor in alternating fashion. That is, the flanges that are cut from, e.g., a 48" LVL board into thirty-two 11/2"flanges are fed alternately to one side of the web and then the other. This is followed by thirty-two flanges cut from a next same board. As the flanges from the same board are exactly the same length, the accumulated length disparity as between the flanges of the two sides of the I-beam is greatly diminished. As concerns the disparity that eventually will unacceptably accumulate, the conveyor system is further provided with sensors to detect the discrepancy as between the leading ends of the pair of flanges. As the leading ends of the flanges pass the sensors, should one flange slightly follow the other, the drive roll speed under the flange that is leading is retarded to insure that the leading ends are fed evenly into the assembly process. The disparity of different length flanges is thereby prevented from accumulating. In that the saws that cut the I-beam to length following assembly are about 1/4" in width and the disparity is rarely greater than 1/4", the beams can be cut at the exact same length regardless of the disparity.
The problem of machine adjustment to different I-beam sizes is addressed. The automated process for assembling the flanges to the webs includes feeding the flanges edgewise in spaced apart relation, cutting elongated grooves along a center line at the inner side of both flanges, positioning a web between the flanges with the side edges aligned with the grooves and guiding the grooves of the flanges onto the side edges of the web. The machines that are involved in this process include, e.g., saws, conveyors and press rollers. The I-beam specifications change wherein the desired I-beam may have flanges 11/2", 21/2" or 31/2" in width and the web thickness may change between 3/8" to 1/2". Previously when this change was made to the automatic assembly, the conveyor for feeding the web remained fixed and the rest of the assembly machines were manually adjusted to accommodate the web height established by the conveyor.
Applicant's invention provides for at least partially automated changeover. In the preferred embodiment, the flange conveyor remains unchanged and the saw height, web conveyor and rollers are all raised or lowered to accommodate the flange height. All of the machinery is essentially adjusted to the location of the center groove in the flanges and this location changes as the flange width changes. For example, if converting from a 21/2" flange to a 11/2" flange with a 3/8" web, the web needs to be lowered to fit in the groove and is dropped down by one-half the difference in flange height. In the present example, this is 1/2". All of the machines that follow the groove height thus need to be lowered 1/2".
A separate support is provided for the flange conveyors and for the machines that have to be adjusted to the flanges, e.g., the web conveyor. The machines to be adjusted are supported on superimposed upper and lower wedge members (or cams) having mated interfaces angled relative to the underlying level support surface, e.g, by 3 degrees. The upper wedge member or cam is fixed to the machine base and the lower member is slidable. All of the movable wedge members or cams are rigidly tied together, e.g., with rigid rods. A pair of cylinders, one attached at each end of interconnected upper web members and tie rods, are controlled to pull the movable cam to either raise or lower the supported machinery. Each machine supported on the superimposed cam members is accordingly raised or lowered by the same amount which in the present case is 1/2".
The various features of the invention will be more fully appreciated and understood upon reference to the following detailed description and drawings referred to therein.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic illustration of a web and flanges being assembled;
FIG. 2 is a top view diagram illustrating the machine and process for assembling flanges to webs to produce I-beams in accordance with the invention;
FIG. 3 is a sectional view as taken on section lines 3--3 of FIG. 4 illustrating the machinery of FIG. 4 and the manner by which a web is positioned at a reference position between opposed flanges;
FIG. 4 is a top plan view of a sharp chain conveyor for transporting the web along a reference position;
FIG. 5 is a side elevation view of the sharp chain conveyor of FIG. 4;
FIG. 6 is view as viewed on view lines 6--6 of FIG. 4; and,
FIG. 7 is a view illustrating the height adjustment mechanism for elevating and lowering certain of the machine components relative to the flange conveyor.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention is a machine and process for assembling flanges to a web to produce I-beams. In this embodiment veneer layers are laminated together to produce the desired thickness of the flanges. The laminated veneer layers are produced in large sheets and strips having the desired width are simply sawn from the laminate sheet to produce the desired flanges. With reference to FIG. 1, milled tapered grooves 13 are provided in each flange 12 with the groove extending along the length and being positioned centrally on the inside of the flange. The webs 28 are produced by a process referred to as oriented strand board whereby wood fiber strands are layered to produce a desired thickness and cut into, e.g., 8' long strips having a width corresponding to the desired web lengths. The side edges 30 of the web strips (webs) are tapered to fit in the tapered grooves 13 of the flanges. Whereas the tapered groove and edges are deemed preferable, the primary objective here is to provide a mated fit between the groove and edges which may be accomplished with, e.g., straight sides, considered more difficult to produce and align for assembly purposes.
The diagram of FIG. 2 illustrates an assembly of machines and a process used to produce I-beams in accordance with the present invention. Flanges 12 and 14 are sawn from the base laminate sheet 10. Formed tapered grooves 13 are milled into the inner face of each of the flanges 12 and 14 (see FIG. 1) by a milling machine as indicated by the letter M in FIG. 2. The assembly machine has conveyors 18 and 20 for conveying the flanges 12 and 14 along the assembly path, the path being designated by arrow P. The flanges 12, 14 are transported on one side edge and the conveyors 18, 20 have a guide such as a trough to maintain the flange's side edge orientation. Sensors 22 are provided to sense the leading end of each of the flanges 12 and 14 as they are being conveyed on the conveyors 18 and 20. The sensors 22 will determine whether or not one of the ends of the flanges 12, 14 is leading the other. It is desirable that the flanges 12, 14 be transported with the leading ends in alignment to assure a proper assembly of the flanges 12, 14 to the web 28. Should one end of one of the flanges 12, 14 be leading, the conveyor transporting the leading flange is slowed down such that the leading end of the flanges 12, 14 come into alignment. The technology for accomplishing this control of one side versus the other is known, e.g., for aligning veneer sheets which process is more fully described in commonly owned U.S. Pat. No. 4,905,843.
As shown in FIG. 2, flange 12 is conveyed by conveyor 18 along one side of the assembly machine and flange 14 is conveyed by conveyor 20 along the opposite side of the assembly machine. The flanges 12, 14 are conveyed on edge with the grooves 13 of each flange facing the center of the assembly machine. The flanges 12, 14 are thus spaced apart a sufficient distance such that a web conveyor 26 may deliver a web 28 and place a web between the flanges 12 and 14. In this embodiment, the web conveyor 26 delivers the webs 28 from the side of the assembly machine. The web conveyor 26 places the web 28 at a known reference between the flanges 12 and 14 on a lug type conveyor 35.
In this embodiment the reference line 34 coincides with the centerline of the conveyance mechanism that conveys the web 28 along a path between the flanges 12 and 14. The reference line 34 thus also coincides with the centerline of the web 28 being conveyed between the flanges 12 and 14.
The web conveyor 26 conveys the webs 28 sequentially onto the lug type conveyor 35. The lug type conveyor 35 transfers the webs 28 in sequence to a roller type conveyor 38. Guide members 40 accurately position the web 28 on the roller type conveyor 38 so that the centerline of the web 28 coincides with the reference line 34.
The roller type conveyor 38 is of the pinch roll type that has bottom rollers 37 and top rollers 39 (see FIG. 3). The top rollers 39 are adjustably mounted and are movable toward and away from the bottom rollers 37 by a cylinder 41. The top roller 39 is essentially adjusted according to the thickness of the web 28. The roller conveyor 38 (rollers 37 and 39) conveys the web 28 onto a gripping conveyor such as a sharp chain conveyor generally indicated as 46 in FIG. 2. The sharp chain conveyor 46 has a lower chain conveyor 48 and an upper chain conveyor 50 as shown in detail in FIG. 5. The lower conveyor 48 and the upper conveyor 50 cooperatively grip or clamp the web 28 between them so that the web 28 will be accurately positioned and rigidly aligned on the conveyor such that the web 28 will not move laterally as it is being propelled by the sharp chain conveyor 46.
The roller conveyor 38 conveys the webs 28 at a higher rate of travel than the sharp chain conveyor 46. Sensors 36 are provided to sense the position of leading ends of the flanges 12, 14 and the first web 28. Succeeding webs 28 are forced into abutment with a preceding web 28 by the conveyor 38. The conveyor 38 has smooth rollers allowing the conveyor to slip when it has forced the succeeding web 28 into abutment with the preceding web 28.
Each succeeding pair of flanges 12, 14 have their leading ends aligned. The sensors 22, 36 determine whether or not the leading ends are in alignment. In this embodiment the I-beams are produced to the length of the flange pair (12, 14). The alignment of the ends of each pair of flanges eliminate any cumulative error due to length variation between flanges. After assembly, the I-beam is cut to the flange length by a known cut-off saw.
The flanges 12, 14 being conveyed by the conveyors 18 and 20 as the web 28 is conveyed by conveyor 46 are forced to converge toward the web 28 by guide rails 58, 60 illustrated in FIGS. 2 and 6. The guide rails 58, 60 force the flanges 12, 14 toward the web 28 to have the side edge 30 of the web 28 inserted into the grooves 13 of the flanges 12, 14 (FIG. 6).
Also, as shown in FIG. 6, each rail 58, 60 is independently controlled and moved by independent cylinders 62. Each cylinder 62 has sensors 64 to sense the position of the cylinder. Each rail 58, 60 is independently controlled to be positioned at a known distance from the reference line 34 (shown as a dot in FIG. 6). Rail 58 is set to urge the flange 12 onto the web 28 with the side edge 30 of the web 28 seated in the groove 13 of the flange 12. Similarly rail 60 is positioned to urge the flange 14 onto the web 28 with the side edge 30 seated in the groove 13 of the flange 14.
The sharp chain conveyor 46 rigidly clamping the web 28 prevents the web from moving laterally due to the forces exerted against the web 28 as the flanges 12, 14 are urged onto the web 28. None of the force exerted by the rails 58, 60 is transmitted to the opposite side of the assembly machine. The flanges 12, 14 are by the above arrangement mounted to the web 28 independent of each other. This assures that the flanges 12, 14 will both be properly mounted to the web 28.
In the event that the flange 12 or the flange 14 may not be seated onto the web 28 due to physical limitations such as an improper groove, material in the groove that limits the insertion of the web into the groove and so forth, the rail in question and the corresponding cylinder 62 will be forced to move outwardly which is sensed by the sensor 64 to trigger a fault condition. This would alert the operator or the computer controlled program that there is a fault in the assembly of the flange to the web. That I-beam would be marked for a final inspection. Similarly, should a condition exist where one or the other or both of the rails 58, 60 move inwardly beyond the desired set point, the sensor 64 again would trigger a fault condition.
The specification for the I-beams can vary and it may therefore be necessary to change the set up of the assembly machine to accommodate a different I-beam specification. In this embodiment, the conveyors 18 and 20 which convey the flanges 12, 14 remain at a fixed height and the conveyance mechanism and related equipment that conveys the web 28 is adjusted to suit a change in the height of the flanges 12, 14. When the dimensions of the flanges 12, 14 are changed, the grooves formed in the flanges 12, 14 will be at a different height relative to the conveyance mechanism for the web 28. It is therefore necessary to adjust the conveyance mechanism for the webs 28 such that the edges of the web 28 will be aligned and may be inserted into the grooves 13 formed in the flanges 12, 14. Other machine components may be adjusted as well, e.g., the saws for cutting the grooves.
FIGS. 7 (and 5) illustrates the manner of adjusting the central conveyance system for the webs 28. The central conveyance system is supported on multiple base units 80. A cam member 82 is mounted to each base unit and is slidably movable on the base unit 80. The cam member 82 has an inclined upper surface 83. Frame members 84 which support the central conveyance system are supported on the cam member 82. The base of the frame member 84 has an inclined surface 86 (follower) that mates the surface 83 of the cam member 82. Each cam member 82 is rigidly coupled to an adjacent cam member by tie rods 90. A cylinder 96 (mounted to a base unit 80) is coupled to one end cam member 82. The cylinder 96 will move the cam members 82 in the direction indicated by arrow 100. The cam members 82 will all move in the direction indicated by arrow 100 since they are coupled together by the tie rods 90. Another cylinder 98 is coupled to the opposite end cam member 82. The cylinder 98 will move the cam member in the direction indicated by arrow 102. Each of the frame members 84 have guide members 106 that prevent the frame members 84 from moving in a horizontal plane. The guide members 106 guide the movement of the frame members in the vertical plane.
When the cylinder 96 is activated to move the cam members 82 in the direction indicated by arrow 100, the inclined surface of the cam members underlying and supporting the frame members 84 is lowered and thus the central conveyance mechanism is lowered. When the cylinder 98 is activated to move the cam members 82 in the direction indicated by arrow 102, the supporting surface of the cam members 82 supporting the frame members is raised and will force the frame members 84 and thus the central conveyance mechanism to elevate.
It is important that the cams 82 all move exactly the same amount and the connections between the cams 82 and rods 90 cannot be allowed to have any slack between the connections, e.g., as may result from wearing. Tapered bolts in conjunction with spring type washers may be used for the connectors between these components which can be tightened periodically to take up any slack resulting from wear.
Those skilled in the art will recognize that modifications and variations may be made without departing from the true spirit and scope of the invention. The invention is therefore not to be limited to the embodiments described and illustrated but is to be determined from the appended claims.
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A machine and process for assembling flanges to a web to produce an I-beam. The machine has conveyors for conveying each flange and a separate conveyor system for conveying the web. The web is rigidly held to prevent lateral movement as the flanges and web are assembled. The conveyance mechanism for the webs is adjustable upwardly and downwardly to accommodate changes in the flange dimension and web thickness. The conveyance mechanism for the web is mounted on inclined ramps. Movement of the conveyance mechanism in one direction elevates the conveyance mechanism and movement in the other direction lowers the conveyance mechanism. The flanges as conveyed are sensed and relatively adjusted to assure alignment of the leading ends.
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BACKGROUND OF THE INVENTION
The present invention relates to a method for producing FRP screw-like fastening elements. The screw-like fastening elements include various screws and rivets. These screws and rivets may be preferably used for aircraft or the like.
Screws made of plastic material have been utilized in various field, for example the aircraft field, because of their lightness and high corrosion resistance. As the name FRP (fiber reinforced plastic) suggests the plastic material is frequency reinforced with fibers in order to improve the mechanical strength. Carbon fibers are mainly utilized as the reinforcement fibers.
Conventionally, FRP screws are manufactured in such a method that a rod plastic material including carbon fibers embedded along the length of the rod is prepared, and then a thread or threads are formed on an outer peripheral surface of the material by machining.
However, when the thread or threads are formed, the fibers which are embedded at a radial outer portion to be the thread groove are torn to pieces. Thus the thread portion has a low mechanical strength in comparison with that of the bulk of the screw. The thread portion does not have enough reinforcement advantage, so it is fragile and can be broken sometimes.
In this regard, another manufacturing method for FRP screws was proposed. As shown in FIG. 1, first, high strength fibers 2 are applied into a matrix of thermoplastic resin 4. The thermoplastic resin 4 is formed by extrusion molding or drawing into a rod material 6. In this time, fibers 2 are arranged in a row along a direction of the length of the rod material 6. The thermoplastic resin 4 is a light and strong material, e.g., a polyether-etherketone resin. The fibers 2 are, e.g., carbon fibers. The material 6 preferably includes carbon fibers 4 constituting 30-80% of the weight, and more preferably 60-70%.
Next, the rod material 6 is cut to have a prescribed length and disposed into a metallic mold 8 as shown in FIGS. 2 and 3. The mold 8 comprises a pair of half mold members 10 and 12. Each of the mold members 10 and 12 includes a semi-circular mold surface which has small grooves carved therein, the grooves forming a thread and threads when the half separated mold members 10 and 12 are combined together. As shown in FIGS. 4 and 5, the material 6 is heated and pressed between the half mold members 10 and 12, to form a screw 14 which has a thread and threads shaped by the small groove. Then, mold members 10 and 12 are separated again to take out the manufactured screw 14. The thread portion includes fibers 2 which are not damaged, having sufficient strength.
However, in the above method, if the plastic material 4 is excessive, the manufactured screw 14 will have burrs 16, so that it is necessary to deburr or reject the screw. If the plastic material is insufficient, the screw will be defective and must be rejected.
Furthermore, the pressure to form the screw 14 is limited by the capacity of the mold and the volume of the material. The pressure is also limited in order prevent the occurrence of deburr 16. Therefore, the material 6 is not subjected to a large pressure. If the material 6 includes defects such as cavities, the cavities may remain in the manufactured screw 14. Consequently, the manufactured screw 14 sometimes does not have a prescribed strength.
In addition, the above-described method is not suitable for producing a screw with a head, because the rod material 6 is originally of a uniform cross section.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide a method for producing an FRP screw-like fastening element which has sufficiently strong threads.
It is another object of the present invention to provide a method for producing an FRP screw-like fastening element, in which it is easy to manage the accuracy of the element's dimensions, so that any deburring is unnecessary, and no screws are rejected.
It is a further object of the present invention to provide a method for producing an FRP screw-like fastening element with a head, and in which is easy to manage the accuracy of the screw's dimensions.
According to a method of producing an FRP screw of a first embodiment of the present invention, the method comprises the steps of: (a) preparing a rod material including an elongated matrix formed of a plastic material and a plurality of elongated parallel fiber elements embedded within the matrix along the length of the matrix, the fiber elements having melting points substantially higher than the softening point of the matrix; (b) placing the prepared rod material within a cylindrical molding wall in such a manner that the longitudinal axis of the rod material is generally aligned with the axis of the molding wall, the molding wall having an internal thread formed thereon; (c) heating the placed rod material to a temperature not less than the softening point of the matrix; (d) inserting a stick member into the heated rod material along the longitudinal axis of the rod material so as to laterally expand the rod material and to bring the peripheral face of the rod material into contact with the entire molding wall, thereby an external thread is formed on the peripheral face of the rod material; (e) cooling the thread-formed rod material to a temperature lower than the softening point of the matrix; and (f) taking the cooled rod material out of the molding wall.
According to a method for producing an FRP screw of a second embodiment, the method comprises the steps of: (a) preparing a rod material including an elongated matrix formed of a plastic material and a plurality of elongated parallel fiber elements embedded within the matrix along the length of the matrix, the fiber elements having melting points substantially higher than the softening point of the matrix; (b) placing the prepared rod material within a cylindrical molding wall in such a manner that the longitudinal axis of the rod material is generally aligned with the axis of the molding wall, the molding wall defining a generally cylindrical first molding chamber and having an internal thread formed thereon; (c) heating the placed rod material to a temperature not less than the softening point of the matrix; (d) axially pressing the heated rod material so as to laterally expand the rod material and to bring the peripheral face of the rod material into contact with the entire molding wall, whereby an external thread is formed on the peripheral face of the rod material; (e) cooling the thread-formed rod material to a temperature lower than the softening point of the matrix; and (f) taking the cooled rod material out of the molding wall.
In accordance with a method for producing an FRP screw of a third embodiment, the method comprises the steps of: (a) preparing a rod material including an elongated matrix formed of a plastic material and a plurality of elongated parallel fiber elements embedded within the matrix along the length of the matrix, the fiber elements having melting points substantially higher than the softening point of the matrix; (b) placing the prepared rod material into a molding chamber, the molding chamber including an internal surface of a generally semi-circular cross section, the internal surface having an internal thread formed thereon, the rod material being placed in the molding chamber in such a manner that the longitudinal axis of the rod material is generally aligned with the axis of the internal surface of the molding chamber; (c) heating the placed rod material to a temperature not less than the softening point of the matrix; (d) pressing the heated material perpendicularly to the axis thereof by a ram which has a plane surface facing to the internal surface of the molding chamber, thereby forming a half round bar from the material, the half separated round bar being generally in the form of half a round bar that has been cut at a plane including a center axis thereof, the half bar having an external thread on the peripheral face thereof; (e) cooling the thread-formed half round bar to a temperature lower than the softening point of the matrix; (f) taking the cooled half round bar out of the molding chamber: and (g) joining the half round bar to another half round bar which is processed similarly to the half round bar to form a generally full cylindrical material the full cylindrical material having an external thread thereon.
In accordance with a fourth embodiment for producing an FRP screw of the present invention, the screw to be produced has a thread portion and a head of which the cross section is larger than that of the thread portion. The method includes the following steps of a primary molding process and secondary molding process. The primary molding process includes the following steps of: (a) preparing a rod material including an elongated matrix formed of a plastic material and a plurality of elongated parallel fiber elements embedded within the matrix along the length of the matrix, the fiber elements having melting points substantially higher than the softening point of the matrix; (b) placing the prepared rod material of the screw into a molding chamber, the molding chamber including an internal surface of a semi-circular cross section, the internal surface having a small diameter portion and a large cross section portion communicating concentrically to the small diameter portion, the material being placed in the molding chamber in such a manner that the longitudinal axis of the rod material is generally aligned with the axis of the internal surface of the molding chamber; (c) heating the placed rod material to a temperature not less than the softening point of the matrix; (d) pressing the heated material perpendicularly to the axis thereof by a ram which has a plane surface facing to the internal surface of the molding chamber, thereby forming a half round bar from the material, the half round bar being generally in a form of half a round bar that has been cut at a plane including a center axis thereof, the half bar having an end portion and other portion, the end portion being of a radius larger than the radius of the other portion; (e) cooling the half round bar to a temperature lower than the softening point of the matrix; and (f) taking the cooled rod material out of the molding chamber. The secondary molding process includes the following steps of: (g) joining the half round bar to another half round bar which is processed similarly to the half round bar to form a generally full cylindrical material, the full cylindrical material having a head portion of a larger cross section constituted by the end portion; (h) placing the full cylindrical material within a cylindrical molding wall in such a manner that the longitudinal axis of the rod material is generally aligned with the axis of the molding wall, the molding wall including a large cross section portion for receiving the head portion and small diameter portion having an internal thread formed thereon to receive the portion except for the head portion of the full cylindrical material; (i) heating the placed full cylindrical material to a temperature not less than the softening point of the matrix; (j) inserting a stick member into the heated full cylindrical material along the longitudinal axis of the full cylindrical material so as to laterally expand the full cylindrical material and to bring the peripheral face of the full cylindrical material into contact with the entire molding wall, thereby an external thread is formed on the peripheral face of the full cylindrical material; (k) cooling the thread-formed full cylindrical material to a temperature lower than the softening point of the matrix; and (l) taking the cooled full cylindrical material out of the molding wall.
According to the fourth embodiment, a rivet can be produced as well as the screw. The rivet to be produced has a shank portion and a head with a cross-section larger than that of the shank portion. In accordance with the fourth embodiment for the rivet, the method comprises the steps of: (a) preparing a rod material including an elongated parallel fiber elements material and a plurality of elongated parallel fiber elements embedded within the matrix along the length of the matrix, the fiber elements having melting points substantially higher than the softening point of the matrix; (b) placing the prepared rod material of the rivet into a molding chamber, the molding chamber including an internal surface of a semi-circular cross section, the internal surface having a small diameter portion and a large cross section portion communicating concentrically to the small diameter portion, the material being placed in the molding chamber in such a manner that the longitudinal axis of the rod material is generally aligned with the axis of the internal surface of the molding chamber; (c) heating the placed rod material to a temperature not less than the softening point of the matrix; (d) pressing the heated material perpendicularly to the axis thereof by a ram which has a plane surface facing to the internal surface of the molding chamber, thereby forming a half round bar from the material, the half round bar being generally in the form of half a round bar that has been cut at a plane including a center axis thereof, the half bar having an end portion and the other portion, the end portion being of a radius larger than the radius of an other portion; (e) cooling the half round bar to a temperature lower than the softening point of the matrix; (f) taking the cooled rod material out of the molding chamber: and (g) joining the half round bar to another half round bar which is processed similarly to the half round bar to form a generally fully cylindrical material, the fully cylindrical material having a head portion of a larger cross section constituting the end portion.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view showing a screw-like fastening element of a material such as FRP according to the prior art and also according to various preferred embodiments of the present invention.
FIG. 2 is a sectional side elevation showing a metallic mold for producing the FRP screws according to the prior art.
FIG. 3 is a cross-sectional view showing the mold along the III--III line of FIG. 2.
FIG. 4 is a sectional side elevation showing the metallic mold during production of an FRP screw.
FIG. 5 is a cross-sectional view showing the mold along the V--V line of FIG. 4.
FIG. 6 is a sectional side elevation showing a metallic mold including the material, and a pressure stick used in a method according to a first embodiment of the present invention.
FIG. 7 is a sectional side elevation showing the mold and the stick during the molding process.
FIG. 8 is a sectional side elevation showing another metallic mold including the material, and another stick used in a modification of the first embodiment, during the molding process.
FIG. 9 is a sectional side elevation showing a metallic mold including the material, and a ram used in a method according to a second embodiment of the present invention.
FIG. 10 is a sectional side elevation showing the mold and ram during a primary molding process of the second embodiment.
FIG. 11 is a perspective view showing a head core to be embedded into a product made by the primary molding process.
FIG. 12 is a sectional side elevation showing the mold and ram during a secondary molding process for uniting the product and the head core.
FIG. 13 is side view showing a unitary screw made by the secondary molding process.
FIG. 14 is a front sectional elevation showing a mold containing the material, and a ram used in a method according to a third embodiment of the present invention.
FIG. 15 is a sectional side elevation showing the mold and ram along the XV--XV line of FIG. 14.
FIG. 16 is a sectional side elevation showing the mold and ram during a molding process.
FIG. 17 is a front elevation showing the mold and ram along the XVII--XVII line of FIG. 16.
FIG. 18 is a perspective view showing a product made by the molding process, that is, a half round screw.
FIG. 19 is a perspective view showing a finished half round screw.
FIG. 20 is a sectional front elevation showing a mold and ram used in a primary molding process of a method according to a fourth embodiment of the present invention.
FIG. 21 is a sectional side elevation showing the mold and ram of FIG. 20.
FIG. 22 is a sectional front elevation showing the mold and ram during a primary molding process of the fourth embodiment.
FIG. 23 is a sectional side elevation showing the mold and ram of FIG. 22.
FIG. 24 is a perspective view showing the mold and ram.
FIG. 25 is a perspective view showing a half shoulder round bar made by the primary molding process.
FIG. 26 is a perspective view showing a completed half shoulder round bar that is formed from the half round shoulder bar shown in FIG. 25.
FIG. 27 is a perspective view showing a united shoulder round bar which is made from a pair of the half bars shown in FIG. 26.
FIG. 28 is a perspective view showing a head core which should be embedded in the united shoulder round bar shown in FIG. 27.
FIG. 29 is a sectional side elevation showing a mold containing the material, and a pressure stick for a secondary molding process of the fourth embodiment.
FIG. 30 is a sectional side elevation showing the mold and stick during the secondary molding process.
FIG. 31 is a perspective view showing a united shoulder round bar formed by a method of a modification of the fourth embodiment of the present invention.
FIG. 32 is a sectional side elevation showing a subject matter of a mold used in the secondary molding of the modification.
FIG. 33 is a sectional side elevation showing a mold and pressure stick during the secondary molding of another modification of the fourth embodiment.
FIGS. 34 and 35 are side views showing modifications of the pressure stick used in the first and fourth embodiments of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Various preferred embodiments of the present invention will be described hereinafter with reference to accompanying drawings.
First Embodiment
A first embodiment is described as follows. First, as well as conventional method shown in FIG. 1, high strength elongated fibers 2 are applied into a matrix of thermoplastic resin 4. The thermoplastic resin 4 is formed by extrusion molding or drawing to form a rod material 6 of a circular cross section. At this time, fibers 2 are parallely arranged in a row along a direction of the length of the material 6. The thermoplastic resin 4 is a light and strong material, e.g., a polyether-etherketone resin. The fibers 4 are, e.g., carbon fibers. The material 6 preferably contains the fibers 2 constituting 30-80% of the material's weight. More preferably, the material 6 contains the fibers constituting 60-70% of the material's weight.
Next, the rod material 6 is cut to a prescribed length and inserted into a metallic mold 20 as shown in FIG. 6, and heated to soften but not to melt. In FIG. 6, the material 6 is cross-sectionally shown together with other elements.
The mold 20 is preferable for producing screws which have no head. The mold 20 consists of a first mold member 22 which has a plane face 28 for forming an end surface of the screw, a second mold member 24 for forming a lateral thread of the screw, and a third mold member 26 for forming another end surface of the screw. The second mold member 24 consists of a pair of half mold members 25 and 27 which are generally symmetric to each other and can be separated from each other. When the half mold members 25 and 27 are combined together, the second mold member 24 has a plane 30 which adequately fits against the plane face 28 of the first mold member 22, and a through hole 32 which is perpendicularly extending from the plane 30. The through hole 32 has an axis on a plane on which the half mold members 25 and 27 contact each other. The through hole 32 has an internally threaded portion and a circular smooth hole portion which are concentric to each other. The smooth hole portion, which is farther from the first mold member 22, is of a smaller diameter than the minor diameter of the internal thread portion. The third mold member 26 has a cylinder-shaped projection 34 which can be inserted into and adequately fits the smooth hole portion of the hole 32. The third mold member 26 has a guide hole 36 extending therethrough which is concentric with the projection 34, i.e., which is concentric with the hole 32. The rod material 6 is placed into the internally threaded portion of the hole 32 in such a manner that the longitudinal axis of the rod material 6 is generally aligned with the axis of the hole 32.
After that, a pressure stick 40 of a circular cross section is inserted into the guide hole 36, by a pressure device (not shown). The stick 40 is further advanced to be inserted into the heated rod material 6 along the longitudinal axis thereof as shown in FIG. 7. The stick 40 radially expands the rod material 6 and brings the peripheral face of the rod material 6 into contact with the entire threaded portion of the hole 32 so that the rod material 6 can have a thread on the peripheral surface so as to form a screw 42. The stick 40 remains and is embedded in the screw 42 so as to form a core of the screw 42. The forward end of the stick 40 is preferably sharpened like a pencil for smooth insertion.
The screw 42 is cooled to harden. The half mold members 25 and 27 of the second mold member 24 are separated from each other, to remove the screw 42. The stick 40 is cut along the end surface, that is A--A surface of the screw 42. At the end surface of the screw 42, a slit to be engaged with a screwdriver may be inscribed by machining. The stick 40 is preferably made of high compressive strength material, such as a steel or FRP similar in properties to the main portion of the screw 42. For exerting a high pressure on the screw 42, steel is more preferable for the material of the stick 40. However, in order to make light screws 42, FRP is more preferable as the material of the stick 40. It may be preferable to insert a steel stick into the rod material 6 and then replace the steel stick by an FRP stick as the core. The dimensions of the stick 40 are selected to be suitable for the dimensions of the screws 42, so as to produce adequate radial pressure to expand the rod material 6 into the internal thread of the second mold member 24.
In accordance with the method for producing FRP screws of the embodiment of the present invention, the fibers 2 remain uncut from one end to another end of the screw 42. The fibers 2 near the peripheral thread of the screw 42 are held in the thread form in such a manner that the fibers 2 bent to follow the zigzag (wavy cross sectional figure) of the thread of the screw 42. The pressure stick 40 exerts sufficient pressure on the material 6 (screw 42). Therefore, strong FRP screws with a similar strength thread portion can be produced. Furthermore, it is easy to manage the accuracy of the screw's dimensions.
If the stick 40 has a mechanical strength which is in excess of that of the FRP, the manufactured screw 42 with the stick 40 has higher tensional strength along its axis than that of the conventional screws which is made of only FRP.
While the stick 40 is cut off at the end surface of the screw 42 in the above embodiment, a stick which has a same length as the screw 42 can be used to omit the cutting process.
While the manufactured screw 42 has no head in the mentioned embodiment, a screw with a head can be manufactured as follows. In the method, the pressure stick has a head to be a counter sunk head of a screw when the stick is inserted into and embedded in the rod material. As shown in FIG. 8, in this regard, the stick 48 includes a rod core portion 50 whose end is preferably sharpened like a pencil, and head portion 52 which is in form of a counter sunk head of the screw and concentric to the core portion 50. Although the first mold member 22 is the same as that in FIGS. 6 and 7, the second mold member 54 which is separable the same as the second mold member 24 has a conical hollow 56 being concentric with the hole 32, for fitting the head portion 52. The third mold member 26 is substituted by a ram 58. The ram 58 has a circular projection 60 for thrusting the stick 48 into the material 6.
Using the mold shown in FIG. 8, the screw which has a counter sunk head is produced as follows. The material 6 is inserted into and placed in the threaded hole 32 of the second mold member 54 and heated to soften; and then the stick 48 is pushed by the ram 58 and inserted into the material 6. Consequently, the screw 62 can be manufactured in such a manner that the core portion 50 of the stick 48 is embedded in the screw's threaded portion, and the head portion 52 becomes the head of the screw 62. When the screw 62 is cool, the second mold member 54 is separated to remove the screw 62.
In the first embodiment, the stick 40 is of a simple circular cross section as shown in FIGS. 6 and 7. However, in order to improve physical contact between the remained stick 40 and the produced screw 42, the stick 40 preferably is of a shape shown in FIGS. 34 or 35. The stick 40 shown in FIG. 34 has a plurality of projections on the outer peripheral surface thereof. The projections are spaced apart from each other along the axis of the stick 40. The stick 40 shown in FIG. 35 has a thread formed on the outer peripheral surface thereof. Accordingly, slipping between the remained stick 40 and the screw 42 are prevented for producing the screw having high tensile strength.
Second Embodiment
Next, a second embodiment of the present invention will be described referring to FIGS. 1 and 9 through 13. The material 6 shown in FIG. 1 is also utilized in the second embodiment.
As shown in FIGS. 9 and 10, a mold 70 for molding a screw consists of a first mold member 72 for producing a cone-shaped head of the screw, and a second mold member 73 for producing a thread portion of the screw. The first mold member 72 includes a circular plate 76 for producing an edge of the head, and a cone-shaped projection 78 concentrically extending from the plate 76.
The second mold member 73 consists of a generally symmetric half separated upper and lower mold members 74 and 75. When the upper and lower mold members 74 and 75 are combined together, the second mold member 73 includes a circular positioning hole 80 which is adequate to be held in engagement with the circular plate 76 of the first mold member 72 and perpendicular to circular plate 76, a conical hollow 82 which is concentric to the positioning hole 80, and a through hole forming a first molding chamber 84 of a circular cross section and partially threaded, which is concentric to the positioning hole 80. The axis of the hole 80, hollow 82, and the hole 84 is on a plane in which the half mold members 74 and 75 contact each other. When the first and second mold members 72 and 73 are combined together, the apex of the cone-shaped projection 78 is located on the axis and the conical hollow 82 is parallel to and spaced apart from the cone-shaped projection 78, so that a conical second molding chamber in direct communication with the through hole 84 is formed therebetween. The through hole 84 includes an internal female threaded portion 86 at the end near the conical hollow 82, and a smooth portion 88 at the opposite end. The diameter of the smooth portion 88 is smaller than the minor diameter of the internal thread 86.
The rod material 6 is cut off to have a prescribed length and inserted into the hole 84 of the second mold member 73 in such a manner that the longitudinal axis of the rod material 6 is generally aligned along with the axis of the hole 84. Then, a primary molding process begins. The material 6 is heated to soften. Next, a ram 90 is advanced and inserted into the hole 84 by a pressure device (not shown). The ram 90 has a rod-like presser 92 of a circular cross section and a flange 94 concentrically attached to the presser 92. The presser 92 is of a length and a diameter the same as that of the smooth portion 88. The presser 92 has a circular recess 96 at the forward end thereof, whose diameter is smaller than that of the material 6. The depth of the recess 96 is selected to suit the capacity of the mold 70, the volume of the material 6, and the desired pressing ratio of the material 6.
Accordingly, the heated material 6 is axially pressed by the ram 90 as shown in FIG. 10. One end of the material 6 which is closer to the first mold member 72 spreads and broadens around the projection 78 and is injected into the second molding chamber under the guidance of the projection 78 and the hollow 82. Especially, because of the hole 96, the outer of the material 6 effectively flows into space. The rod material 6 also radially expands and the peripheral surface thereof is brought into contact with the threaded portion 86, whereby an external thread is formed on the peripheral surface. The flange 94 stops at an end surface of the second mold member 73.
Therefore, a half-finished screw 114 which has a cone-shaped head wall 116 and a thread portion 118 concentrically attached to the head wall 116 is produced from material 6. At the head wall 116, the continuous carbon fibers 2 align along the projection 78 and hollow 82. At the outer region of the thread portion 118, the fibers align along the zigzag of the thread. At the inner region of the thread portion 118, the fibers align along the screw's axis.
Then, the first mold member 72 is released from the second mold member 73. Next, a secondary molding process begins. A cone-shaped head core 120 shown in FIG. 11 is embedded into the cone-shaped head wall 116 in a coaxial relation. The head core 120 is made of FRP which is similar to the material 6. The head core 120 includes a positioning projection 122 at the center of a bottom surface thereof. The head core 120 is inserted into the head wall 116 of the half-finished screw 114 which still rests in the second mold member.
A forth mold member 124 is combined with the second mold member 73. The forth mold member 124 is a circular plate which is adequate to be fitted into the positioning hole 80 of the second mole member 73. The fourth mole member 124 has a positioning aperture 126 at the center of one of its plane surfaces, which engages with the positioning projection 122 of the head core 120. Thus, the half-finished screw 114 and head core 120 is surrounded by the second mold member 73 and the fourth mold member 124, in the manner that the half-finished screw 114 and the head core 120 is combined.
The half-finished screw 114 and the head core 120 are heated to be soft. The ram 90 is inserted into the hole 84 again, and presses the half-finished screw 114 and the heat core 120 to make them into a unitary screw 130. After the united screw 130 is cooled, the fourth mold member 124 is released from the second mold member 73, and the upper and lower mold members 74 and 75 of the second mold member 73 are separated from other, thereby enabling the united screw 130 to be taken out. Accordingly, the cone-shape head wall 116 is filled with the head core 120, so that the united screw 130 shown in FIG. 13 is obtained. The united screw 130 has the projection 122, and an unnecessary end portion 132 provided so the material 6 might have sufficient volume to receive a sufficient pressure. Therefore, the projection 122 and the unnecessary end portion is cut off from the main portion of the screw 130, along the two-dot-and-dashed lines in FIG. 13. A slot 134 to be engaged with a screw driver is inscribed at the surface of the head.
In accordance with the method for producing FRP screws of the second embodiment of the present invention, the fibers 2 remain uncut from one end to another of the screw 130. The fibers 2 near the peripheral thread of the screw 130 are held in the thread form in such a manner that the fibers 2 bent to follow the zigzag (wavy cross sectional figure) of the thread of the screw 130. The ram 90 exerts sufficient pressure on the material 6 (screw 130). Therefore, strong FRP screws with a similar strength thread portion can be produced. Furthermore, it is easy to manage the accuracy of the screw's dimensions. It is unnecessary to prepare a material which has a larger cross section portion to be a head and smaller cross section portion to be a thread portion.
Third Embodiment
The third embodiment of the present invention will be described hereinafter, referring to FIGS. 1 and 14 through 19. In the third embodiment, a screw without a head may be produced. The material of the screw is the same as shown in FIG. 1. The material 6 is cut off to a prescribed length, and then laid on and placed into a mold 140 as shown in FIGS. 14 and 15. The mold 140 consists of a rectangular solid-shaped thread mold member 142 for producing the lateral thread of the screw to be manufactured, and two plate-like end mold members 144 for producing the end portions of the screw, which are attached to both sides of the thread mold member 142. The thread mold member 144 consists of two separable half mold members 146 and 148 which are generally symmetrical with each other, for enabling the smooth removal of the manufactured screw. When the half mold members 146 and 148 are combined together, the thread mold member 144 has a guide groove 150. A semi-circular surface 152 exists at the bottom of the guide groove 150. The semi-circular surface 152 includes a center axis located in a plane in which the half mold members 146 and 148 contact each other. The semi-circular surface 152 has small grooves 154 for producing a thread of the screw. The width of the guide groove 150 is slightly larger than the major diameter of the semi-circular surface 152. The material 6 is placed on the semi-circular surface 152 in such a manner that the longitudinal axis of the material 6 aligns with the axis of the semi-circular surface 152 and is surrounded by the entire mold 140.
The material 6 is heated to soften. Then, a ram 160 is downwardly advanced inserted into the guide groove 150. The ram 160 has a presser 162 which is of a shape to engage with the guide groove 160 and of which forward end is plane. As shown in FIGS. 16 and 17, the material 6 is pressed by the presser 162, to be a half screw 164 which has an unnecessary burr 166. The screw 164 is generally in a form of a screw to be cut at a plane including a center axis thereof and the burr 166 laterally and perpendicularly projects from the plane. The unnecessary burr 166 is caused by the material 6 having excess volume for providing sufficient pressure. At the inner portion of the half screw 164, the continuous carbon fibers 2 align along the screw's axis. At the outer portion, the fibers 2 approximately align along the zigzag of the thread of the half screw 164 and remain uncut from one end to another end of the half screw 164.
The ram 160 is removed from the mold 140. The end mold members 144 are removed from the thread mold member 142. The half mold members 146 and 148 are separated from each other. Then, the half screw 164 is taken out. Because the half screw 164 has an unnecessary burr 166, the unnecessary portion 166 is cut off by machining, along a surface determined by line (A)--(A) and line (B)--(B) shown in FIG. 18. A complete half screw 168 shown in FIG. 19 is therefore shaped.
The half screw 168 is combined with another one in a manner so that the phase of the thread is aligned to produce a unitary screw without a head. The half screws 168 can be adhere together by a gluing agent, or can be thermally welded together. The unitary screw is finished by inscribed a slot at one end of the unitary screw.
In accordance with the method for producing FRP screws of the third embodiment of the present invention, the fibers 2 remain uncut from one end to another end of the produced screw. The fibers 2 near the peripheral thread of the screw ar held in the thread from in such a manner that the fibers 2 bent to follow the zigzag (wavy cross sectional figure) of the the thread of the screw. The ram 160 exerts sufficient pressure on the material 6 (screw). Therefore, strong FRP screws with a similar strength thread portion can be produced. Furthermore, it is easy to manage the accuracy of the screw's dimensions.
Fourth Embodiment
A fourth embodiment of the present invention will be described hereinafter with references to FIGS. 1 and 20 through 30. In the fourth embodiment, the material 6 shown in FIG. 1 is also utilized. The material 6 is cut off to a prescribed length, and then laid on and placed into a mold 180 as shown in FIGS. 20 and 21. A primary molding process begins. As shown in FIGS. 20, 21, and 24, the mold 180 comprises a rectangular solid-shaped lateral mold member 182 for producing the lateral face of a product to be manufactured by the primary molding process. The lateral mold member 182 consists of a pair of separable half molds which are generally symmetric, for enabling the smooth removal of the manufactured product. The lateral mold member 182 has a guide groove 190, the bottom of which is formed in a semi-circular cross section. At the bottom of the guide groove 190, three semi-circular surfaces 192, 194, and 196 which concentrically communicate each other are formed. In other words, from one end to another end of the guide groove 190, a small diameter surface 192, a middle diameter surface 194, and a taper surface 196 are aligned. The small diameter surface 192 whose length is the largest, shapes a portion to be a thread portion of a screw, as described later. The middle diameter surface 194 shapes a portion to be the neck of the screw. The taper surface 196 shapes a portion to be a head of the screw. The taper surface 196 tapers from the end of the lateral mold member 182 to the middle diameter surface 194. The lateral internal surfaces of the guide groove 190 curves in such a manner that the width of the guide groove 190 is slightly larger than the respective surfaces 192, 194, and 196. The material 6 is placed on the surfaces 192, 194, and 196 in such a manner that the longitudinal axis of the material 6 is generally aligned with the axis of the surfaces 192, 194, and 196, and surrounded by the entire mold 180.
The material 6 is heated to soften. Then, a ram 200 is downwardly advanced and inserted into the guide groove 190. The ram 200 has a presser 202, the cross section of which in plan view engages with the guide groove 190. A pressing surface of the presser 202 is generally a plane but has a semi-conical projection 204 which is adequate to fit into the taper surface 196. When the ram 200 is held in engagement with the mold 180, the projection 204 is surrounded by and parallel to but spaced apart from the surface 196.
As shown in FIGS. 22 and 23, the material 6 is pressed by the presser 202, to be a half shoulder round bar 210 which has an unnecessary burr 212. The unnecessary burr 212 is caused by the material 6 having excessive volume for providing sufficient pressure. The half shoulder round bar 210 is generally in a form of a shoulder round bar cut at a plane including a center axis thereof and the burr 212 laterally and perpendicularly projects from the plane. At the inner portion of the half shoulder round bar 210, the continuous carbon fibers 2 align along the bar's axis. At the outer portion, the fibers generally align along the zigzag of the shoulder and still remain uncut. The half round bar 210 has concentrically and orderly aligned a small diameter portion 214, a middle diameter portion 216, and a taper diameter portion 218 The small diameter portion 214 is to be a thread portion of a screw. The middle diameter portion 216 is to be the neck of the screw. The taper diameter portion 218 is to be a head of the screw. The taper diameter portion 218 tapers from an end of the half shoulder round bar 210 to the middle diameter portion 216. The taper diameter portion 218 has a recess 222 of a semi-circular cross section aligned with the axis of the half bar 212 formed by the projection 204.
The ram 200 is removed from the mold 180. The elements of the mold 180 are separated from each other for removal of the half shoulder round bar 210, as shown in FIG. 25. Then, the unnecessary burr 212 is cut off by machining. A complete half shoulder round bar 228 shown in FIG. 26 is therefore produced.
As shown in FIG. 27, the half shoulder round bar 228 is combined with another one, so that a unitary shoulder round bar 230 is formed. The shoulder round bar 230 has a head wall which is constituted by the taper portions 218 containing a hollow 232 of a conical shape which is constituted by the recesses 222. The two half shoulder round bars 228 can be adhered together by a gluing agent, or can be thermally welded together.
Next, a head core 240 of a conical shape shown in FIG. 28, which can fit into the hollow 232 is inserted an united with the hollow 232 by a gluing agent or thermal welding process. The conical core 240, which is for resistance to lateral transformation of the taper portion 218, is made of an FRP as well as the material 6. The fibers 2 are preferably aligned in a perpendicular direction to the axis of the conical shape of the head core 240.
While a method for producing an FRP screw is described above, the shoulder round bar 230 with the head core 240 can be utilized as a rivet. The rivet 230 has a head portion and shank portion. For use of the shoulder round bar 230 as a screw, the shoulder round bar 230 has to pass the following secondary molding process.
After uniting the head core 240 and the shoulder round bar 230, a secondary molding for forming a thread of a screw begins. In the secondary molding process, as shown in FIG. 29, the shoulder round bar 230 with the head core 240 are placed in a mold 250. The mold 250 consists of a lateral mold member 251 for forming a lateral face including a thread of a screw and two end mold members 254 and 256 for forming ends of the screw attached to both sides of the lateral mold member 251, respectively. The mold member 251 consists of a pair of half mold members 252 and 253 which are generally symmetric to each other to enabling the smooth removal of the screw to be manufactured. When the half mold members 252 and 253 are combined together, the lateral mold member 251 has a hole 258 of a circular cross section in such a manner that the axis of the hole 258 is located on a plane in which the half mold members 252 and 253 contact each other. The hole 258 includes a smooth small diameter portion 260 for engaging with the end mold member 254, an internally threaded portion 262, another smooth small diameter portion 264, a taper diameter portion 266, and a large diameter portion 270 for engaging with the end mold member 256, which concentrically communicate with each other. The thread portion 262 has threaded grooves to shape a thread portion of a screw to be formed. The small diameter portion 264 shapes a neck of the screw. The taper diameter portion 266 which tapers from the larger diameter portion 270 to the small diameter portion 264 shapes a head of the screw.
The end mold member 254 in the shape of a plate engages with the small diameter portion 260. The end mold member 256 of a shape of a cylindrical plug is held in engagement with the largest diameter portion 270. The end mold member 254 has a projection 272 of a circular cross section to be inserted into the small diameter portion 260, and which cooperates with the end mold member 256 to clamp the shoulder round bar 230 whose axis is generally aligned with the axis of the hole 258 . The end mold member 254 includes a through hole 274 axially and concentrically passing through the circular projection 272 as well as the plate portion of the end mold member 254.
After positioning of the shoulder round bar 230, it is heated to be soft. A cylindrical pressure stick 40 which is similar to the stick 40 described in the first embodiment is inserted into and through the through hole 274 as shown in FIG. 30. Moreover, the pressure stick 40 is advanced along the axis of the shoulder round bar to a location that is inward of the middle diameter portion 264 of the heated shoulder round bar 230. The stick 40 radially presses and expands the small diameter portion 214 of the shoulder round bar 230. The outer peripheral face of the small diameter portion 214 is brought into contact with the internally threaded portion 262, so that the small diameter portion 214 can have a thread on its peripheral face. Therefore, the shoulder round bar 230 becomes a screw 280 which comprises a head 282, neck 284, and thread portion 286. The stick 40 remains embedded in the screw 280 so as to be a core of the screw 280. The end of the stick 40 is preferably sharpened like a pencil for smooth insertion.
The elongated fibers 2 remains uncut, in the screw 280. The fiber 2 near the peripheral thread of the screw 280 are held in the thread in such a manner that the fibers 2 bent to follow the zigzag (bending in the cross-sectional figure) of the thread of the screw 280. Furthermore, the head core 240 and the shoulder round bar 230 are tightly united.
The screw 280 is cooled to be hard. The half mold members 252 and 253 are separated from each other, for removing the screw. The stick 40 is cut along the end surface of the screw 280. At the end surface of the head, a slit to be engaged with a screwdriver may be inscribed by machining. Therefore, the manufactured screw 280 is completed. The stick 40 is preferably made of a high compressive strength material, such as a steel or FRP similar to the main portion of the screw 280. For providing high pressure to the screw 280, steel is more preferable for the sick 40. In order to make light screws, FRP is more preferable as the stick 40. More preferably, when the stick is inserted into the shoulder round bar 230, the stick is made of steel; and this steel stick can then be replaced by an FRP stick as the core. The dimensions of the stick 40 are selected to be suitable for the dimensions of the screws 280, so as to press to sufficiently expand the shoulder round bar into the internal thread of the lateral mold member 251.
In accordance with the method for producing FRP screws of the embodiment of present invention, the fibers 2 remains uncut, in the screw 280. The fibers 2 near the peripheral thread of the screw 280 are held in the thread in such a manner that the fibers 2 bend to follow the bending cross-sectional pattern of the screw 280. Therefore, sufficiently strong FRP screws whose thread portion also has a similar strength can be produced. Also, because in the outer portion of the head 282, the elongated fibers are arranged in the direction of the conical shape of the head 282, strength against shearing of the head 282 is highly improved.
Furthermore, since the half shoulder round bar 210 is made by pressing in the primary molding process with sufficient pressure, the bar 210 has good mechanical strength. For example, even if the material 6 includes cavities, the primary molding process provides a bar 210 without cavities due to application of sufficient pressure.
Provided the material 6 has enough volume to fill the surfaces 192, 194, and 196 of the mold 180, to form a half shoulder round bar 210, the material 6 dimensions do not need to have high accuracy. Furthermore, it is unnecessary to prepare a material which has a larger cross section portion to be a head and smaller cross section portion to be a thread portion.
If the stick 40 has a mechanical strength which is in excess of that of the FRP, the manufactured screw 280 embedded with the stick 40 along its axis has a higher tensional strength along its axis than that of conventional screws made only of FRP.
A method of modification of the fourth embodiment is described hereinafter with reference to FIGS. 31 and 32. When the half shoulder round bar 210 is manufactured in the primary molding process, a semi-ring-shaped projection projecting concentric from the taper diameter portion 218 is formed simultaneously. Consequently the shoulder round bar 230 united by a pair of the half shoulder round bar 210 includes a ring-shaped projection 290 which is constituted by the semi-ring-shaped projections.
Then, the shoulder round bar 230 with the head core 240 is subjected to the secondary molding process. The mold 250 is generally similar to that shown in FIGS. 29 and 30. However, the end mold member 256 has a projection 292 of a circular cross section to be held in inserted engagement with the outer peripheral face of the ring-shaped projection 290. Also, the lateral mold member 251 includes a hollow 294 communicating directly to the taper diameter portion 266 to be held in engagement with the ring-shaped projection 290. After the secondary molding process, the ring-shaped projection 290 is cut off along the end faces of the taper diameter portion 218 and the head core 240. The ring-shaped projection 290 may be cut off directly after uniting the shoulder round bar 230 and the head core 240.
With the above method of the modification of the fourth embodiment, a disorderment of the arrangement of the fibers 2 which may be generated at an end portion during pressing molding (in this case, the ring-shaped projection) can be rejected. Therefore, the arrangement of the fibers 2 inward of the head 282 is improved.
Another modification of the fourth embodiment is described as follows referring to FIG. 33. This modification improves the secondary molding process. The embedding and uniting of the conical head core 240 into the hollow 232 can be omitted. As shown in FIG. 33, a mold 300 for the secondary molding process comprises a lateral mold member 302 for forming a lateral thread of a screw and an end mold member 304 in a form of a plate attached to one side of the lateral mold member 302 for forming an end face of the screw. The lateral mold member 302 comprises a hole 306 of a circular cross section which includes an internally threaded portion 308, smooth hole portion 310, a taper portion 312, and a large diameter portion 314. The details of the portions 308, 310, 312, and 314 are respectively the same as the internally threaded portion 262, middle diameter portion 264, taper diameter portion 266, and the large diameter portion 270 indicated in FIG. 29.
Returning to FIG. 33, after placing of the shoulder round bar 230 in such a manner that the axis of the bar 230 is aligned with the axis of the hole 306, the shoulder round bar 230 is heated to soften. Then, a stick 316 in a form of a nail which has a bar portion 318 of a circular cross section and a conical head 320 attached concentrically and tapering to the bar portion 318 is advanced by a ram 322 of a circular cross section to be engaged with the large diameter portion 314. The stick 316 is advanced along the axis of the shoulder round bar 230 and inserted therein until the head 320 is held in inserted engagement with the hollow 232 of the shoulder round bar 230. At the outer peripheral face of the shoulder round bar 230, a thread is formed. The stick 316 is kept in embedded condition in the shoulder round bar 230. After cooling, a screw 330 which has a head 332, neck 334, and thread portion 336 and contains a head core 320 (the head of the stick 316) and an axial core 318 (the bar portion of the stick 316) is obtained. In the method, nevertheless to say, the stick 316 is preferably made of FRP as well as the main portion of the screw 330.
In the fourth embodiment, as shown in FIGS. 29 and 30, the stick 40 is of a simple circular cross section. However, in order to improve physical contact between the remained stick 40 and the produced screw 280, the stick 40 preferably is of a shape shown in FIGS. 34 or 35. The stick 40 shown in FIG. 34 has a plurality of projections on the outer peripheral surface thereof. The projections are spaced apart from each other along the axis of the stick 40. The stick 40 shown in FIG. 35 has thread formed on the outer peripheral surface thereof. Accordingly, slipping between the remained stick 40 and the screw 280 are prevented for producing the screw having high tensile strength.
While the matrix 4 of the material 6 is a thermoplastic resin such as polyether-etherketone in the above various preferred embodiments of the present invention, the matrix 4 is not limited to being thermoplastic resins as long as the matrix can be softened during molding processes. Various thermo-setting resins can be utilized as the matrix 4. For Example, various epoxy resins are preferable because of the properties such as mechanical strength thereof. In the preliminary stages before molding a final product, with a material such as a prepreg to be united, this can be heated to a temperature such that epoxy resin is in a semi-polymerized condition known as B-stage. Then, when molding the final product, the material can be heated again to a temperature at which the material becomes completely polymerized and hardened.
While in the various embodiment, the material 6 is in a circular cross section form, it is not limited to this cross section and various other cross sectional shape of the material can be utilized.
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A method for producing fiber-reinforced plastic screw-like fastening element including a thread portion and a head having a cross section which is larger than that of the thread portion. The method includes preparing a rod material including an elongated matrix formed of a plastic material and a plurality of elongated parallel fiber elements embedded within the matrix material along the length of the matrix, with the fiber elements having melting points substantially higher than the softening point of the matrix. Thereafter the prepared rod material of the screw is placed into a mold chamber having an internal surface of a semi-circular cross section with the internal surface having a small diameter portion and a large cross section portion communicating concentrically to the small diameter portion. The rod material is then heated to a temperature equal to or greater than the softening point of the matrix material. The heated material is then pressed to form a half round bar from the material, and cooled to a temperature lower than the softening point of the matrix material; and finally, the cooled rod material is removed from the mold chamber.
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TECHNICAL FIELD
The present invention relates to control systems for internal combustion engines, and more particularly to control systems for compensating throttle area of a throttle body.
BACKGROUND OF THE INVENTION
Electronic throttle control (ETC) systems replace the mechanical pedal assemblies that are currently used in vehicles. ETC systems enhance overall engine management while reducing the cost of the vehicle. Traditional engine controls rely on direct input from drivers and numerous valves and linkages to manage the engine. These systems do not allow consistent throttle control.
ETC sensors eliminate the linkage that is used to connect the accelerator pedal to the throttle body. ETC sensors take input from the driver's foot and send it to an engine control system in real time. The engine control system modulates the air/fuel flow to the engine. Direct control of the engine is shifted from the driver to the engine control system to improve efficiency.
ETC also can be coordinated with the shifting of the transmission, whereas mechanical systems react solely to the torque applied by the engine. Mechanical systems shift under high-load conditions, which may decrease the life of the transmission over time. ETC systems can reduce throttle, shift, and then increase throttle. This approach will increase the life of the transmission.
As throttle body coke deposits build up on a throttle blade/bore during the life of a vehicle, a relationship between pedal position and throttle response may deteriorate. This deterioration can lead to reduced idle quality. Customers experiencing poor idle quality during a warranty coverage period will request service. As a result, the warranty cost of the vehicle increases. Customers experiencing poor idle quality after the warranty coverage period ends will have higher operating costs. Other conditions that may adversely impact throttle response include variations in an airflow breakout region position, dirty air cleaners, and/or non-linearity in throttle position sensors.
SUMMARY OF THE INVENTION
A method and apparatus according to the present invention compensates throttle area in an engine control system with an electronic throttle using intake diagnostic residuals. A plurality of tables relate throttle area, breakpoint numbers, flow loss factors and residual values. At least one of the tables is updated based on the intake diagnostic residuals to generate a compensated throttle area.
In other features of the invention, a first table relates throttle area to breakpoint numbers and residual values. A second table relates residual values to flow loss factors. A third table relates flow loss factors to breakpoint numbers. A fourth table relates throttle area to breakpoint numbers.
In another feature of the invention, a desired throttle area is obtained from a pedal position sensor and/or a cruise control. A current throttle area is used to lookup a first breakpoint number in the first table. The first breakpoint is rounded. An absolute value of a difference between the rounded first breakpoint number and the first breakpoint number is compared to a hysteresis calibration value. The third or fourth tables are updated only when the absolute value is less than the hysteresis calibration value.
In other features of the invention, a current residual value is obtained from an intake diagnostic. Based on the current residual value, a flow loss factor is obtained from the second table. Using the rounded first breakpoint number, a flow loss factor is obtained from the third table. A filtered flow loss factor is calculated from the flow loss factors of the second and third tables. The filtered flow loss factor is stored in the third table in a position corresponding to the rounded first breakpoint number.
In still other features, a clean throttle area is obtained from the first table using the rounded first breakpoint number. The filtered flow loss factor is multiplied by the clean throttle area to provide a product. The fourth table is updated with the product in a position corresponding to the rounded first breakpoint number.
In still other features, a compensated breakpoint number is obtained from the fourth table based on the desired throttle area. A compensated throttle area is obtained from the first table using the compensated breakpoint number.
Further areas of applicability of the present invention will become apparent from the detailed description provided hereinafter. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will become more fully understood from the detailed description and the accompanying drawings, wherein:
FIG. 1 is a functional block diagram of a throttle area compensation system according to the present invention that employs estimated and actual airflow;
FIG. 2 is a functional block diagram of a throttle area compensation system according to the present invention that employs estimated and actual manifold absolute pressure (MAP);
FIG. 3 is a functional block diagram of a throttle area compensation system according to the present invention that employs estimated and actual airflow and estimated and actual MAP;
FIG. 4 is a first lookup table relating throttle area to breakpoint numbers and residual values;
FIG. 5 is a second lookup table relating flow loss factors to residual values;
FIG. 6 is a third lookup table relating flow loss factors to breakpoint numbers;
FIG. 7 is a fourth lookup table relating throttle area to breakpoint numbers; and
FIG. 8 is a flowchart illustrating steps performed by the throttle area compensation system.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The following description of the preferred embodiment(s) is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses.
Part of the responsibility of an engine control diagnostic system includes the compensation of airflow due to VE, exhaust gas recirculation (EGR), intake air temperature (IAT), variable valve timing, variable displacement, and other engine system inputs. Suitable engine control diagnostic systems with compensation include “Fault Identification Diagnostic for Intake System Sensors”, Ser. No. 09/961,537, filed Sep. 20, 2001, which is assigned to the assignee of the present invention and is hereby incorporated by reference. The engine control diagnostic system disclosed therein includes an intake diagnostic that generates residual values that represent differences between actual and estimated airflow and actual and estimated manifold absolute pressure (MAP).
The present invention uses the residuals that are generated by the intake diagnostic systems to compensate the throttle body for actual airflow progression throughout an operating range of a throttle blade opening. As used herein, residuals refer to a ratio between (sensed-estimated)/estimated. Generally, the present invention employs the throttle body airflow relationship (or progression) for an ideal throttle body and creates a learned table representing the actual airflow progression using the residual values from the intake diagnostic system. The present invention employs inverted functions such as table lookups with interpolation as will be described more fully below.
Referring now to FIG. 1, a throttle body compensation system is shown and includes a residual generator 12 that generates actual and estimated mass airflow (MAF) signals. A compensation calculator 14 is connected to the intake diagnostic 12 , a pedal position sensor 18 , and a cruise control 20 . A compensated throttle area is output by the compensation calculator 14 to an electronic throttle control 22 . Alternately, the compensation calculator 14 and the electronic throttle control 22 are combined into a single functional block. The electronic throttle control 22 controls a throttle area of a throttle body 24 .
In use, the pedal position sensor 18 and/or cruise control 20 generate a desired throttle area (ta_desired). The compensation calculator 14 , the electronic throttle control 22 and/or another device arbitrates between the signals that are generated by the pedal position sensor 18 and the cruise control 20 . Due to throttle body coke deposits that build up on a throttle blade/bore during the life of a vehicle, a relationship between pedal position and throttle response may deteriorate. Other conditions that may adversely impact throttle response include variations in an airflow breakout region position, dirty air cleaners, and/or non-linearity in throttle position sensors. Therefore, the actual throttle area may need to be more or less than the desired throttle area to achieve the desired acceleration or pedal response. The compensation calculator 14 and/or the electronic throttle control 22 calculate a compensated throttle area based on the desired throttle area and the residuals as will be described further below.
Referring now to FIG. 2, a throttle body compensation system 10 ′ can also use MAP residuals. For purposes of clarity, reference numbers from FIG. 1 are used in FIG. 2 where appropriate to identify similar elements. The intake diagnostic 12 ′ generates actual and estimated MAP signals.
Referring now to FIG. 3, a throttle body compensation system 10 ″ can also use both airflow and MAP residuals. For purposes of clarity, reference numbers from FIG. 1 are used in FIG. 2 where appropriate to identify similar elements. The residual generator 12 ″ generates both actual and estimated MAP and airflow signals. These residual values can be used individually, averaged or otherwise weighted. Alternately, other schemes may be employed.
Referring now to FIG. 4, a first lookup table relates throttle area to breakpoint numbers and residual values. Residuals start at or near zero for a new throttle body. The third column in FIG. 4 represents residuals that are typically encountered in an aged throttle body with coke deposits and/or nonlinearity. The third column is not part of the stored table. The first and second columns are preprogrammed.
Referring now to FIG. 5, a second lookup table relates flow loss factors to residual values. The table in FIG. 5 represents a relationship between residual and flow loss factors that are allowed for the amount of coking. The purpose of the values in FIG. 5 is to place limits on the authority of the throttle body compensation system.
Preferably, the tables in FIGS. 4 and 5 are programmed by the manufacturer and are not updated during operation.
Referring now to FIG. 6, a third lookup table relates flow loss factors to breakpoint numbers. The table in FIG. 6 is updated during operation of the vehicle based on the residual values. Referring now to FIG. 7, a fourth lookup table relates throttle area to breakpoint numbers. The table in FIG. 7 is also updated during operation of the vehicle based on residual values. As can be appreciated, the values listed in FIGS. 4-7 are exemplary values. Other values can be used.
Referring now to FIG. 8, steps for compensating the throttle body are shown generally at 100 . In the following description, F 1 AXIS refers to the first table in FIG. 4 . F 3 refers to the second table in FIG. 5 . F 1 refers to the third table in FIG. 6 . F 2 refers to the fourth table in FIG. 7 .
Control begins with step 101 . In step 102 , a throttle area is obtained from the accelerator pedal 18 or cruise control 20 before modification and conversion to desired throttle area (ta_desired). In step 104 , residuals from an intake diagnostic (that generates differences between actual and estimated airflow and/or MAP) are monitored at several current throttle area points. In step 106 , the throttle break points are used to set up calibration axis (F 1 AXIS—FIG. 4) to allow more breakpoints around a breakout region. In step 108 , control determines whether Breakpoint_number=round(lookup(F 1 AXIS, ta_current)). In step 112 , control determines whether the engine is running. If not control ends at step 114 . Otherwise control continues with step 116 wherein a hysteresis calculation is performed as follows: Abs(Lookup(F 1 AXIS, ta_current)−Breakpoint_Number))<Hysteresis_Cal. The Hysterisis_Cal is a hysteresis calibration value such as 0.3 that determines how close the breakpoint number must be to update the tables. A maximum value of 0.5 can be used.
In step 120 , the Flow_Loss_Factor is set equal to Lookup(F 3 , residual). In step 122 , F 1 @ (Breakpoint_number) is set equal to F 1 @ (Breakpoint_number)+Filter_Cal*(Flow_Loss 13 Factor−F 1 @ (Breakpoint_number))−which is a filter calculation. The Filter_Cal is a filter calibration value such as 0.1 that provides a weighting to the new air flow progression calculation. The filter calibration value can be a constant or a function of sign and/or magnitude of the residuals to handle rapid learning if a new/clean throttle body is detected. The filter coefficient can be reduced further by multiplying it by a 5 th table that is a function of the hysteresis calculation in step 116 to give higher weighting to values closer to the breakpoints.
In step 126 , F 2 @ (Breakpoint_number) is set equal to F 1 @ (Breakpoint_number)*Lookup(F 1 AXIS,(Breakpoint_number)). In step 130 , Ta_current is set equal to (F 1 AXIS, Lookup(F 2 ,ta_desired). In step 134 , ta_current is converted to position and sent to the throttle body. Control ends at step 136 . The compensations are performed periodically, for example every 12.5 ms.
EXAMPLE
The following example will employ the exemplary values that are found in the tables of FIGS. 4-7. The pedal position sensor 18 and/or the cruise control 20 transmits a desired throttle area of 30. Therefore, ta_desired is set equal to 30. In this example, ta_current is equal to 28.47758 from the previous loop.
If the engine is running, a hysteresis calculation is performed. The value ta_current is used to determine a non-rounded breakpoint number, which is equal to 4.847758. The value is calculated as follows: 4+(5-4)* (30−18.44256)/(32.08355−18.44256)=4.847758. As can be appreciated, the non-rounded breakpoint number is interplated between table values. The rounded breakpoint number is equal to 5. The absolute value of the non-rounded breakpoint number (4.847758) is subtracted from the rounded breakpoint number (5). In this case, the absolute value is less than a Hysteresis_Cal (0.3). Therefore, the tables are updated. As can be appreciated, other values can be used for the hystersis calibration value to adjust the sensitivity of the update function.
A residual value is obtained from the intake diagnostic 12 . In this case, the residual is equal to 0.069452. The Flow_Loss_Factor is obtained from the second table in FIG. 5 using the residual value from the intake diagnostic 12 . In this case, the flow loss factor is 1.05+(1.1−1.05)*(0.069452−0.05)/(0.1−0.05)=1.069452.
A filtered flow loss factor is calculated. The current value of the flow loss factor is obtained from the third table F 1 in FIG. 6 based on the rounded breakpoint number (5). In this case, the current flow loss factor is equal to 1.069452. The filtered flow loss factor is equal to (1.069452)+(0.1)(1.069452−1.069452)=1.069452, which is no change in the flow loss factor in this example. The filtered flow loss factor is saved in the third table a position corresponding to the rounded breakpoint number (5).
Then, clean throttle body area is multipled by the flow loss factor and stored for the breakpoint. First, the rounded breakpoint number (5) is used to lookup the clean throttle body area (30). The filtered flow loss factor for the rounded breakpoint number (5) is 1.069452. The fourth table in FIG. 7 is updated with the new value 30*1.069452=32.08356 for the rounded breakpoint 5 .
Using an independent lookup, the compensated throttle area ta_current is determined based on the new fourth table. Using ta_desired=30, the breakpoint value is determined and is equal to 4+(5−4)*(30−18.44256)/(32.08356−18.44256)=4.8472575. Then this value is used to lookup ta_current in the first table, which is equal to 28.472575. This value of ta_current is the compensated throttle area. Since this example decreases throttle, the compensation in this region is for sensor nonlinearity or variation in the break-out region. An increase in the compensation throttle area typically represents compensation due to coking.
Those skilled in the art can now appreciate from the foregoing description that the broad teachings of the present invention can be implemented in a variety of forms. Therefore, while this invention has been described in connection with particular examples thereof, the true scope of the invention should not be so limited since other modifications will become apparent to the skilled practitioner upon a study of the drawings, the specification and the following claims.
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A method and apparatus compensates throttle area in an engine control system with an electronic throttle using intake diagnostic residuals. A plurality of tables relate throttle area, breakpoint numbers, flow loss factors and residual values. At least one of the tables is updated based on the intake diagnostic residuals to generate a compensated throttle area.
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[0001] This patent document claims the benefit of German Patent Application No. DE 10 2007 056 432.7 filed on Nov. 23, 2007, which is hereby incorporated by reference.
BACKGROUND
[0002] The present embodiments relate to controlling a display of medical images on a large-format display unit.
[0003] Medical examinations in a hospital may include using a number of displays and/or images to capture the examined part of the body. A number of different perspectives can be displayed, for example, using a medical imaging method. Different imaging methods and/or modalities (e.g. x-ray, computed tomography, ultrasound, magnetic resonance tomography, video, laser beam scatter, etc.) are combined to obtain as much information as possible about the patient's health problems. A number of displayed images are used, when images recorded under different conditions (e.g. before and after the assimilation of contrast agents) are superimposed, to obtain a display with the greatest possible contrast (differential methods).
[0004] Different medical images are generally displayed respectively on individual, dedicated image reproduction devices. A separate image reproduction device is required for each video (graphics card) output of a medical imaging system. As a result eight or even more image reproduction devices are required in the examination room with modern x-ray system examination stations, including, for example, color displays for ECG and ultrasound.
[0005] A solution with a number of display units is unclear, inflexible and not easily scalable. “New Display Solutions for the Image-Centric Era of Healthcare” by S. Bonfiglio and L. Albani in SID Symposium Digest of Technical Papers—May 2007—Volume 38, Issue 1, pp. 123-126, discloses that a number of medical images may be displayed on a large-format display unit, so that it is possible to manage the medical images with one display unit per examination station. This publication describes an input device, which can be used to select images to be displayed on a large-format display unit from a plurality of possible medical images. The input device (e.g., a tablet PC) has a display, which has a first region with selectable images and a second region showing the images displayed on the large-format display unit. An image is selected by pushing the image from the first into the second region, whereupon it is displayed on the large-format display unit.
SUMMARY AND DESCRIPTION
[0006] The present embodiments may obviate one or more of the drawbacks or limitations inherent in the related art. For example, in one embodiment, medical image combinations may be optimally displayed on a large-format display unit.
[0007] In one embodiment, a number of programs are provided to control the display on a large-format display unit. The programs are assigned respectively to a medical workflow and serve to control the display on a large-format display unit to support the medical workflow.
[0008] A program may be a sequence of instructions, which are suitable for execution on a computer, for example, a computer program. The term “program” is however not intended to make a statement about the possible structure of suitable software. Sub-routines or sub-programs may correspond to the programs in respect of the structure of the software, these being called up by a different program part.
[0009] A medical workflow may be a sequence (e.g. work sequence or process sequence) during the treatment or examination of patients in a hospital. The workflow can also be defined implicitly, for example, in that organs or parts of the body to be examined or treated can be selected by the physician and a corresponding program is started, with the examination and/or treatment of the organ and/or part of the body corresponding to a defined workflow.
[0010] The display may be controlled according to requirements for the display of images arising during the workflow (and/or the corresponding examination or treatment). The requirements relate, for example, to the perspective, the type, the number, the arrangement or the processing of the images displayed. The display may be dynamically modified according to the workflow, for example, by updating images (for example, during the display of a stream of images) or displayed information or by adjusting the image combination shown on the large-format display unit, for example perspective, type, number, arrangement and processing of the images displayed. An update can also be triggered, for example, by the start of a new segment or act of a treatment or examination being carried out. A manual trigger (e.g., input at an input device) or an automatic trigger (e.g., automatic identification mechanism for the start of a new segment) can be provided for the input.
[0011] The large-format display unit or large-format screen may be an image reproduction device, a display unit, a monitor, or a display, which with respect of its technical characteristics (e.g., resolution, luminosity and dimensions) allows the simultaneous display of at least two images or image streams of adequate size and quality for diagnostic or therapeutic applications in hospital. In one example, a monitor having a resolution of 4 M pixels to over 8 M pixels and a screen size from 30″ to 64″ may be suitable for use as a large-format display unit in a hospital.
[0012] Selecting a workflow starts the associated program. This determines and/or sets for example an optimized image configuration for the workflow for display on the large-format display unit. An image configuration may include the selection and arrangement of elements (e.g., images and information) for display on the large-format display unit. An image configuration may include a number of images.
[0013] Workflow-related or process-oriented information may be displayed on the large-format display unit, for example, treatment acts to be carried out or status information (e.g. status information relating to devices or error messages). The treating physician may input additional information for display on the large-format display unit or to modify, adjust or delete displayed information using an input unit.
[0014] In one embodiment, a program is configured to adjust the display on the large-format display unit according to an input of an input unit (e.g., operating console). The input unit may correspond to the device on which the programs are stored and run. With regard to the input, different acts of the workflow (e.g. treatment steps or examination steps) may be identified on the large-format display unit and for the treating physician to adjust the display on the large-format display unit after the end of an act by inputting information identifying the next act to be implemented or by depressing a key or key combination. The program may control the display on the large-format display unit to adjust the workflow act to be carried out. Accordingly, this may be semi-automatic control of the display according to the workflow. It is also possible for the physician to input information about his/her position (e.g. the side of the patient table from which he/she is working) so that the program can adjust the display.
[0015] In one embodiment, fully-automatic control of at least some of the workflow-related display adjustments is provided. Position information relating to a medical device or the treating physician is automatically captured, the position information is transferred to the program, and the program adjusts the display according to the position information. For example, acts of the workflow correspond to different positions of a medical device. In one example, anesthesia and then a surgical intervention are carried out as two separate acts during a treatment. Movement of the surgical device from the rest position may be the trigger for adjustment of the display for the second act, the surgical intervention. This example is only intended for the purposes of illustration. Generally the processes are more complex, which can also result in more complex trigger mechanisms. For example, it can be expedient to make the adjustment dependent on a number of position information items, to ensure, for example, (by verifying additional position information) that the preceding act has been completed (e.g. medical device A is in the rest position and medical device B is in a deployment position). Another embodiment relates to the automatic capturing (e.g. by sensors or a video camera) of position information relating to the treating physician (e.g. the direction from which the physician treats the patient). The position information is then transferred to the program and triggers an adjustment of the display.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 shows a first image configuration;
[0017] FIG. 2 shows a second image configuration;
[0018] FIG. 3 shows one embodiment of a display on a large-format display unit; and
[0019] FIG. 4 shows one embodiment of a medical display system;
DETAILED DESCRIPTION
[0020] By calling up a program corresponding to a workflow, an image configuration may be initially predetermined, which has been put together for optimal support for the workflow. Examples of such image configurations are shown in FIG. 1 and FIG. 2 .
[0021] FIG. 1 shows an image configuration, in which six images are displayed on the large-format display unit. The images identified as Life Sub A, Life Sub B, Life Nat Ref A, Live Nat Ref B, Ref 2 A, and Ref 2 B. Life Sub A and Life Sub B are subtraction images. Life Nat Ref A and Live Nat Ref B are unprocessed recordings. Ref 2 A and Ref 2 B are reference images.
[0022] Such an image composition is used, for example, during an angiography examination. In angiography, vessels are examined using x-ray recordings. A radioactive contrast agent is introduced into the vessels and an x-ray recording is taken. A contrast is obtained by using an x-ray recording before the application of the contrast agent to remove the background of the recording, so that only the vessels can still be seen (e.g., a differential image). A recording before administration of the contrast agent (e.g., Ref 2 A and Ref 2 B) is superimposed with the recording after administration of the contrast agent (e.g., Life Nat Ref A and Live Nat Ref B) to remove the background, in order to generate a differential recording (e.g., Life Sub A and Life Sub B), in which essentially only the vessels are still shown.
[0023] In addition to the image configuration, a strip may be provided at the lower edge of the large-format display unit in which ECG data and system control information are shown. The image configuration shown in FIG. 2 differs in that the two images on the right side in FIG. 1 have been moved into the center and system-related information (e.g., Syngo Workplace) and ECG data is shown or displayed in the place of the two images on the right side in FIG. 1 . The image configurations in FIG. 1 and FIG. 2 can also be used as an alternative for the same workflow. The physician is then able to choose between two (or more) options for a configuration suitable for the workflow.
[0024] FIG. 3 shows the display of an image configuration on a large-format display unit. On the left of FIG. 3 are four images showing vessels recording using angiography. On the right of FIG. 3 is information relating to the workflow, for example, ECG curves.
[0025] FIG. 4 shows a system for displaying image configurations on a large-format display unit. An operating console 1 , which is connected by a software control interface 2 to a medical system 3 and a graphics controller 4 , can be used to select image configurations to be displayed on a large-format display unit 5 . The operating console 1 may be used to operate and/or control the medical system 3 . The medical system 3 is, for example, an angiography unit, which is used to produce angiography images, for example. The images are transferred to the graphics controller 4 . A number of inputs are provided in order to be able to transmit a number of images (e.g. reference images and differential images) to be displayed from the angiography unit separately to the graphics controller 4 .
[0026] The input device, for example, the operating console 1 , is used to select a workflow. It is possible to select organs or parts of the body, for example, by way of the input device, causing an associated program (e.g. organ program) to be started. A workflow corresponds to the program and/or the examination or treatment of the organ or part of the body. The display on the large-format display unit 5 may be controlled by the program to support the workflow. An image configuration appropriate for the workflow is determined for display on the large-format display 5 . The image configuration is transferred to the graphics controller 4 . The graphics controller 4 includes inputs to external video sources, for example, ECG, endoscopy, or ultrasound. The external video sources may be referenced by the image configuration. The external video sources may be selected for display on the large-format display unit 5 . The graphics controller 4 represents an adjustment device, which composes (generates) an image according to the selected image configuration and in some instances other control information, and transmits a corresponding image signal to the large-format display unit 5 .
[0027] Additional control information may be specified by a user input at the operating console 1 . Another possibility is the automatic generation of control information for the composition of the image by the graphics controller 4 by the program, which is also responsible for adjusting the image configuration displayed on the large-format display unit according to the workflow and/or the treatment or examination process.
[0028] While the invention has been described above by reference to various embodiments, it should be understood that many changes and modifications can be made without departing from the scope of the invention. For example, although the embodiments were discussed in conjunction with a particle therapy system, the same problems and solutions arise in photon therapy as well. It is therefore intended that the foregoing detailed description be regarded as illustrative rather than limiting, and that it be understood that it is the following claims, including all equivalents, that are intended to define the spirit and scope of this invention.
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A device for controlling the display of medical images on a large-format display unit is provided. The device includes a number of programs, which are assigned respectively to a medical workflow. The programs are configured for control of the display on the large-format display unit according to the associated workflow and can be called up by selecting the workflow. Accordingly, the display on a large-format display unit may be controlled according to medical workflows.
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This application claims priority benefits from French Patent Application No. FR 07 07959 filed Nov. 13, 2007, the disclosure of which is hereby incorporated by reference.
The invention relates to the field of automated solar protection, in particularly awnings driven by an actuator.
BACKGROUND OF THE INVENTION
A fabric forming the awning is designed to be wound onto a tube called the roller tube, the rotation of the latter being produced either by means of an electromechanical actuator or thanks to a manual operation device or a handle.
Tubular actuators are very commonly used for these automatic operations. They are located inside the roller tube and enable the fabric of the awning to be unwound or wound without particular effort. In addition, associated with automation or sensors, the operation of the awning may be remotely carried out, without the need for user intervention (for example, automatic unwinding in the presence of sun to protect both the terrace or the windows from too much heating in summer, automatic winding in the event of wind to protect the awning itself).
Electromechanical actuators are generally connected to the mains for their power supply. To provide for the event of urgent use in case of a power cut, some versions are proposed with an emergency control. The actuator then combines the automatic and manual functions.
For the operation of the actuator it is preferable that the latter knows the extension position of the awning, especially in order to manage the particular operations over different zones of the travel: arrival at the upper stop, arrival at the low point, locking zone of the extension arm of the awning.
DESCRIPTION OF THE PRIOR ART
Various solutions exist in the prior art for determining the position by counting, these dividing mainly into electronic or mechanical counting devices.
Mechanical counting devices are commonly used. A movement of the screen in one direction or the other is mechanically recorded by the counting device. Adjusting the limit of travel generally requires access to the actuator. Then, whatever the origin of movement (motorized or manual), the counting is active and positions are always properly located.
Electronic counting devices also have become available on the market. The current position is located in a non-volatile electronic memory, which enables the information to be preserved even in the event of a power outage. Adjustment of such an electronic counting device may be carried out at a distance, which obviously has many advantages, as the actuators are not easily accessible once fitted on site.
However, if such actuators with an electronic counting device are equipped with a manual emergency control, a manual movement carried out during a power outage may disturb the position counting: the awning is indeed moved without the electronic counting system changing the value of the current position. It is also unlikely that the awning will return to its initial position after this manual operation. The position in memory therefore no longer corresponds to the current position, in other words the installation is not properly adjusted.
This situation can be avoided by using absolute position sensors, but these are made of complex technology and rarely, or even never, used in the field of automated solar protection.
A simple practice consists of detecting each interruption of current and resetting the system to a hard stop (if there is one) each time. This has many disadvantages. Each micro-power outage may lead to a resetting. The latter is not well understood by the user, who notices that his or her installation is behaving curiously each time the mains power returns or not corresponding to the simple instruction given to raise or lower the solar protection.
Another solution, described in the patent application IT MI2002001549, consists in adding a second detection system that will enable counting to be carried out or more simply detecting a movement during an emergency manual operation. The second detection system is supplied with power by an energy storage means (supercapacitor type) that is recharged when a voltage is applied to the actuator. The installation will then be able to reset only in cases in which a manual operation has taken place. However, this solution requires the employment of new counting means apart from the existing means or adapted counting means, which further increases the price of devices with emergency operation.
Whatever solution is used, it is necessary to reset the installation when needed and/or automatically. This resetting is based on the recognition of a fixed position, such as a hard stop or a position in which it is no longer possible to continue moving and similar to a hard stop. The position of this stop can be determined by analyzing the torque or a variation in torque exerted by the motor or a lack of speed. These parameters are then independent of the counting position. The position of the stop is associated with a reference position value. The counting can then be updated from this reference position which represents the current position of the awning unambiguously.
The recognition of such a stop is known to the person skilled in the art. Patent EP 1 269 596 describes a device for stopping the motor when the load on the motor exceeds a predetermined value. It comprises means for converting the variation in voltage at the terminals of the phase-shifting capacitor, corresponding to a variation in the predetermined torque, into a chosen variation in the voltage whatever the maximum torque developed, means for comparing the converted voltage with a reference voltage and means for stopping the motor when the converted voltage is less than the reference voltage.
An automatic resetting procedure is known from document US 2005/0237015 in the field of motorized garage doors. In this type of installation, a manual operation is also foreseen which can be used when the actuator is without power. This document describes a system of locatable passpoints which define the limits of the operational zones. When reconnected to the power-supply network following a detected manual operation, the electronics of the installation determines which zone the door is positioned in on the basis of information specific to each zone, for example a voltage value specific to each zone. A preferred direction of movement is defined for each zone so as to be sure of reaching a passpoint where the position counter is reset.
The use of this system for a garage door requires the fitting of passpoint sensors or zone indicators distinguishing the operational zones, which increases the cost of the system.
Furthermore, this document proposes only the definition of a preferred direction of movement as the action to be implemented as a function of the zone in which the door is positioned.
In the case of the awning, a single stop and not a set of passpoints is enough to enable resetting. However, in order to locate this stop, it is necessary to activate the stop detection means, as mentioned above. It is also necessary to avoid activating these means in other zones of the travel, in particular in a zone called the arm-locking zone, where an increase in torque, variation in torque or lack of speed may express an event different from an arrival at a hard stop. The patent EP 0 770 757 thus describes activation of the stop detection means, called the load surveillance means, only during the return of the awning, just before reaching the initial position corresponding to the stop and not over the remainder of the travel, thus avoiding any untimely load. However, this method can be applied only if the position is known reliably, i.e. it is not suitable in the previously presented case in which the installation is not properly adjusted following a manual operation.
A method of controlling an awning is known from document DE 90 03 416. The awning comprises sensor means for determining the zone of travel in which a load bar of the awning is located. This document relates to a method for controlling an awning with multiple extension and retraction positions. These multiple positions are attained automatically depending on the surrounding wind conditions. The mode of operation described implies that the positions are located precisely. When there are variations in wind speed relative to a threshold value, the awning is brought into another position.
A method for managing the extension of a wind-sensitive awning is known from document EP 1 752 597.
A method for tensioning the fabric of an awning with arms in its completely extended position is known from document US 2007/0247100.
Means for stopping an awning with arms in extended positions and in the retracted position is also known from document US 2002/089209.
SUMMARY OF THE INVENTION
The aim of the invention is to provide a method of operating an actuator that solves the above mentioned problems and improves the methods of operation known from the prior art. In particular, when resetting is necessary, the invention allows prior determination in an overall manner of the position of the awning in order to authorize an automatic position reset without intervention by the user and without error. It also enables the use of fairly low detection thresholds so as not to damage the installation when detecting the stop.
DESCRIPTION OF THE DRAWINGS
The appended drawing represents, by way of example, an embodiment of a solar protection installation according to the invention and an implementation of a method for operating such an installation.
FIG. 1 is a diagram of a solar protection installation according to the invention.
FIG. 2 is a diagram of an actuator of such an installation.
FIGS. 3 , 4 and 5 are diagrams illustrating the principle of the method of operation according to the invention.
FIGS. 6 and 7 are diagrams illustrating the principles of parameter measurement used in the method of operation according to the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The solar protection installation 1 , in particular a motorized awning with arms, comprises a roller tube 21 around which an awning fabric 3 is wound in a box 2 . The installation also comprises hinged arms 4 mounted on one side on a bearing structure and equipped with springs 10 that are stretched when the arms are retracted. The other end of the arms is connected to a bar 5 fixed at the bottom of the fabric 3 . A tubular actuator 6 inserted inside the roller tube 21 (or drive tube) causes the latter to rotate. The actuator comprises a control unit 8 allowing it to manage control commands to extend or retract the fabric. When there is a command to extend, the actuator permits an extension of the arms under the action of the springs and a rotation of the roller tube in a first direction, which leads to extension of the fabric. Conversely, when there is a command to retract, the actuator causes rotation of the roller tube in the opposite direction, which has the effect of tightening the fabric and of retracting the arms while stretching the springs.
The actuator 6 comprises a driver or geared motor part 6 a and a brake 6 b . The brake is able to obstruct rotation of the output axis so as to control the speed of rotation and also to keep the roller tube locked.
During extension of the fabric, the actuator 6 at least partly releases the brake 6 b and therefore allows rotation of the roller tube in the first direction under the action of the springs 10 . The load bar 5 and the fabric 3 are then driven towards the completely extended position.
The actuator also comprises measurement means 7 for measuring an internal parameter of the actuator, representing the torque exerted by the actuator 6 on the tube 21 driving the fabric.
The actuator also comprises stop detection means 9 . The means may, for example, operate by detecting a predetermined torque, a variation in torque or a predetermined variation in speed. The measurement means 7 and the stop detection means may be at least partly common. The stop detection means enable detection of the end stop of the travel to retract the awning (i.e. the position in which the awning is completely wound) or an obstacle in the travel of the load bar of the awning.
The electronic control unit 8 manages control commands to rotate the roller tube in one direction or the other, and manages stops, especially using information provided by the measurement means 7 , the stop detection means 9 and/or a position sensor. The control unit also comprises software means for implementing a method of operation according to the invention, this method governing the operation of an actuator of an awning with arms. These software means comprise computer programs.
For such a terrace awning with arms, six particular operational zones (ZF) are distinguished:
These zones are marked in FIG. 3 .
ZF 1 : when being extended, between the high position and the position called the arm-locking position, the latter corresponding generally to a lower limit of travel.
ZF 3 : when being extended, beyond the arm-locking position, the fabric hence unwinding freely.
ZF 4 : when being raised, before the arm-locking position, the fabric hence winding freely.
ZF 6 : when being raised, after this locking position.
ZF 2 , ZF 5 : border operational zones, corresponding to passing the particular position of the locking of the arms during extension and during retraction respectively.
Also distinguished are fabric positioning zones ZP 1 , ZP 2 , situated on both sides of the particular arm-locking position, and a positioning zone ZP 3 corresponding to the zone of the arm-locking position.
An operational zone differs from a positioning zone in particular through the effect of the direction of movement.
Awnings with arms have the particular feature of being extended under the effect of springs linked to the arms, each arm being provided with a central hinge and capable of being extended slightly more than 180°. The particular position in which the arms are extended slightly beyond 180°, in a maximum stable position, is called the locking position.
When being extended in an operational zone ZF 1 , the arms therefore extend under the effect of the springs and pull the awning fabric, the actuator then being released or functioning as a generator. When the hinge is opened by more than 180°, called arm locking (operational zone ZF 2 ) the fabric abruptly shifts from a stretched state to an unstretched state in so far as the arms have reached a position of maximum stable extension. They no longer stretch the fabric. The arms are then said to be locked. Beyond this, if the awning continues to be unwound, the operational zone ZF 3 becomes applicable: the fabric unwinds freely.
Conversely, when being raised, if the fabric has been unwound in a mode of operation of the type ZF 3 , the fabric must be re-wound. As the fabric is unstretched, this movement causes only a very small load on the actuator. This mode of operation is hence a mode of operation in the zone ZF 4 .
Next, in an operational zone ZF 5 , the actuator must create a large torque in order to retract the arms from this arm-locking position, i.e. in order to unlock the arms and leave this stable position. In an operational zone ZF 6 the actuator acts on the fabric and this must pull on the arms in order to bring them, against the action of the springs, into a retracted position.
If the trigger level of the stop detection means is low, in order not to risk damaging the awning when it arrives at the stop, passing this locking position may be considered by the stop detection means as equivalent to arriving at a stop. Depending on the real position of the awning during resetting, it may be impossible to reset the product to a real stop or even to learn a false reference position. These errors may lead to serious damage to the awning or undesired behaviors.
Some operational zones are, however, characterized by a particular signature linked with the torque, in particular with the voltage U capa at the terminals of a phase-shifting capacitor of an asynchronous motor. The measurement of the voltage U capa stands for an increase or a drop in torque depending on whether the actuator is functioning as a motor or a generator.
The various operational zones are marked on the graph of FIG. 4 , showing the voltage taken at the terminals of the phase-shifting capacitor as a function of time over one operating cycle of extension and retraction.
The value of the voltage U capa alone does not, however, allow the positioning zone to be determined with certainty (the voltage value possibly varying according to various parameters such as temperature). In order to determine the positioning zone in which the awning is situated before resetting, the invention proposes carrying out a test defined by a short sequence of extension and retraction movements and analyzing the characteristics of the operational zones encountered (for example, the average value of the voltage U capa over each movement). These two values are then compared to determine the positioning zone of the awning.
Depending on the positioning zone the actuator defines whether it is necessary to render the stop detection inactive in order to pass the arm-locking position, or on the contrary to activate it in order to produce a reset towards a dead stop without damaging the product.
The operation is the following for the various positions defined in FIG. 5 :
Starting from Position 1 :
The operational zones successively encountered are ZF 1 and ZF 6 respectively. As the value of the parameter U capa (extension) in the zone ZF 1 is greater than the value of the parameter U capa (retraction) in the zone ZF 6 , the actuator deduces that the awning is in the positioning zone ZP 1 and that the stop detection should be activated when being raised.
Starting from Position 2 :
The operational zones successively encountered are ZF 3 and ZF 4 respectively. The forces to be provided by the actuator are solely to unwind and wind the unloaded fabric. As the value of the parameter U capa (extension) in the zone ZF 3 is approximately equal to the value of the parameter U capa (retraction) in the zone ZF 4 , the actuator deduces that the awning is in the positioning zone ZP 2 and that it is necessary to deactivate the stop detection for a first predetermined time when being raised, in order to pass the arm locking, then to reactivate it to detect the high stop.
Starting from Position 3 (During the Extension Phase, Arms Locked):
The operational zones successively encountered are ZF 1 /ZF 2 /ZF 3 and ZF 4 /ZF 5 /ZF 6 respectively. The moment the fabric is relaxed, i.e. the moment the arms lock, a large fall in the value of the voltage U capa occurs. A proper return to a position from the positioning zone ZP 1 must therefore be ensured during the raising phase of the test. As a precaution, when being raised, the stop detection is deactivated for a second predetermined time, in order to pass the arm locking, then later activated to detect the high stop.
If the first test is not enough to determine the positioning zone, the actuator may repeat this test, optionally with longer periods of movement.
Other parameters dependent on the operation of the actuator may be used to determine the characteristics of the operational zones encountered during the test, for example the rotation/displacement speed. Advantageously, these parameters directly or indirectly represent the forces applied or the torque provided by the actuator.
The reset test is preferably part of a resetting movement in the course of which the values measured by the stop detection means are analyzed but are not taken into account for stopping, in other words, the stop detection is deactivated over at least part of this resetting movement. The aim of this resetting movement is to allow stabilization of operation and hence of the measurements useful for stop detection, before searching for a hard stop in order to reset the current position counter. Otherwise, the start of the actuator itself may distort the stop detection measurements.
This resetting movement therefore comprises a first extension movement (represented by the symbol ▾) for a duration of around 2 seconds, followed by stopping (represented by the symbol ▪) and a retraction movement (represented by the symbol ▴) for at least 2 seconds. The resetting test preferably comprises data analysis of the back and forth travel of the awning, with the exception of measurements close to the kickturn position ZP AR of the awning.
It is also possible to test the position over a very short path. In the case represented in FIG. 5 , each test movement lasts only around 300 ms, in the course of which the stop detection means provide sample measurements of the voltage U capa . These are analyzed to deduce a mean for the voltage U capa at the kickturn position of the awning.
In the course of the samplings, the n first values, represented by the hatched areas, are not considered in order to account for the starting of the actuator and allow the measurement data to stabilize. By eliminating consideration of the n last values for back and forth travel sampling, symmetric sampling areas are ensured during extension and retraction.
Comparing the averages of samplings considered over the extension and retraction movements enables precise definition of the positioning zone ZP AR in which the awning is located at the moment of this kickturn. It is thus possible to deduce the positioning zone (ZP 1 , ZP 2 or ZP 3 ) at the time of the start of the resetting movement.
The positioning zones with risks of confusion are the areas ZP 2 and ZP 3 . In these two cases, it is necessary to make sure that the stop detection means are temporarily deactivated to avoid confusing the locking or unlocking of the arms with the arrival at the high stop and hence storing an incorrect reference position.
In these two cases, however, the awning is close to its lower position. It is therefore possible to deactivate the stop detection means temporarily without risking arriving quickly at the high stop. The duration of the temporary deactivation of the stop detection means may then be chosen arbitrarily to suit all types and sizes of awning. It may, for example, be equal to 2 seconds.
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A method of operating an electromechanical actuator ( 6 ) for an awning with arms ( 1 ), comprising a control unit ( 8 ), stop detection means ( 9 ) and means ( 7 ) for measuring a parameter (U capa ) of the actuator, the awning being able to move over its travel in at least a first (ZP 1 ) and a second (ZP 2 , ZP 3 ) positioning zone, the method comprising the following steps: upon detecting an initiating event, automatic determination, from the measurement of the parameter of the actuator, of the positioning zone in which the current position of the awning is located; and if the current position of the awning is located in the second positioning zone, temporary deactivation of the stop detection means for detecting a stop in the course of a movement of the awning towards a stop position.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to brake assemblies, especially vehicular brakes including brake rotors attached to wheel hubs. This invention particularly relates to brake rotor disc assemblies equipped with anti-lock brake devices.
2. Description of Related Art
Typically, vehicles are equipped with a brake system to provide controlled slowing or stopping of the wheels to halt movement of the vehicle. A common type of brake system is a disc brake assembly associated with the wheels that is actuated by hydraulic or pneumatic pressure generated by an operator of the vehicle depressing a foot pedal. As is known, a disc brake assembly generally includes a rotor secured to the wheel of the vehicle for rotation therewith. The rotor has a pair of opposed friction plates that are selectively engaged by brake shoes supported on opposite sides of the rotor for sliding movement relative thereto.
In operation, the brake pads, which are operatively connected to hydraulically actuated pistons, move between a non-braking position in which they are spaced apart from the opposed friction plates of the rotor and a braking position in which they are moved into frictional engagement with the opposed friction plates of the rotor. In response to actuation by an operator, typically by depressing a brake pedal, the piston urges the brake pads from the non-braking position to the braking position. By this, the brake pads frictionally engage the friction plates of the rotor and slow or stop the rotation of the associated wheel of the vehicle.
To improve braking control and vehicle safety, anti-lock brake systems have been developed. In accordance with these systems, rotation of the wheel is sensed, and the braking response is automatically controlled to avoid skidding situations in which the vehicle wheels lose traction and slide over the pavement rather than engaging the surface at a slower rotational speed.
In a typical anti-lock brake assembly 200 seen in FIGS. 8-11 , the rotor 210 is provided with a ring of teeth 212 , which are cast with the rotor, commonly referred to as an ABS (Anti-lock Braking System) tone ring. As the rotor 210 rotates, the rotating teeth 212 are read by an anti-lock brake sensor (not shown) that generates a signal for the anti-lock brake control system representative of the rotation of the wheel associated with the rotor 210 . The sensor reads the peaks of the teeth and the valleys between adjacent teeth, best seen in FIGS. 10 and 11 , and uses an algorithm to determine whether the associated wheel is slipping. If it is determined that the wheel is slipping, braking pressure is released. Obviously, the arrangement and geometry of the teeth influence the signal generated by the sensor. To ensure proper operation of the anti-lock brake system, the teeth must be regularly spaced, sized, and maintained to preserve the profile of the teeth. Many sensors use magnetic pulse generation, which is created as the teeth pass by the sensor. The strength and accuracy of the signal is determined by the magnetic properties of the tone ring and the ring's geometric accuracy. Inadequate magnetic signal strength or incorrect geometric shape may cause signal failure, which can be further influenced by rotating velocity.
Problems have arisen with anti-lock brake systems in terms of poor performance due to irregularities and corrosion of the teeth. In known rotor assemblies in which the teeth are cast with the rotor, the teeth are also subjected to machining and coating treatments that are applied to the rotor. The disc is typically coated with an anticorrosive material, such as Geomet or Magni type coatings, that has a friction property and a corrosion resistance property. The coating is intended to lengthen the shelf life of the rotor and impede corrosion. However, since the coating is present when the rotor is put in use and then wears away from the braking surface, the coating must have adequate friction properties so that the rotor functions properly during braking at the outset before the coating is worn off. These dual property constraints limit the possible types of coatings suitable for this application.
Another consideration regarding the coating relates to the teeth. As noted above, the teeth are cast with the rotor, and the coating is applied to the entire piece. However, the teeth involve different design considerations. As the teeth do not function as a friction surface, the friction property of the coating is irrelevant. Further, it is desirable to maintain the anti-corrosive coating on the teeth for the functional life of the assembly. However, coatings suitable for rotor application degrade at high temperatures. This does not pose a problem with respect to the braking surface, but the teeth are exposed to high temperatures during the braking process. Since they are formed integrally with the rotor, which is normally cast iron, they heat to high temperatures, such as 800-900° F., as the rotor heats up due to the heat generated during braking. When the coating breaks down, the teeth can corrode. Corrosion alters the geometry of the teeth and causes inaccurate readings from the anti-lock braking sensor. This significantly shortens the useful life of the brake rotor assembly. When the sensor generates inaccurate readings, the assembly requires repair or replacement.
A problem also exists due to the state of the art casting methods and tolerances, which exist in casting of the teeth. Cast teeth will not be sufficiently accurate for most applications, and the inaccuracy in geometry will cause signal failure at higher velocities. To further machine the teeth for accuracy adds significant additional cost.
Another problem with cast iron tone rings relates to the magnetic properties of cast iron and how the properties change with temperature. Since cast iron has a high carbon content, its magnetism is reduced when heated to high temperatures experienced during braking.
There is a need, therefore, to provide a brake rotor assembly for use with anti-lock brake systems that provides an accurate and durable sensor system. There is also a need for a sensor system that can be retrofit in existing assemblies that no longer provide accurate readings.
SUMMARY OF THE INVENTION
An aspect of the invention provides a brake assembly having a rotor with an ABS tone ring for use with an anti-lock brake assembly that provides accurate and reliable readings.
Another aspect of the invention provides a brake assembly having a rotor with an ABS tone ring for use with an anti-lock brake assembly that has a relatively long service life.
An additional aspect of the invention provides a brake assembly having a rotor with an ABS tone ring for use with an anti-lock brake assembly that accommodates more versatile and durable coatings suitable for high temperature environments at a reasonable cost.
A further aspect of embodiments of the invention provides a tone ring assembly that can be retrofit in existing brake rotor systems.
The invention is directed to a brake rotor disc assembly comprising a rotor disc having a braking surface and a hat portion for mounting to a wheel hub, wherein the hat portion includes a cylindrical body and a radial mounting flange, and a tone ring insert for use with an anti-lock braking system. The tone ring insert includes a cylindrical portion and a sensor flange having a radial surface with a plurality of spaced sensing formations disposed thereon. The cylindrical portion is mounted to the radial mounting flange such that the tone ring insert is positioned within and spaced from the cylindrical body.
The invention is also directed to a brake rotor disc assembly comprising a rotor disc, which has a braking surface and a hat portion for mounting to a wheel hub, and a tone ring insert assembly. The hat portion includes a cylindrical body and a mounting flange. The tone ring insert assembly is designed for use with an anti-lock braking system and includes a cylindrical spacer positioned in the hat portion and mounted to the mounting flange and a cap coupled to the cylindrical spacer and having a toothed flange.
The invention includes the brake rotor disc assembly in combination with an anti-lock braking system including a sensor that generates signals based on rotation of the tone ring insert assembly and in combination with a vehicle.
The invention further relates to a tone ring assembly for use in an anti-lock braking system comprising a cylindrical spacer having a first end and a second end, wherein the first end has a plurality of axial openings formed therein, and a cap having an axial engaging portion and a radial flange extending from the axial engaging portion, wherein the radial flange has a ring of spaced teeth formed in a surface thereof. The axial engaging portion is fixed to the second end of the cylindrical spacer.
In the tone ring assembly, the cylindrical spacer can be made of cast iron, while the cap is made of powder metal in a high precision process and has a corrosion resistant coating thereon.
These and other aspects of the invention will become apparent in view of the detailed description and drawings herein.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is described in conjunction with the following drawings in which like reference numerals designate like elements and wherein:
FIG. 1 is a top perspective view of the rotor disc assembly in accordance with this invention;
FIG. 2 is a bottom view of the rotor disc assembly of FIG. 1 ;
FIG. 3 is a top view of the rotor disc assembly of FIG. 1 ;
FIG. 4 is a side view of rotor disc assembly of FIG. 1 ;
FIG. 5 is an exploded side view in partial section taken along line A-A of FIG. 3 ;
FIG. 6 is an enlarged partial side view of in section taken along line A-A of FIG. 3 ;
FIG. 7 is an exploded bottom perspective view of the assembly of FIG. 1 ;
FIG. 8 is a bottom perspective view of a prior art rotor disc assembly;
FIG. 9 is a bottom view of the rotor disc assembly of FIG. 8 ;
FIG. 10 is a sectional side view taken along line B-B of FIG. 9 ; and
FIG. 11 is an enlarged view of section C of FIG. 9 .
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The disc brake rotor assembly described herein is preferred for use on vehicles, including automobiles, racing vehicles, trucks, heavy duty trucks, motorcycles and the like. The vehicles particularly suitable for use with this invention can include those vehicles having a gross vehicle weight of about 10,000 pounds and above, especially delivery trucks and buses. However, the inventive concepts discussed herein can be used in any type of application that uses rotary brakes, including automotive, other types of motorized vehicles, or railcars. The invention is especially applicable for retrofitting in existing vehicles.
FIG. 1 shows a brake rotor disc assembly 10 in accordance with the invention. The brake rotor disc assembly 10 includes a rotor disc 12 having a pair of opposed braking plates 14 , 16 with friction material on the surface of each plate and a hat portion 18 for connection to a wheel hub (not shown) as is known. The hat portion 18 is defined by a cylindrical body 19 and a mounting flange 20 . The mounting flange 20 has a series of openings 21 to receive fasteners for connection to the wheel hub. Another series of openings 22 , best seen in FIG. 3 , are provided on the outer edge of the mounting flange 20 . Preferably, the openings 22 are formed as counterbores. The rotor disc 12 shown in FIG. 1 is a ventilated disc with vanes 24 formed between the braking plates 14 , 16 ; however, this invention can be employed in single plate discs as well, as would be readily recognized by those of ordinary skill in the art. The rotor disc 12 is preferably made of cast iron. However, any conventionally known material may be used, including a composite.
In accordance with this invention, an independent toothed ring insert assembly or ABS tone ring insert is coupled to the rotor disc 12 . The toothed ring insert can be formed as a single piece in which the ring has teeth formed on a radial flange. With a single piece, any suitable material could be used. For example, the insert could be made entirely of powder metal with a corrosion resistant coating formed thereon. Alternatively, the insert could be made by molding a steel stamping into a high temperature resistant plastic or rubber. To reduce costs and offer additional material alternatives, the insert could be formed in two pieces. This configuration is illustrated in the drawings, but it will be recognized to those of ordinary skill in the art that the design of a one-piece insert would be similar except that the two pieces would be a unitary piece.
Referring to FIGS. 1-7 , a toothed ring insert 26 is shown coupled to the rotor disc 12 . The insert 26 is formed in two pieces. The first piece is a cylindrical portion or spacer 28 having an annular side wall with a series of axial counterbore threaded openings 30 formed in one end. The other end has an interior annular groove 32 formed therein. Preferably the cylindrical spacer 28 is formed of cast iron, which is durable and relatively low cost. The second piece is a cap 34 that is formed as a toothed ring. The cap 34 is formed as a radial flange 36 including a ring of spaced teeth 38 and an axial engaging portion 40 . The cap 34 is made with highly accurate geometry to form well defined teeth that interact with the ABS sensor. The teeth 38 can be any type of sensing formations, such as serrations, alternating peaks and valleys, or openings. Preferably, the cap 34 is made by stamping, molding with powder metal or by machining. For cost purposes, a powder metal part or stamped part is preferred.
This assembly takes advantage of the lower cost of the cast iron cylindrical spacer 28 and high geometric accuracy and heat resistant magnetic properties of the powder metal cap 34 by connecting the two pieces together to act as the tone ring insert assembly 26 . The coupling can be achieved by a press fit, bolt, screw, pin, snap ring, thread or tongue and groove. One method of connection would be to use a protruding lip on the cap that is press fit within the spacer 28 to engage the annular groove 32 . Alternatively, the annular groove in the spacer 28 could be formed as an exterior annular groove with the same connecting effect. As best seen in FIGS. 5 and 6 , a preferred method of connection is to knurl or serrate the axial engaging portion 40 and press fit the portion 40 into the groove 32 of the spacer 28 . Of course, any type of known connecting method can be used to achieve an integral component formed of two separate pieces. For example, connection can be made by a bolt, a pin, a snap ring, threads, or tongue and groove.
Another advantage of using two pieces for the tone ring insert 26 is that only the cap 34 needs corrosion resistant coating to protect the geometry of the teeth 38 and prevent corrosion build up to ensure accurate readings from the ring. This reduces costs as the cast iron spacer 28 does not need a coating. A preferred coating is an electroless plating process, as is known in the art. For example, electroless nickel can be used for corrosion resistance. Of course, any suitable coating can be used, including any electro-plating, electroless-plating or metallurgical plating. In the case of a one piece insert, the entire piece could be coated if desired.
The ring insert 26 is assembled with the rotor disc 12 by inserting the ring insert 26 into the hat portion 18 , as seen in FIGS. 6-7 . A plurality of fasteners is used to connect the ring insert 26 to the mounting flange 20 by extending through openings 22 into threaded openings 30 . By this, the ring insert 26 is fastened to the rotor disc 12 at the wheel mounting face, which is the farthest point from the heat generating friction faces 14 , 16 and is least susceptible to thermal deformation. As seen in FIG. 6 , the ring insert 26 is independent of and spaced from the cylindrical body 19 , which provides some thermal insulation to the ring insert 26 , especially as compared to conventional integral toothed rotors in anti-lock brake assemblies. Also, since the ring insert 26 is fastened to the mounting flange 20 and sits within the hat portion 18 , radially inwardly from the braking plates 14 , 16 , any twisting or bending experienced by braking plates 14 , 16 due to thermal stresses induced during braking would not be translated to the ring insert 26 . Additionally, by forming the ring insert 26 separately from the rotor disc 12 , the choice of coating materials for the cap 34 is expanded as the coating material for the teeth does not need the friction quality required by the braking plates 14 , 16 .
The assembly 10 can be originally manufactured or retrofit on vehicles into existing brake rotor systems to replace ABS systems that no longer provide accurate readings due to incorrect geometries and/or corrosion. First, the cap 34 is fixed to the spacer 28 to assemble the tone ring insert assembly 26 . The assembly 26 is then secured to the mounting flange 20 of a brake rotor disc 12 with the fasteners as described above. The entire assembly 10 is then installed in place of a conventional brake rotor. Of course, if a one-piece insert is used, the entire insert is simply installed to the mounting flange of the brake rotor disc. Since the toothed cap 34 is formed with a high precision process such as stamping, molded from powder metal, or machined, the geometry is highly accurate. The corrosion resistant coating on the toothed cap 34 ensures that corrosion will not occur and compromise the geometry of the teeth or interfere with sensor readings. Accordingly, a highly reliable brake rotor disc assembly 10 can be retrofit into an existing vehicle at a relatively low cost.
It can be appreciated that the ring insert 26 functions in the same manner as known toothed rings associated with brake rotor discs with anti-locking braking systems. The rotation of the teeth 38 is sensed by an anti-locking sensor to assess whether the wheel is slipping. The braking action is adjusting accordingly. Using this invention, however, will provide a more accurate and reliable reading since corrosion of the teeth is minimized and the teeth can be formed with high precision. This invention will also provide a longer service life for brake assemblies, especially in large vehicles, such as delivery trucks and buses and allow degraded tone rings to be easily replaced.
The invention is not limited to those embodiments described herein and may encompass various changes and modifications. It will be understood that the various modifications shown herein can be used in any combination. It is also possible to eliminate various components of the assembly and still have an effective connection. Further, different materials may be used to obtain similar results.
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A disc brake assembly includes a rotor with an ABS tone ring insert assembly that functions as a rotation indicator in an anti-lock braking system. The insert is positioned in the hat of a rotor disc in a spaced relationship and is mounted to the mounting flange of the rotor disc. Forming the ring insert separately from the rotor disc also allows different coating materials to be used on the tone ring that may be more heat resistant. The ring insert assembly can be made of powder metal or made as a cast iron cylinder with a toothed cap made of powder metal having a corrosion resistant coating. Cost savings can be realized along with high performance when only a portion of the assembly if made of powder metal and coated.
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BACKGROUND OF THE INVENTION
This invention relates to control switch assemblies, and more particularly, to a digitally rotatable control switch assembly, which is adapted for use in an electric appliance capable of multiple mode operation wherein each mode may contain a range of differing values.
A wide increase in the use of consumer-operated convenience appliances has occurred in recent years, and an increased adaptibility of these appliances has imposed additional requirements for the control systems or switches utilized in these appliances. Due to the increased sophistication of these appliances, a need has arisen for improved switches capable of controlling use of these machines through a full range of their operation. Additionally, even complicated appliances adapted for consumer use should have controls which are simple to operate.
For example, improvements in consumer appliances such as hand-held hair stylers have increased the need for more complex control switches to operate same. Simple on-off switches have been inadequate for controlling hand-held hair stylers for some time. Multiple position switches have been developed which provide hand-held hair stylers with high air flow capability for drying hair, and with low air flow capability for styling hair. Further, providing increased wattage in hair stylers has allowed more heat to be generated for faster drying of a user's hair. However, while added wattage is desirable for faster drying, it may have drawbacks where styling is concerned. Therefore, multiple separately and cooperatively operable heating elements have been developed for hair stylers, thus necessitating switches engineered to control the increasingly complex machines.
In addition to these developments, the types of fans utilized with these appliances have changed over the years from radial flow fans to transverse flow fans, and more recently, to axial flow fans. The recent introduction of axial flow fans has allowed the shape of hair styler-dryers to be changed by eliminating the necessity for a handle extending perpendicularly to the flow of air such as found in stylers utilizing a transverse flow fan. With use of transverse flow fans, elongate in-line movable type control switches, such as is found in U.S. Pat. No. 3,839,614, issued Oct. 1, 1974 to the assignee of the present application, were conventionally positioned in a hollow area in the styler handle. However, the elimination of the elongate handle in axial flow fan type hair stylers has increased the need for an improved control switch.
It is therefore an object of the present invention, generally stated, to provide an improved digitally rotatable control switch assembly for an electric appliance operable in a plurality of changeable modes.
It is a more specific object of the present invention to provide an improved, more compact, rotatable control switch assembly for a hair styling appliance.
Another object of the invention is the provision of a rotatable control switch assembly adapted for use in a hair styling appliance of the axial flow fan type wherein the rotation of a single control switch knob provides digital control for both fan speed and heating element wattage output.
SUMMARY OF THE INVENTION
The invention is directed to an appliance which is operable in a digitally changeable first electrical mode and a digitally changeable second electrical mode. The appliance incorporates a body having a knob rotatably mounted thereon which controls the changes in each respective mode. The appliance further includes a control switch assembly comprising a switch housing having a plurality of resilient electrical contacts fixedly mounted in spaced relation therearound. A rotatable commutator assembly is mounted on the housing and includes an insulative disc shaped base having a generally circular outline defining a plurality of detent portions positioned therearound. The detents are adapted to engage the fixed contacts with the contacts resisting the rotation of the base between the detents to define a plurality of discrete stops or operating positions. Primary and secondary contacts are mounted on opposing sides of the disc-shaped base. The primary and secondary contacts are made of conductive material and extend slightly outwardly of the circumference of the base at desired positions therealong for conductively connecting and disconnecting the chosen ones of the plurality of fixed contacts as the base is rotated on the switch housing.
BRIEF DESCRIPTION OF THE DRAWINGS
The features of the present invention, which are believed to be novel, are set forth with particularity in the appended claims. The invention may best be understood from the following detailed description of a currently preferred embodiment thereof, taken in conjunction with the accompanying drawings, wherein:
FIG. 1 is a perspective view of the hand-held hair styling appliance of the axial flow fan type incorporating the rotatable control switch assembly of the present invention therein.
FIG. 2 is an exploded perspective view of the hair styling appliance of FIG. 1 showing the interrelation of the heating element, motor, fan, and control switching assembly parts utilized therein.
FIG. 3 is a fragmentary cross-sectional view taken along line 3--3 of FIG. 1.
FIG. 4 is a schematic diagram of an electric circuit for the hair styler-dryer shown in FIG. 1.
FIG. 5 is a fragmentary cross-sectional view of the control switch assembly taken along line 5--5 of FIG. 3.
FIG. 6 is a cross-sectional view taken along line 6--6 of FIG. 3.
FIG. 7 is a cross-sectional view similar to FIG. 6 with the switch commutator rotated one operating position clockwise from that shown in FIG. 6.
FIG. 8 is a cross-sectional view similar to FIG. 6 with the switch commutator rotated two operating positions clockwise from that shown in FIG. 6.
FIG. 9 is a cross-sectional view similar to FIG. 6 wherein the switch commutator has been rotated three operating positions clockwise from that shown in FIG. 6.
FIG. 10 is a cross-sectionl view similar to FIG. 6 wherein the switch commutator has been rotated four operating positions clockwise from that shown in FIG. 6.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, the hand-held hair styling appliance incorporating the control switch assembly of the present invention, generally indicated at 20, includes a tubular fan and heater assembly housing 21 together with an annular air inlet and switch housing 22. Housing 22 is releasibly connected to housing 21 by a plurality of bayonet fasterners. Hair styling appliance 20 further includes an annular rotatably mounted switch knob 23 positioned axially adjacent housing 22. Knob 23 is operatively attached to a six position rotatable switch assembly of the invention which is fixedly secured to the interior of the housing 22. The electrical cord 24, through which power for the appliance is obtained, extends axially outwardly of the appliance at the distal end of the switch knob 23 and includes a conventional electric plug 25 positioned at the external end thereof. The changeable fan speed and adjustable heating power of the appliance is controlled by rotating the switch knob 23 to any one of the six positions marked thereon as shown in FIG. 1. In this embodient, the two outer operating positions, as marked, both produce off of open circuit conditions. The four internal operating positions provide both dual fan speed operation and four differing heater output wattages. The low fan speed operating condition is utilized with the two lower wattage output positions and the high fan speed operating condition is associated with the two higher wattage output positions.
As shown most clearly in FIG. 1, air passing through the styler 20 enters same through a plurality of air inlet ports 26--26 positioned around the tubular outline of the air inlet and switch housing 22. From the inlet ports 26--26 air flows through the fan and heater housing 21 from right to left as shown. First the air is pushed through the housing 21 by the fan and then is warmed by the heating element which is positioned adjacent the left end of the housing 21 as shown. The warm and rapid flowing air exits the styler 20 through a circular air outlet port 27 defining the left end of the appliance as shown. It should be noted that the styling attachments (not shown) may be releasibly attached to the air outlet housing 27 to adapt the appliance for various combing and brushing operations in connection with the styling and drying of a user's hair. The apparatus for providing the releasible connection between the housing 21 and the styling appliances (not shown) is the subject matter of a co-pending application Ser. No. 868,403, filed Jan. 10, 1978, which is assigned to the assignee of the present application.
The operating parts and portions of the appliance 20 are most clearly shown in FIG. 2 to include, in addition to the fan and heater housing 21, from the left the heater assembly 30 including an insulative frame 31, a protective perforate end cover 32, and heating coils 33 wrapped around the insulative frame 31. Additionally, a plurality of elongate buss bard 34--34 extend axially outwardly of the heating assembly frame 31. Buss bars 34--34 are electrically connected to respective ones of the fixed contact terminals of the switch assembly, to be discussed in further detail below. An annular plastic coupler 35 is positioned inside the hollow end arms 31a--31a of the insulative frame 31. A bridge rectifier 36 is also positioned inside the hollow end of the insulative frame 31 in conductive relation with the heating element 33 and selective ones of the buss bars 34--34. A conventional appliance motor 37 is conductively connected to the rectifier 36 and is affixed to the insulative frame 31 by being mounted in the hollow interior of the coupler 35. The electric motor 37 includes a power shaft 40 extending, as shown, from the right end thereof.
A tubular fan shroud 41 is mounted outwardly of the right end, as shown, of the insulator frame 31 so as to cover a portion of same and also cover a portion of the electric motor 37. An axial flow fan 42 is securely mounted on the output shaft 40 and positioned inside the fan shroud 41 to provide efficient flow of air through the appliance. An additional set of stationary fan blades (not shown) is positioned inside fan shroud 41. The stationary blades straighten the flow of air from fan 42 and change same from turbulent to laminar flow, thus providing more efficient passage across the heating coils 33. The fan and blades are the subject matter of a co-pending application Ser. No. 868,436, filed Jan. 10, 1978, and assigned to the assignee of the present invention. An annular ring 43 is mounted to the interior of the air inlet ports 26--26 in housing 22 to prevent the insertion of solid objects in those inlet ports.
As stated previously, the entire control switch assembly 44 is mounted in the air inlet and switch housing 22 and is covered by the switch control knob 23. In this embodiment, the control switch 44 of the invention is annular and has a hollow area centrally therethrough in which the electric cord 24 is positioned.
The switch assembly 44 of the invention includes a hollow switch body 45 having a generally hollow annular area (FIG. 3) therein and a central hollow stem 46 extending axially therethrough. A plurality (in this embodiment four) of resilient fixed contact arms 47--47 are mounted at one end thereof against the outer wall of the annular hollow portion of the switch body 45. The free ends of each contact 47 include a curved contact portion 47a which extends in a resilient manner inwardly of the fixed end thereof. An annular switch commutator or current distributing body 50, made of insulative material, is rotatably mounted in the hollow annular portion of the switch body 45 in a manner surrounding the body stem 46. The insulative comutator 50 includes a disc-shaped body and has a primary electrical contact or current-carrying bridge 52 mounted on one side thereof, and a secondary contact or current-carrying bridge 53 mounted on the opposing side thereof. The commutator 50 together with both contacts 52-53 mounted thereto will be referred to as the commutator assembly 49. The first primary contact 52 is generally crescent-shaped (almost annular) with a cylindrical surface and an irregular outer surface 67 which will be discussed in connection with FIGS. 5-10 below. The secondary contact 53 is also irregular in shape, is much smaller in this embodiment than primary contact 52, and the functional outer surface 70 thereof will be discussed in connection with FIGS. 5-10 below. The commutator 50 also includes a pair of hollow post member 51--51 extending in an axial direction from opposed sides of the disc.
An annular switch driver ring 54 is mounted on the dual commutator posts 51--51 by a pair of elongate rivets 55--55. The annular switch driver includes a pair of opposed arm receiving indents 56--56, the function of which will be discussed below. An annular switch cover 57 is secured to the air inlet and switch housing 22 by a plurality of elongate screws 60--60 in order to retain the switch assembly 44 in fixed position on housing 22. A cord strain relief member 62 and a flex relief member 63 are mounted around the electrical cord 24 and to the switch cover 57 to provide for the passage of electrical cord 24 therethrough. The switch knob 23 is then positioned in axial alignment with the switch assembly 44 over the switch cover 57 such that an opposed pair of arms 64-64 (only one shown in FIG. 2) extend through the switch cover 57 into driving engagement with the arm receiving indents 56--56 of the annular switch driver 54. Therefore, rotation of the switch knob 23 acts through its switch arms 64--64 to rotate the switch driver 54 and the current distributing assembly 49. In the switch assembly, differing combinations of electrical connections are made between the plurality of fixed electrical contacts 47--47 and the respective primary and secondary rotatable contacts 52,53.
Referring to FIG. 3, the switch assembly 44 of the present invention is mounted to the switch housing 22 by a pair of mounting posts 22a (only one shown) which extend in an axial direction from the interior of the housing 22. A pair of opposed semi-cylindrical indents 65--65 in the outer surface of the switch body 45 are positioned in alignment with the mounting posts 22a--22a to rotatably fix the switch body 45 in the appliance. The hollow annular switch cover 57 is mounted over the switch assembly 44 and secured to the mounting posts 22a--22a by elongate screws 60--60 (FIGS. 2 and 3) to prevent any axial movement of the switch assembly 44. Next, the switch knob 23 is mounted over the switch cover 57 until the annular bottom surface 58 of the knob engages the upper annular surface 22b of the switch housing 22 in sliding engagement therewith. Also, the sliding engagement between an inner annular flange 23b on the switch knob and a plurality of retaining surfaces 57a--57a on the switch cover 57 maintains the annular center of knob 23 in fixed relation along the axis of the appliance while allowing its rotation thereon.
As shown most clearly in FIG. 3, the hollow annular interior of switch body 45 is defined by an axially extending outer flange or wall 65, an annular bottom wall 66 extending inwardly of the flange 65, and the body tubular stem 46 which extends axially from the inner edge of wall 66. Together, the three surfaces define a hollow annular mounting area for the switch contacts 47--47 and commutator assembly 49. The width of resilient fixed switch contacts 47--47 is sufficient to extend from switch body bottom surface 66 to the plane defined by the annular distal end 65a of the switch outer flange 65. Therefore, each distal end 47a of the contacts 47--47 is slidably engageable with the outer circumferential surface 68 of the insulative commutator 50, the outer surface 67 of the primary contact 52 and the outer surface 70 of the secondary contact 53. As is also shown in FIG. 3, an axially extending detent 71 is positioned in an arcuately extending indent 72 positioned in the bottom surface 66 of the switch body 45. In this embodiment, the length of indent 72 is sufficient to limit the rotation of the commutator 50 in the switch body 45 to the six desired switch positions.
The shapes of the respective operative portions of the fixed contacts 47--47, the commutator 50, the primary contact 52 and secondary contact 53 are shown most clearly in FIGS. 5-10 for each of the six operative positions of the rotatable switch assembly 44 of the invention. Further, the opposing disc-shaped sides of the commutator 50 shown in FIGS. 5 and 6 disclose the digitally operative indent-detent relation between the outer circumferential surfaces 67, 68 and 70 making up the current distributing assembly and the curved end portions 47a--47a of the resilient biased contacts 47--47.
In this embodiment, the outer circumference of each switch body 45 includes a T-shape indent 72 in communication therewith at four positions equally spaced therearound. One end of a fixed resilient contact 47 is fixedly mounted to each T-shape indent such that a wire lead 73 may be secured thereto. The four wire leads, in this embodiment, are connected to the respective heating coils, and the bridge rectifier, through the conductive strips 34--34 mentioned previously. In addition, one of the wire leads 73 is attached to the input side of the electric cord 24 to provide a source of electricity to pass through the switch assembly 44. As shown most clearly in FIGS. 5-10, a plurality of convex curved surfaces 74--74 are positioned around the interior surface of the outer radial flange 65 of the switch body 45 adjacent each T-shape indent 72 to inwardly bias the curved distal end 47a of each of the resilient contacts 47. Further, as each contact 47 is bent outwardly by rotating the commutator 50, the area of surface engagement between the contact 47 and the concave surface 74 thereadjacent increases, thereby de-localizing the bending stress in the contact. Speading the bending stress across a substantial portion of the length of the contact 47 increases the operating life of the switch.
While the outer annular surface 68 or circumference of the commutator 50 is generally circular, as shown most clearly in FIGS. 5-10 the surface includes a plurality of evenly spaced gently curved detent-indent portions, lettered A-T counterclockwise around the commutator in FIG. 5 and clockwise in FIGS. 6-10. Each letter indent portion has associated with it an outward curved detent portion positioned immediately adjacent thereto counter-clockwise therefrom in FIG. 5 and clockwise therefrom in FIGS. 6-10 which will be designated by the same letter. Indents-detents on both the primary and secondary contacts are aligned with the indents-detents A-T on the commutator and will also be so designated by those same letters. Also, the respective fixed contact arms 47 have, for clarity, been designated 47(1) through 47(4).
It is understood that since each of the fixed contact arms 47(1-4) exerts a radially inwardly directed pressure on the commutator assembly 49, the rotatable position of the commutator 50 is stabilized when the respective resilient contacts 47)1-4) are resting in respective indent portions (A-T) around the outer circumference of the commutator 50. By applying a twisting or moment force to the switch knob 23, the commutator assembly 49 is moved digitally from one indent portion to the next adjacent indent portion thereon, up to the limits determined by detent 71 and arcuate indent 72.
Referring to FIG. 4, the electric circuit for the present embodiment of the hair styler includes the switch assembly 44, a bridge rectifier 36 connected to the motor 37, and a heating coil 33a in one line, adding heating coils 33b and 33c in additional lines, and a bi-metallic strip type thermostat 82 positioned in-line with a thermal fuse 83 as a back-up safety device completing the circuit to the power source. The operation of the circuit will be discussed below in connection with the operation of the swtich assembly 44.
As shown most clearly in FIG. 5, the secondary contact 53 is riveted at 75 to the commutator 50. The secondary contact 53, in this embodiment, is irregularly shaped as shown in solid line and includes a portion of the detent designated H, the indent and detent both designated I, the indent J and a portion of the detent designated J. The outer circumferential surface 68 of the commutator 50 has been notched inwardly at 76 (shown in dotted line) a small distance to allow the outer surface 70 of the secondary contact 53 to extend slightly radially outwardly thereof, thus providing improved biased surface engagement with any fixed contact 47(1-4) which the surface 70 touches.
Referring to FIGS. 5 and 6, the irregular, but generally annular or crescent shaped primary contact 52 is riveted at 86 to the annular commutator 50 and extends around a substantial portion thereof. In an identical manner as with the secondary contact, additional portions of the circumference 75 of commutator 50 are notched at 77, 80, 81, and 82 to allow respective portions of the outer circumference of primary contact 52 to extend slightly radially outwardly of the commutator and provide better contact with the respective fixed contacts 47(1-4). As shown in FIGS. 5 and 6, a portion of the detent H on secondary contact 53 is overlapped with a portion of the primary contact 52 which is rigidly mounted on the opposite side of commutator 50. This overlap, designated A-A, assures continuity of current flow in the circuit when the commutator 50 is rotated such that a fixed contact 47 moves between indent H and I. As further shown in FIGS. 6-10, the portions of the outer circumference of the primary contact 52 such as those portions shown most clearly in indents Q and S, have radially extending side surfaces which are positioned off-center from the respective indents and detents to time the respective start-up and break of current flow between the respective fixed contacts 47--47. This will be discussed in detail in connection with the operation of the switch through each of the six operating positions shown in FIGS. 5-10. The operation of the appliance should also be followed by reference to the schematic diagram of FIG. 4 as differing switch positions are described below.
Referring to FIG. 5, the switch assembly 44 of the invention is shown in a first operating position, which provides the appliance with an off or open circuit condition. One of the fixed contacts 47(1-4) is positioned in each of the respective detents A, F, K, and P of the outer circumference of the commutator 50 such that no current flows between the respective contacts.
As shown most clearly in FIG. 6, the commutator assembly 49 has been rotated one indent from the position shown in FIG. 5 to what is identified as a second operative position. It should be noted that the view of FIG. 6 is of the opposite side of the commutator 50 from that shown in FIG. 5. Therefore, the positions of the respective indents-detents A-T are reversed from that shown in FIG. 5. In the second operative position, current flows through contact 47(4) from electrical cord 24 and into the primary contact 52 at indent O. Current then flows through the primary contact 52 through the rivet 77, through a half-wave rectifier or diode 80 affixed to the rivet 77, and through the rivet 81, which is rigidly affixed to both the opposing end of diode 80 and the secondary contact 53. At indent J on the secondary contact 53 the half-wave rectified current passes to fixed contact 47(3). Next (FIG. 4), the current flows out of the switch assembly 44, through the conventional three-phase bridge rectifier 36, and from the rectifier to the motor 37 and through the heating coil 33a. The switch of the invention is engineered such that the motor 37 is turned on before any heating coil is turned on, and the motor may not be turned off until the last heating coil is turned off. Also, since the current passes through the half-wave rectifier 80 as it travels between contact 47(4) and 47(3), the rotational speed of motor 37 is substantially lowered from that speed the motor would obtain if the half-wave rectifier were eliminated from the circuit line. Approximately 100 watts of power in the form of half-wave current passes through the motor 37 and heating coil 33a to move air through the fan and concurrently heat it.
Referring to FIGS. 4 and 7, the commutator assembly 49 of the switch 44 has been rotated one indent clockwise from that position shown in FIG. 6 to a third operative position. In this position, current moves from the fixed contact 47(4) into the primary contact 52 at indent N. Next, one branch of current moves through primary contact 52, through the diode 80 as described previously, through the secondary contact 53, and then to fixed contact 47(3) at indent I. From fixed contact 47(3) the half-wave rectified current again flows out of switch 44, through the bridge rectifier 36, into the motor 37 to drive the fan 42, and also into the heating coil 33a. It should be noted that there is no interruption in current flow into the motor 37 as the contact 47(3) is moved from indent J to indent I by rotation of the commutator assembly 49.
As shown in FIG. 7, the primary contact 52 engages the fixed contact 47(1) at indent S and a second branch of current flows therethrough. It should be noted that what is termed indent S on the commutator assembly 49 also defines a detent portion on the primary contact 52. Portions of the contact 52 to either side (angularly) of S are cut radially inwardly such that the insulative commutator 50 forms the adjacent indent-detent R and the detent S. From contact 47(1) an additional heating coil 33b is electrically energized to provide, together with coil 33a, a total of approximately 400 watts of heating power to the air flowing through the appliance.
Referring to FIGS. 4 and 8, the commutator assembly 49 has been rotated one indent clockwise from that shown in FIG. 7 to the fourth operating position. The current flow through the commutator assembly is from fixed contact 47(4) to the primary contact 52 through contact 47(3) at indent H. It should be noted that this current does not flow through the secondary contact 53 and is therefor of full wave strength. This full wave current flows from contact 47(3) out of the switch and through the bridge rectifier 36, the motor 37, and through the heating coil 33a. As stated previously, an overlap exists between the engagement of the primary and secondary contacts with the fixed contact 47(3). This overlap provides continuous operation of the motor 37 while the commutator assembly 49 is being rotated to raise the motor output speed. The continuous motor operation feature also is present when the commutator 50 is rotate counter-clockwise and the motor output speed is lowered. Additionally, current flows in another branch from the primary contact 52 to the fixed contact 47(2) through indent C. From contact 47(2) the current flows through heating coil 33c. It should be noted that the current flowing through contact 47(1) in FIG. 6 has been opened as contact 47(1) now resides in indent R of commutator 50. Timing wise, the primary contact indents are shaped as shown in the drawings such that the motor speed increases (contact 47(3) engages primary contact 52) before the coil 33a is turned on (contact 47(2) engages primary contact 52 at indent C). Further, the primary contact 52 disengages contact 47(1) at indent S before coil 33a is turned on. The combination of heating coils 33a and 33c provide approximately 600 watts of heating power to the air flowing through the appliance and the full wave strength current through the motor 37 provides for high-speed fan operation.
As shown most clearly in FIGS. 4 and 9, the fifth operative position of the commutator assembly 49 is rotated one indent clockwise from the position shown in FIG. 8. In FIG. 9, current flows from the contact 47(4) to the primary contact 52 through the indent L. From primary contact 52, one branch of the full-wave current flows into fixed contact 47(3) at indent G and thence, as described previously, through the bridge rectifier 36, the motor 37, and the heating coil 33a. A second branch of current flows from primary contact 52 to fixed contact 47(2) through indent B and thence through heating coil 33c. A third branch of current flows from indent Q of the primary contact 52 to the fixed contact 47(1) which actuates heating coil 33b. The combination of heating coils 33a, 33b, and 33c provides approximately one thousand watts of heating power to the air flow. In addition, the motor is moving in the high speed mode as the current through the motor is of full wave direct current strength.
Referring to FIGS. 4 and 10, the commutator assembly 29 of the rotatable switch 44 of the invention is shown rotated one indent clockwise from its position in FIG. 9 which is the sixth and last operative position, a second off or open circuit condition. None of the contacts 47(1-4) in FIG. 10 is in contact with either primary contact 52 or secondary contact 53. All contacts are engaging the insulative commutator 50. This duplication of the open circuit conditio is beneficial as it is positioned immediately adjacent the high-power fast-speed fifth operating position shown in FIG. 9. Therefore, if an appliance user prefers the high-speed operating position to any other, the appliance may be maintained in the final off-position to any other, the appliance may be maintained in the final off-position shown in FIG. 10 unil the appliance's use is desired. The high-speed high-power output condition can be reached from the sixth operating position by one click of the switch, rather than by five clicks of the switch from the opposing first operating or off position shown in FIG. 5.
It should be noted that reverse rotation of the switch provides opposite phasing for the various operational changes from position to position. Regardless of the change of switch positions, it should be noted that the contact 47(3) is engaged first and disengaged last, such that the motor 37 and fan 42 run both before the heating coils have been turned on, and after the heating coils have been turned off, with the exception of the smallest heating coil 33a.
This safety feature assures that the heating coils cannot be turned on inadvertently when the motor 37 is not running. This condition is maintained even if the switch is stopped or held from moving between indents on the commutator assembly 49. Further, the construction of the switch is such that the motor speed is always increased before the high wattage heating coils are energized, and the high wattages heating coils are always de-energized before the motor speed is decreased.
While one embodiment of the present invention has been shown and described, it will be obvious to those skilled in the art that changes and modifications may be made without departing from the invention in its broader aspects. For example, while the embodiment of the appliance shown provides a maximum of approximately 1000 watts heating power, the switch of the invention may also be utilized with appliances having differing maximum power outputs, such as 1200, 1500, or even higher wattage values. Also, it should be noted that if the maximum wattage values for the appliance change, the intermediate switch position outputs will be changed in a like manner. Therefore, it is the aim in the appended claims to cover all such changes and modifications as fall within the true spirit and scope of the invention.
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A hand-held hair styling appliance incorporates an improved rotatable switch assembly which is mounted in the styler in axial alignment with the fan, thus eliminating the need for a handle in the appliance. The switch is constructed such that the heating elements are energized only when the motor is running, and the higher heat elements are energized only when the motor is operated in a high speed mode. The improved switch assembly is of an annular configuration having a central axial aperture through which a conventional electric cord is positioned. A switch housing includes a hollow annular work area in which a plurality of resilient electrical contacts are fixedly mounted. A commutator assembly includes a disc-shaped base which is rotatably mounted in a working portion of the housing. The base includes a plurality of evenly spaced detents positioned along the outer circumference thereof which engage the fixed contacts to provide discrete stopping positions during the rotation of same. Primary and secondary contacts are mounted on opposing sides of the disc and are shaped so as to provide a flow of current between fixed contacts, as desired, as the switch is discretely rotated in its various operating positions.
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BACKGROUND
[0001] This disclosure relates to a roof edge cable raceway that forms a channel at an edge of a roof of a structure for accommodating a cable. The raceway may accommodate a heating cable that melts snow and ice at an edge of a roof of a structure and otherwise prevents ice from accumulating on roof eaves. Although the disclosure is more focused toward a heating cable application, the raceway may also be used for other low voltage wiring applications like running security or audio wires adjacent the eave.
BRIEF DESCRIPTION OF THE DRAWINGS
[0002] Further detail of the disclosed embodiments follows in the detailed description below and is shown in the accompanying drawings wherein:
[0003] FIG. 1 is a schematic drawing showing a roof edge cable raceway comprising an edge attachment assembled with an overhanging drip edge mounted on an edge of a roof of a structure to form an open channel for housing a heating cable;
[0004] FIG. 2 is a schematic drawing showing an alternate embodiment of a roof edge cable raceway comprising the edge attachment of FIG. 1 and an overhanging drip edge with a second channel formed in a roof engagement portion of the overhanging drip edge for housing a second heating cable;
[0005] FIG. 3 is a schematic drawing showing an alternate embodiment of a roof edge cable raceway mounted on an edge of a roof of a structure with a monolithically formed open channel for housing a heating cable;
[0006] FIG. 4 is a schematic drawing showing an alternate embodiment of roof edge cable raceway mounted on an edge of a roof of a structure with a J-shaped cross-section adapted for housing a heating cable;
[0007] FIG. 5 is a schematic drawing showing an alternate embodiment of a roof edge cable raceway comprising an edge attachment secured to existing facia flashing provided on a structure to form a channel adapted for housing a heating cable;
[0008] FIG. 6 is a schematic drawings showing a partial edge view of a channel formed along an edge of a roof of a structure using any one of the roof edge cable raceways shown in FIGS. 1-5 with a heating cable disposed therein;
[0009] FIG. 7 is a schematic drawing showing a partial edge view of a channel formed along an edge of a corrugated roof of a structure with a curvilinear roof edge cable raceway with a heating cable disposed therein;
[0010] FIG. 8 is a schematic drawing of a clamping mechanism used to secure a heating cable to a point on a seam of a metal roof; and
[0011] FIG. 9 shows alternate embodiments of radiuses for sides of the channel or end edges of any of the edge attachments described herein.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0012] Often, ice dams form in very cold climates on the roof of a structure. The heat from inside the structure combined with ambient heat from sunlight will cause snow and ice from the upper roof to melt and drain as water to the roof overhang. Oftentimes, the roof overhang is colder than the upper roof because the underside of the roof overhang is not heated and sees no direct sunlight. This causes the melting snow and ice from the upper roof to refreeze at the roof edge causing an ice dam. An ice dam often causes the draining melting snow and ice to pool. Often, the pooling water backs up behind the ice dam and leaks into the structure causing damage to walls, ceilings, insulation, and electrical systems. The water can also lead to environmental issues such as mold and mildew. Often, an ice dam causes the formation of icicles an edge of a structure that cause a hazard.
[0013] Generally speaking, correct roof drainage requires about a three-quarter inch additional overhang of roofing material from the structure front face (facia board) to ensure drainage water flows into a gutter positioned adjacent to an edge of a roof of a structure. If the overhang is too short, melting snow and ice, and rain water will flow behind the gutter leading to rotted wood sheathing and facia, stained siding, soil erosion at the foundation below and, potentially, flooded basements. In some construction techniques, asphalt roofs often have a three-quarter inch overhang of shingles to drain water into the gutters. In some construction techniques, shingle or shake roofs have a metal drip edge that acts as a support for the extended shingles or shakes, and the shingles or shakes completely cover the metal drip edge.
[0014] The roof edge cable raceway with an associated heating cable installed therein as described below prevents the formation of ice dams while improving the visual appearance of the structure in which the apparatus and heating cable is installed. The roof edge cable raceway described below may be used with many roofing types, including metal, raised seam metal, corrugated metal, shake, and conventional asphalt shingles, and may be used on residential housing, industrial buildings, bridges, electrical transformers, outdoor cabinets, enclosures and other structures. As described below and shown in FIG. 1-7 , the roof edge cable raceway forms a channel that extends along an edge of a roof of a structure. When a heating cable is installed in the channel, the effect of heat transfer from the cable to a heat conductive portion of the drip edge heats the edge of the roof sufficiently to prevent or melt any ice dams, thereby enhancing drainage of melting snow and ice and preventing the formation of icicles. As described below and shown in FIG. 1-7 , the roof edge cable raceway may comprise an edge attachment fitted to a drip edge, for instance, an existing overhanging drip edge already installed on an edge of a roof of a structure, or may comprise a drip edge, or an overhanging style drip edge, with an integrally formed (if not monolithically formed) open channel structure.
[0015] The roof edge cable raceway and open channel structure may be configured to house a resistance-type heating cable, or a self-regulating heating cable, or other low voltage style cabling applications, for instance, cables used for lighting, security cameras or audio speakers. Generally speaking, in a heating cable application as described below, the heating cable must have a snug fit in the channel to maximize heat transfer from the heating cable to the roof. Although not necessary, the entire roof edge cable raceway may be formed from a heat conductive material to simplify construction. In the alternative, the side of the channel adjacent the edge of the roof, and the portion of the roofing materials in contact therewith may be formed from a heat conductive material to allow heat transfer to the area adjacent the roof edge, or in an alternate use where heat transfer is not critical, i.e., low voltage style cabling applications, the raceway may be formed of plastic or PVC materials.
[0016] As an example, and not in any limiting sense, FIGS. 1-5 show various embodiments of a roof edge cable raceway 20 used to form an open channel structure along an edge of a roof of a structure in which a heating cable is housed. The heating cable transfers heat directly to a heat conductive portion of the roof edge cable raceway preventing ice build-up at the drip edge and the formation of ice dams on the roof edge. Heat from the cable is concentrated at the drip edge. The open channel structure allows ready replacement and inspection of the heating cable. The channel is defined by channel sides that preferably extend along the length of the channel and define an opening into the channel. The channel may extend along the entire length of the roof edge or a portion of the roof edge desired to be heating.
[0017] FIG. 1 shows a roof edge cable raceway 20 comprising an edge attachment 22 assembled with mechanical fasteners 24 to an overhanging drip edge 26 to form a channel 28 for housing a heating cable 30 . The channel 28 has a first side 32 positioned adjacent a roof edge 34 and a second channel side 36 spaced therefrom. Together, the channel sides 32 , 36 define an opening 38 for the channel 28 . The open channel 28 allows replacement and inspection of the heating cable 30 through the opening 38 from a position in front of the channel opening. As shown in FIG. 1 , the second channel side 36 may be formed by mounting the edge attachment 22 at a position sufficient to allow the cable 30 to be visible in the opening 38 of channel from a position in front of the channel while allowing the sides of the channel to be urged against the cable with a snug fit to removably secure the cable in the channel. The second channel side 36 may comprise a radiused outer edge 39 . The radiused outer edge provides additional resiliency to springably retain and/or removably secure the heating cable in the channel. The radiused outer edge also assists installation personnel in installing the heating cable in the channel. Although the radiused outer edge 39 is shown in FIG. 1 , the distal edge of the edge attachment may also be flat without a radius.
[0018] As described above, the edge attachment functions as a biasing member urging the heating cable upward in FIG. 1 toward the channel first side. However, this may be reversed and the channel first side may function as a biasing member urging the heating cable downward in FIG. 1 toward the edge attachment. In the alternative, the biasing member may be a separate resilient member that is inserted in the channel, for instance, below the cable to urge the cable upward in FIG. 1 toward the channel first side. The separate resilient member may comprise a wave form elongated member disposed in the channel adjacent one or both of the channel sides; a foam rubber material disposed in the channel adjacent one or both of the channel sides; rubber, silicone, or plastic inserts that extend along the channel sides and/or engage one or both of the channel sides; or rubber, silicone, or plastic inserts periodically spaced along the length of the channel sides, for instance, in openings in one or both of the channel sides. The biasing member may be made from a heat conductive material to maximize heat transfer from the cable to the adjacent roof structure. The drawings show a relatively simplified construction of the raceway, involving less components, where one or both of the channel sides is formed to be resiliently deflected or springably moved to allow the heating cable to be removably secured in the channel.
[0019] The first channel side (i.e., the channel side adjacent the roof edge) 32 has a roof engagement portion 40 extending therefrom adapted to overlie and be secured to a portion 42 of the roof of the structure adjacent the roof edge 32 . As shown in FIG. 1 , the roof engagement portion 40 may also extend beyond the roof edge to form the overhanging portion of the drip edge. While the roof engagement portion of FIG. 1 has an exposed lower part with shingles or shakes 43 covering an upper part of the roof engagement portion, additional row(s) of shingles or shakes may cover the lower exposed part of the roof engagement portion and may extend to or beyond the roof edge thereby covering a majority or all of the roof engagement portion, as may be desired depending upon the construction techniques used. A fascia mounting portion 44 may extend from the first channel side 32 in a direction generally transverse to the roof engagement portion 40 , and the edge attachment 22 forming the second channel side may be mounted thereto.
[0020] The overhanging style drip edge (or drip edge) may comprise a pre-existing installation on the edge of the roof of the structure, thus allowing one to secure the edge attachment to the overhanging drip edge to form the channel, for instance in a retrofitting type of application. In this regard, the edge attachment 22 may comprise a member with a generally L-shaped cross-section that is mounted below the overhanging drip edge with a space therebetween that forms the channel 28 . While FIG. 1 shows the use of mechanical fasteners 24 to secure the edge attachment to the facia board to form the channel, other methods may be used, including providing the facia mounting portion of the overhanging drip edge with a system of locking tabs that cooperate with the edge attachment to secure the edge attachment in the proper location to form a channel suitable for housing the heating cable.
[0021] Using an edge attachment comprising a member having a generally L-shaped cross-section allows flexibility for the scope of work to be performed by on-site metal fabricators. For instance, on-site metal fabricators may form the edge attachment and install the edge attachment on the existing structure to form the open channel at the necessary dimensions to snugly fit the heating cable in the channel, and then the heating cable may then be installed in the open channel. To assist in mounting the edge attachment at the required spacing so that the channel accommodates the heating cable with a snug fit, the generally “L”-shaped edge attachment 22 may have a removable, and/or detachable (i.e., “knock-out” style) tab 29 projecting from its corner. In the alternative, the heating cable may be positioned adjacent the roof edge and then the edge attachment installed with the cable in place. As another example, the edge attachment may be mounted to an preexisting F-style overhanging drip edge installed on the structure. In the alternative, on site-metal fabricators may install the F-style overhanging drip edge and then the edge attachment. In the alternative, on-site metal fabricators may bend sheets of flat or rolled flashing materials as necessary to form and then install an overhanging drip edge and edge attachment. Various other combinations and sequences are also possible depending upon whether the work involves new construction, or remodeling or retrofitting of an existing structure.
[0022] Generally, the drip edges, such a F-style overhanging drip edges, comprise aluminum materials, for instance, extruded aluminum materials. Flashing generally also comprises aluminum sheets or rolls of aluminum. By closely mounting the edge attachment to the overhanging drip edge, the edge attachment and/or overhanging drip edge may be resiliently deflected or springably moved slightly to allow the heating cable to be snugly fit therebetween. As discussed before, forming a radiused outer edge 39 on the edge attachment provides additional resiliency for snugly retaining and/ore removably securing the heating cable in the channel. Additionally, when replacement of the cable is needed, the cable may be removed by pushing the channel sides to an apart position an amount sufficient to release the cable from the channel through the opening without mechanical deformation of the edge attachment or drip edge. A new heating cable may be then be readily installed using the existing raceway by moving the channel sides to an apart position to allow the new heating cable to inserted through the opening into the channel. Alternatively, mechanical fasteners holding the edge attachment in place may be removed (or loosened if the edge attachment is provided with elongated or “peanut-shaped” holes) thereby allowing the heating cable to be removed. A new heating cable may then be installed in the channel using one of the aforementioned methods.
[0023] The tight contact between the heating cable and the channel sides allows heat transfer through the heat conductive materials (i.e., aluminum) from the cable to a heat conductive portion of the roof edge cable raceway to a portion of the roof adjacent the drip edge, thus enabling the drip edge to be heated sufficiently to prevent ice formation at the edge of the roof of the structure. However, it is not necessary that the edge attachment be formed from a heat conductive material. Rather, the roof engagement portion and the channel first side may be made from a heat conductive material to allow heat transfer from the heating cable to the underside of the roofing materials for heating at the roof edge, and the edge attachment as well as the fascia engagement portion may be made from a different material.
[0024] FIG. 2 shows an alternate embodiment of a roof edge cable raceway having the same basic arrangement of that of FIG. 1 . In that regard, elements appearing in FIG. 2 that are related to those of FIG. 1 will be indicated with a (′). As with the embodiment of FIG. 1 , the edge attachment 22 ′ is assembled with mechanical fasteners 24 ′ to the fascia mounting portion 44 ′ of the overhanging drip edge 26 ′ to form the channel structure 28 ′ for springably retaining and/or removably securing the heating cable 30 ′, and the channel has a first side 32 ′ positioned adjacent the roof edge 34 ′ and a second side 36 ′ spaced therefrom defined by the mounted position of the edge attachment 22 ′. The second channel side 36 ′ may have a radiused outer edge 39 ′. Together the first and second sides 32 ′, 36 ′ define an opening for the channel. As with the embodiment of FIG. 1 , the channel first side 32 ′ has a roof engagement portion 40 ′ extending therefrom up the roof 42 ′ and beyond the roof edge 34 ′ to form the overhanging portion of the drip edge. Also as with the embodiment of FIG. 1 , shingles or shakes 43 ′ do not extend to the roof edge and a lower part of the roof engagement portion is exposed. Also, as with the embodiment of FIG. 1 , a fascia mounting portion 44 ′ may extend from the channel first side in a direction generally transverse to the roof engagement portion with the edge attachment 22 ′ forming the second channel side may be mounted thereto.
[0025] However, in the embodiment of FIG. 2 , a spacer 45 is integrally formed on the edge attachment 22 ′ to assist in locating the edge attachment at the proper spacing to form the channel opening 38 ′ to accommodate the heating cable, rather than the tab of FIG. 1 . Although not shown in the drawings, the generally “L”-shaped edge attachment of FIG. 1 may be similarly configured with an integrally formed spacer. Also, in the embodiment of FIG. 2 , the roof engagement portion 40 ′ is provided with a second channel 46 having an opening 48 at an upper portion 50 of the roof engagement portion. The opening 46 of the channel 48 may be formed by overlapping the upper portion 50 of the roof engagement portion 40 ′. An additional section of flashing material 52 may interlock with the upper portion 50 in the second channel 46 and may extend under the roofing materials 43 ′ (i.e., shingles, shakes, etc.) (not shown) a further distance up the roof 42 ′ from the edge 34 ′ of the roof of the structure. The second open channel 46 a houses a second heating cable 54 to increase the area of snow and ice that may be melted at the edge of the roof of the structure. Channel sides 56 , 58 define the second channel opening 48 , and at least one of the sides 56 , 58 of the second channel is sufficiently resilient to allow the heating cable 54 to be inserted through the opening into the second channel 46 in manner to allow the heating cable to be secured in the second channel with the heating cable being visible through the opening from a position in front of the opening of the second channel. For instance, as shown in FIG. 2 , the second channel first side 56 may have a relatively large radiused edge 59 to assist in providing added resiliency for the second channel first side to springably retain and/or removably secure the second heating cable 54 in the second heating channel. This radius feature may be reversed and provided on the second channel second side. Although FIG. 2 shows the added flashing 52 interlocking with the roof engagement portion 40 ′, it should be appreciated that the second channel 46 may be monolithically formed with the roof engagement portion of the overhanging drip edge and/or monolithically formed with the added flashing. Additionally, it should be appreciated that a biasing member may be provided in a manner as previously described in one or both of the first and second channels to assist in removably securing a cable therein.
[0026] FIG. 3 shows a roof edge cable raceway 60 with a monolithically formed channel 62 that is pre-formed for a heating cable 64 . The channel 62 has a first side 66 positioned adjacent a roof edge 68 and a second side 70 spaced therefrom. Together the channel sides 66 , 70 define an opening 72 into the channel 62 , and one or more of the channel sides may be sufficiently resilient to be springably moved to allow insertion of the heating cable 64 through the opening 72 into the channel 68 in a manner to allow securing the heating cable in the channel with the heating cable being visible through the opening from a position in front of the opening. The resiliency of the channel sides also allows replacement of the heating cable without deformation of the channel. The channel second side 70 may have a relatively large radiused edge 73 to assist in providing added resiliency for the channel second side to springably retain and/or removably secure the second heating cable 54 in the second heating channel. It should be appreciated that a biasing member may be provided in a manner as previously described in the channel to assist in removably securing a cable therein. The roof edge cable raceway 60 may comprise a roof engagement portion 74 that is adapted to overlie and be secured to a portion 76 of a roof of the structure on the channel first side, and a facia engagement portion 78 extending from the channel second side. The roof engagement portion may also extend beyond the roof edge 68 to form an overhanging roof edge. Preferably, the roof engagement portion 74 , the fascia engagement portion 78 , and the channel sides 66 , 70 are monolithically formed. In the alternative, the roof engagement portion and the channel first side may be made from a heat conductive material to allow heat transfer from the heating cable to the underside of the roofing materials 79 for heating at the roof edge, and the fascia engagement portion may be made from a different material. The embodiment of FIG. 3 may also be provided with a second channel (not shown) on the roof engagement portion similar in arrangement to that of FIG. 2 or a second channel monolithically formed with the roof engagement portion in the manner mentioned previously. Also, the embodiment of the roof edge cable raceway of FIG. 3 may be extruded as a monolithic member or may be formed on-site by metal fabricators bending flashing as needed into the form as shown FIG. 3 in the manner mentioned previously.
[0027] FIG. 4 shows an alternate embodiment of a roof edge cable raceway 80 comprising a open J-style channel. In the embodiment shown in FIG. 4 , a channel 82 is formed monolithically with a first side 84 of the channel adjacent a roof edge 86 and an opposite, second side 88 of the channel having a facia engagement portion 90 extending therefrom. Together, the channel sides 84 , 88 define an opening 92 extending along the length of the channel 82 . The channel first side 84 may engage roofing materials 94 , for instance, a metal roof. As described previously, one or more of the channel sides 84 , 88 may be sufficiently resilient to be springably moved to allow insertion of a heating cable 96 into the channel 82 through the opening 92 , while retaining the heating cable in the channel with a snug fit sufficient to allow heat from the cable to transfer to the channel and roof to prevent the formation of an ice dam. The channel second side may be provided with a large radiused outer edge 97 to assist in providing added resiliency for the channel second side to springably retain the heating cable 96 in the channel. The J-style open channel also allows the heating cable to be removably secured in the channel thereby allowing inspection and/or replacement at a later date as needed. It should be appreciated that a biasing member may be provided in a manner as previously described in the channel to assist in releasably securing a cable therein. As shown in FIG. 4 , the channel and fascia engagement portion are monolithically formed. However, it should be appreciated that the first channel side may be made from a heat conductive material to allow heat transfer to the roofing materials with the second channel side and/or fascia engagement portion made from a different material. Also, the embodiment of the roof edge cable raceway of FIG. 4 may be extruded as a monolithic member or may be formed on-site by metal fabricators bending flashing as needed into the form as shown in FIG. 4 . The roof edge raceway of FIG. 4 may be secured to the structure being using mechanical fasteners 98 at the fascia engagement portion 90 .
[0028] FIG. 5 shows an alternate embodiment of a roof edge cable raceway 100 wherein an edge attachment 102 is assembled with existing facia flashing 104 provided on a structure in a manner to form a channel 106 at an edge 107 of the roof of the structure for accommodating a heating cable 108 . As with embodiment of FIG. 2 , the edge attachment 102 of FIG. 5 may be provided with a spacer 109 to assist in locating the edge attachment at a spacing corresponding to the size of the heating cable. As shown in FIG. 5 , the fascia flashing 104 comprises a generally “L”-shaped member with a roof engagement portion 110 . The edge attachment 102 may also comprise a member having a generally L-shaped cross-section that may be secured to the structure and/or fascia flashing 104 with mechanical fasteners 112 . In the alternative, the fascia flashing and edge attachment may have a system of cooperating tabs and notches to allow the edge attachment to be positioned on the fascia flashing in a manner to create a channel sufficient to house the heating cable in a manner as described previously. As shown in FIG. 5 , the roof engagement portion 110 of the existing fascia flashing 104 forms a channel first side 114 , and the mounted position of the edge attachment defines a channel second side 116 . Together, the channel sides define an opening 118 for the channel 106 . The first channel side 114 may engage roofing materials 120 , for instance, a metal roof. At least one of the sides of the channel, for instance, the side of the channel formed by the edge attachment, may be sufficiently resilient to allow it to be springably moved to allow insertion of the heating cable in the channel in a manner to allow securing the heating cable in the channel with the heating cable visible from the opening. As shown in FIG. 5 , the channel second side may be provided with a large radius edge 119 to assist in providing added resiliency for the second side in snugly retaining the heating cable in the channel. The spacer 109 assists in setting the spacing to allow the heating cable to be snugly fit in the channel. The open channel of FIG. 5 also allows the heating cable to be inspected and/or replaced at a later date as needed, using one or more of the methods discussed above. Again, a snug fit ensures maximum heat transfer to the flashing and the roof structure to provide adequate melting at the roof edge. However, it should be appreciated that a biasing member may be provided in a manner as previously described in the channels to assist in releasably securing a cable therein. In the embodiment of FIG. 5 , the engagement portion 110 of the fascia flashing may be made from a heat conductive material and the edge attachment may be made from a different material.
[0029] FIG. 5 also shows a cover 130 that may be provided to cover the opening of the channel and also a biasing member 132 to urge the heat cable upward in the channel. The cover 130 and biasing member 132 shown in FIG. 5 may be added to any of the channels of the preceding Figures. After the heating cable is installed, the cover 130 may be fitted into the channel so the biasing member 132 fits under the cable and pushes the cable against the roof engagement portion. Preferably, the biasing member provides a tight fit for the cable against the roof engagement portion thereby maximizing heat transfer to the roof engagement portion and drip edge. Preferably, the cover 130 and biasing member 132 are made from a heat conductive material so as to maximize heat transfer to the roof engagement portion and drip edge and to reduce the effects of air being trapped between the cable and the roof engagement portion and drip edge that may otherwise reduce the rate of heat transfer.
[0030] FIG. 6 shows a schematic drawing of roof edge cable raceway 200 with an open channel structure 202 with a heating cable 204 disposed therein and channel sides 206 , 208 springably urged against the cable 204 to removably secure the cable in the channel.
[0031] FIG. 7 shows a corrugated roof 250 with a raceway 252 formed on its edge for housing a heating cable 254 . In the embodiment of FIG. 7 , corrugated roofing materials 256 that have curved features that match the corrugated roof 250 of the structure are secured to the structure below the edge of the existing corrugated roof with a space 258 sufficient in dimension to house the heating cable 254 therebetween.
[0032] Each of the heating cables described herein may be used in connection with a roof clamp 300 in a system shown schematically in FIG. 8 . Some roofs 302 have raised metal seams 304 that require protection from water leaking into the seam and penetrating the structure. Oftentimes, a heating cable 306 is extended from the drip edge up to a point on the roof past the interior wall to provide a drain path for melted snow or ice. For instance, a heating cable may extend around a fireplace or in the areas where different peaks of a roof converge. On raised seam metal roofs as shown in FIG. 8 , the clamp 300 may be secured to the roof with mechanical fasteners 308 . On conventional shingle or shake roofs, the clamps may be adhered to the roof with glue. A loop 310 is secured to the clamp with a mechanical fastener 312 with the heating cable 306 passing through the opening of the loop. The roof edge cable raceway and heating cable described herein may be used in connection with one or more of heating cable clamps 300 in the illustrative example shown in FIG. 8 . Accordingly, a portion of the heating cable may exit the roof edge cable raceway channel through the opening and extend up the roof to the clamp before returning down the roof to the roof edge and back into the roof edge cable raceway channel through the opening. Thus, it is not necessary that the entire heating cable be housed in the roof edge cable raceway channel.
[0033] FIG. 9 shows alternate embodiments of radius styles that may be provided on one or more of the sides of the channel for added resiliency to springably retain and/or removably secure the heating cable in the channel. The radius or hem style may also be provided on the edge of any of the edge attachments, fascia mounting portions, or roof engagement portions. For instance, the edge attachment comprising a generally “L”-shaped cross section may have a distal edge folded back onto itself with a radius in one of the exemplary styles 350 , 352 , 354 , 356 , 358 thereby forming a channel second side with added resiliency. As mentioned previously, providing one or more channel sides with a radiused edge facilitates installation, although one or more of the channel side may be flat. The distal end of the fascia mounting portion may also have a radius edge in one of the exemplary styles 350 , 352 , 354 , 356 , 358 to direct drainage away from the structure.
[0034] While specific embodiments have been described in detail in the foregoing detailed description and illustrated in the accompanying drawings, those with ordinary skill in the art will appreciate that various modifications and alternatives to those details could be developed in light of the overall teachings of the disclosure. Accordingly, the particular arrangements disclosed were meant to be illustrative only and not limited as to the scope of the invention which is to be given the full breadth of the appended claims and any equivalents thereof.
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A raceway extends along an edge of roof of a structure and is adapted to house a cable, such as an industry standard ice and snow melt heating cable designed, Listed and approved for the purpose. An open side of the raceway exposes the cable and allows for the insertion, replacement and inspection of the cable per industry practice. A side of the raceway may have a radiused edge providing added resiliency to springably retain and/or removably secure the cable in raceway. In the case of a heating cable, heat is transferred to the surrounding structure, and may be concentrated at the drip edge to maximize ice melt efficiency. Methods of installation of the raceway are applicable to new construction and retrofitting existing structures, including drainage systems, bridge structures and other outdoor enclosures, and may be used with many types of roofing materials including asphalt, wood and metal.
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FIELD
The present invention relates to a method of difference sensing through optical coherent change detection.
BACKGROUND
Difference imaging, in its simplest form, is carried out by talking two separate images of the same object or scene with each image being separated by a certain duration of time (the reference and test images). When the two images or brought into spatial alignment, and the values of the individual pixels of one image is computationally compared with the other image (usually by subtraction), the result is a “difference image” where the pixel values quantify (and spatially map) the magnitude of change that has occurred in the scene during the interval between the two samples.
SUMMARY
According there is provided a method of difference sensing. A first step involves producing a reference image using temporal averaging and spatial averaging. A second step involves producing a test image. A third step involves computationally comparing the reference image with the test image to arrive at a resulting difference image. The temporal averaging and spatial averaging effectively isolates in the difference image coherent changes imbeded in a complex and rapidly changing environment from transient changes inherent to the complex and rapidly changing environment.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other features of the invention will become more apparent from the following description in which reference is made to the appended drawings, the drawings are for the purpose of illustration only and are not intended to in any way limit the scope of the invention to the particular embodiment or embodiments shown, wherein:
FIG. 1 labelled as PRIOR ART is a time line relating to processes in time leading to creation of difference images.
FIG. 2 is a time line relating to processes in time leading to creation of an optical coherent change detection image.
FIG. 3 is a time sequence diagram regarding producing an optical coherent change detection image through subtraction of stationary background objects in a video sequence.
FIG. 4 is a time sequence diagram regarding using an optical coherent change detection image for the purpose of locating snipers.
FIG. 5 is a time sequence diagram regarding combining optical coherent change detection image processing with real-time polarization difference imaging.
DETAILED DESCRIPTION
Difference imaging, in its simplest form, is carried out by taking two separate images of the same object or scene with each image being separated by a certain duration of time (the reference and test images). When the two images or brought into spatial alignment, and the values of the individual pixels of one image are subtracted from the other image (or otherwise computationally compared with the other image), the result is a “difference image” where the pixel values quantify (and spatially map) the magnitude of change that has occurred in the scene during the interval between the two samples. FIG. 1 illustrates the relationship of various processes in time, which leads to the creation of typical different images. Different images can be produced using any form of imaging technology (for example, either chemical or digital photographic methods), therefore this figure is meant only to illustrate the salient features or processes underlying the creation of any typical or traditional difference images. Object 2 represents the flow of time, from arbitrary time T (the beginning of the difference imaging process) to time T+3 (the production of the final difference image). Object 4 represents the first image taken at time T. this is a completely exposed image covering a specific field of view. At time T+1 a second such image of the same field of view is taken (object 6 ). At time T+2, images 1 and 2 are spatially aligned, and a difference operation is applied (such as subtracting or ratioing the intensity value at one spatial location in image 1 from the corresponding spatial location in image 2 ). The result of this operation leads to the creation of a difference image (object 10 at time T+3) which highlights spatial variations in pixel intensity between the two initial images (objects 4 and 6 ) over time. The rate at which future reference frames are subsequently generated is dependent on the extent and rate of average change in the environment.
While difference imaging are extremely sensitive for detecting even the smallest changes which have occurred over time, this same sensitivity results in significant signal noise due to also highlighting random variations. At present, the utility of this technique is therefore limited when dealing with complex or natural settings, due to the presence of random temporal variations within the scenes. For example, in an image taken in a setting with grass and trees being gently blown by wind, complex and subtle variations in the positioning of leaves or blades of grass will result in the generation of a large random signal in the difference image. Likewise, the appearance of any transient object in either of the two images will result in a large difference image signal. Under these conditions, areas with changing pedestrian or vehicular traffic effectively render the technique of difference imaging useless for security applications.
It is to be noted that while the prior art speaks to polarization difference imaging (PDI), the present application speaks to polarization difference sensing (PDS). The technology that will be hereinafter described can be used in a variety of other applications such as RADAR and LIDAR. For the purpose of this discussion, PDI is considered to be a subset of PDS, which results in the creation of visual images.
In the present patent, we describe a concept and technique of difference imaging created through a process, which we have named Optical Coherent Change Detection (OCCD). While the present patent focuses on the utility of this new technique using visible, near infrared or ultraviolet wavelengths of light, this process may be applied to any wavelength in the electromagnetic spectrum, and can be carried out by utilizing either reflected, emitted or transmitted stimuli.
In its simplest form, OCCD utilizes temporal averaging of the imaging input to create both the reference and test images used to produce the final difference image. Temporal averaging of an image can be carried out by a number of methods. For example, one may decrease the amount of light falling on the sensor during a given period of time by inserting an optical component such as a neutral density filter in the stimulus pathway. By limiting the intensity of the input, the time required to gain adequate exposure required for image formation is increased. A second approach is to increase the rate at which data is read off of digital imaging chips (so a full exposure time is never achieved), and then to digitally combine these pixel values in such a way that they come to a normal exposure level.
Both of the above techniques result in what has traditionally been known as a “time-lapse photograph”. Time-lapse photographs have a unique characteristic in that any temporal variation or movement (over a time scale significantly shorter than the exposure time) is effectively averaged out. The resulting image is a temporal average of spatial variability within the image. With appropriately chosen exposure times, pedestrian and vehicular traffic, as well as the natural movement of leaves, grasses and their resultant shadows effectively vanish from the image. As a result, only significant changes that have occurred in the environment during the interval between the reference and test images are highlighted in the difference images. These changes can be detected in the background even through intervening traffic. Consequently, OCCD allows for the rapid video detection, spatial localization and identification of any object (such as an explosive device) dropped in a complex and constantly changing security environment.
FIG. 2 illustrates the underlying processes mediating the creation of an Optical Coherent Change Detection (OCCD) image. There are two operationally different (yet conceptually identical) methods for producing an OCCD image. First, a series of underexposed images of the same scene are collected (object 12 ), they are spatially aligned, and their corresponding pixel values are summed (object 14 ) to create a temporal average (“time-lapse”) of pixel intensity over space (object 16 ). After an interval of time, a second series of images (object 18 ) are collected, and a summed (object 20 ) to create a second “time-lapse” image (object 22 ). The first image (object 16 ) is used as a reference image (as designated by the capital letter R), and along with the second image (object 22 : the test image “T”), are processed to create a difference image (object 24 ) which highlights coherent changes in the scene which have occurred during the intervening time between the reference and test images. A second method for obtaining the reference and test images required to calculate an OCCD image is characterized by decreasing the amount of light falling on the detector (such as through the use of neutral density filters), and then allowing for sufficient time to form an adequately exposed image at the level of the detector. This process is repeated again later in time to form the test image, and is processed as outlined above to create the final OCCD image.
OCCD has applications in areas as diverse as security and military, medical and dental imaging, and engineering or structural assessment. Each field of application will determine both the time of exposure for both the reference and test images, as well as determining the most effective time interval required between the two images used to create the difference image. For example, in a complex and changing environment such as the subway station, difference images computed from reference and test images taken with a 30 second interval would guarantee prompt detection and a rapid response to parcels dropped in the environment. In the case of an OCCD surveillance system being used to secure a shipping yard or warehouse, an interval of five minutes between the reference and test images would be sufficient. In medical applications (such as x-rays), the interval between successive reference and test images could be more than a year. The longer the interval between the reference and test image, the more critical it is to obtain proper spatial registration between these two images used to create the difference image.
Our underlying OCCD process can be applied in a variety of unique ways that would have been impossible with earlier difference imaging techniques. For example, in FIG. 3 , a “time-lapse” reference image (object 29 ) can be created (as outlined in FIG. 2 ) to which a sequence of video frames (object 31 ) can be compared (object 30 ) to create a temporally succinct OCCD image. As a result, all stationery background objects in the video sequence will be subtracted from each individual frame (such as object 32 ), effectively isolating only moving and significantly changeable aspects contained within the otherwise potentially complex and cluttered video stream.
The ability to localize and identify significant changes in a complex and variable environment can be greatly enhanced through multi-sensor fusion. For example, when combined with acoustic signal processing techniques, OCCD can be integrated into it an efficient system for detecting and spatially localizing the presence of a sniper or enemy fire in a complex combat or urban setting. For example, FIG. 4 illustrates that if a microphone is used to detect the occurrence of gunfire (such as a sniper), the recorded gunfire (object 48 ) will be displaced in time (object 50 ) by a period of time dependent on the distance to the sniper and the speed of sound. As such, the video frame containing the image of the sniper and the muzzle blast (object 52 ) will occur earlier on the video recording (object 46 ). To detect the exact spatial location and time of the sniper fire a continuous series of reference frames (e.g. boxes Rt 1 —Rt 4 ) are computed and the last reference frame computed before the recorded gunfire (object 40 ) or earlier are used to compute a frame by frame series of difference images. When the video frame containing the muzzle flash is encountered (object 52 ) and included in the calculation of the difference image (object 42 ), the precise temporal and spatial location of the sniper can be isolated in the resultant OCCD image (object 44 ) regardless of the complexity of the surroundings.
Regions where changes have occurred in OCCD images typically give rise to very large changes in the pixel values. For example, the sudden appearance of an object may result in a maximum local pixel value (e.g. an 8-bit pixel value of 255). Since such extreme pixel values are rarely seen in a correctly exposed image, a spatial clustering of such values can be used to (A) trigger an alarm to draw the attention of the system operator to the occurrence of a significant change, or (B) be used to compute a spatial reference within a coordinate system that can be used to automatically drive other security cameras to focus in on the potentially dangerous object in the security setting.
The OCCD process can be further enhanced through integration with the real-time polarization difference imaging (PDI) technique. In FIG. 5 , a series of frames (object 54 ) are imaged utilizing optics which isolate the horizontally polarized components (indicated by Hpol) within the image frame. Likewise, a series of frames (object 58 ) are imaged utilizing optics which isolate the vertically polarized components (indicated by Vpol) within the image frame. Both the Hpol and the Vpol underexposed frames are summed (object 56 and object 60 respectively), and are used to compute a PDI image (object 62 ) which subsequently becomes the reference image (object 64 ) to be used in the computation (object 66 ) of the OCCD image (object 68 ). In this case, the test image (object 72 ) is a frame from a real-time PDI video series (object 70 ).
Within the security context, a strong polarmetric signature also helps to reduce false alarms by highlighting the presence of artificial structures in a natural environment. In addition, periodic computing of an OCCD difference image will enable the operator of such a security system to detect the approach of an assailant regardless of how well they are camouflaged to blend into their surroundings, or how slow and steady their approach may be. While normal security video systems cannot easily distinguish between a camouflaged intruder and natural foliage, a security surveillance system based on our OCCD technology will easily detect such an intruder.
When combined with Polarization Difference Imaging (PDI) techniques, OCCD becomes particularly effective at detecting and documenting structural changes (such as component deformation) caused by excessive compressive, torsional or shearing forces even when such the deformations are so subtle as to not be visually detectable, or detectable by traditional video survey techniques. For example, during underwater inspection of offshore oil well structures, variations in the presence of illuminated particles in the two frames taken during a traditional difference image would create a tremendous amount of image noise. With our paired PDI/OCCD system, not only are variations of particle distributions averaged out, but also the PDI process greatly enhances imaging ability through turbid waters. Further applications of such an imaging system include the detection of icing conditions in aviation. For example, during icing conditions the polarmetric signature of light reflected off in metal wing or structure undergoes a significant change, as the ice creates an optically scattering coating (thereby disrupting the polarization signature). PDI video, in combination with OCCD imaging techniques, can be utilized to create a system for determining the spatial location, rate and extent of ice formation on aircraft or other structures. Through the use of a time series of PDI/OCCD images taken of flight surfaces of an aircraft, the extent and rate of ice formation, as well as the efficiency of de-icing techniques can be readily determined either on the ground or during flight.
When combined with acoustic signal processing techniques, OCCD can be integrated into an efficient system for detecting and spatially localizing the presence of a sniper in a complex combat or urban setting. In this case, a 360° OCCD reference frame is computed and stored in such a way as to maintain a complete temporal record over a predefined period. When the presence of a gunshot is detected utilizing the acoustic signal processor (at time=T+0), a series of individual video frames (taken from seconds before until after the recorded gunshot) are sequentially subtracted from the last OCCD reference image. As a result, the appearance of the muzzle flash, smoke, and movement of the sniper can be rapidly spatially localized.
In this patent document, the word “comprising” is used in its non-limiting sense to mean that items following the word are included, but items not specifically mentioned are not excluded. A reference to an element by the indefinite article “a” does not exclude the possibility that more than one of the element is present, unless the context clearly requires that there be one and only one of the elements.
It will be apparent to one skilled in the art that modifications may be made to the illustrated embodiment without departing from the spirit and scope of the invention as hereinafter defined in the claims.
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A method of difference sensing. A first step involves producing a reference image using temporal averaging and spatial averaging. A second step involves producing a test image. A third step involves computationally comparing the reference image with the test image to arrive at a resulting difference image. The temporal averaging and spatial averaging effectively isolates in the difference image coherent changes imbeded in a complex and rapidly changing environment from transient changes inherent to the complex and rapidly changing environment.
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FIELD OF THE INVENTION
This invention relates to a process for controlling various characteristics of sheet material manufactured on papermaking equipment by filtering data gathered about characteristics and controlling the characteristic based on the filtered data.
BACKGROUND OF THE INVENTION
In the production of sheet materials such as paper, it is necessary to control certain properties of the sheet material. Properties such as basis weight, moisture and caliper will vary along the machine direction which is the path in which the sheet material is moved during production, and these properties will also vary in the cross machine direction which is perpendicular to the machine direction.
In order to control the paper parameters, the sheet material being manufactured must be accurately measured and data concerning the measured parameters used to alter the process to maintain the parameters within desired limits. Collection of samples from scanning measurement systems which traverse the sheet perpendicular to its travel result in the establishment of a high resolution profile. These high resolution profiles are transformed by filtering into a control profile that is used to control actuators that adjust the parameters of the sheet material in a feedback loop.
For example, in order to control sheet thickness in the cross machine direction, calendering machines are used comprising a series of rolls arranged in parallel, one above the other, in a stack. The sheet material is trained through the stack to pass through the nip areas between adjacent rolls. Calender profile actuators are used to adjust the thickness parameter of the sheet material. The profile actuators comprise a plurality of devices that operate to heat or cool the rolls differentially along their length. Each heating or cooling device controls a zone or "slice" of a roll. For example, when a slice of the roll is heated, the diameter of the roll increases and the caliper of the sheet material in that slice is decreased. The caliper of the sheet material downstream of the rolls is monitored by a scanning sensor that collects a plurality of datapoints in the cross machine direction. These datapoints define a high resolution or mini-slice profile of the thickness of the paper sheet. The profile is provided to a profile analyser as a signal indicative of the caliper thickness. The signal is transformed by the profile analyser into a low resolution control profile. The control profile is divided into a plurality of control slices, each control slice being used to adjust a particular actuator to correct for any variation in caliper thickness from a desired profile across the sheet material. Each control slice in the low resolution profile is derived from plurality of mini-slices in the high resolution profile. In other words, each datapoint in the control profile is derived from a plurality of datapoints in the high resolution profile.
Other sheet parameters are controlled in the same general manner. A high resolution profile of a parameter to be controlled is acquired by sensing equipment. The high resolution profile is then transformed into a low resolution control profile that provides control signals to actuators for adjusting the parameter being monitored.
In any control system that works along the foregoing lines, it is important that when the high resolution profile is transformed into the low resolution control profile the datapoints or signal be filtered to prevent aliasing in the control profile. The high resolution profile contains many different frequency components and when the high resolution profile is transformed to a low resolution profile that is aligned to the physical actuator dimensions, the higher frequency components can lead to a distortion of the control profile. Therefore, aliasing is the creation of sampling induced fictitious components that are added to signal content. As a result, control actions can be made on "phantom" variation which does not exist in the original high resolution profile.
SUMMARY OF THE INVENTION
Applicant has developed a process for filtering and decimating a high resolution profile to produce a low resolution control profile that is an accurate representation of the high resolution profile.
Accordingly, the present invention provides a process for transforming a plurality of data points, n, defining a high resolution profile for a parameter of a sheet material being manufactured into a low resolution profile for control of the parameter comprising the steps of:
filtering the data points of the high resolution profile using an anti-aliasing filter function to create an intermediate profile; and
reducing the number of datapoints of the intermediate profile by an integer factor to create the low resolution profile to be used to control the parameter.
In a further aspect the present invention provides a process for controlling a parameter of a sheet material which is being manufactured comprising the steps of:
(a) causing the sheet material to travel;
(b) moving a scanning means across the sheet;
(c) measuring a parameter of the sheet with the scanning means in a plurality of zones, n, which are disposed side-by-side across the sheet to produce a plurality of data points that define a high resolution or mini-slice profile;
(d) filtering the data points using an anti-aliasing filter function to produce an intermediate profile;
(e) reducing the number of data points by an integer factor to create a low resolution or control profile; and
(f) controlling the parameter based upon the low resolution profile.
The processes of the present invention rely on an anti-aliasing filter to remove high frequency components in the high resolution profile. Then, single or multi-stage decimation is performed to construct a profile for cross machine direction control of a sheet parameter.
The processes of the present invention provide a faithful reproduction of the appropriate frequency components in the high resolution profile into the low resolution control profile thereby permitting improved control performance of the parameter actuators.
BRIEF DESCRIPTION OF THE DRAWINGS
Aspects of the present invention are illustrated, merely by way of example, in the accompanying drawings in which:
FIG. 1 is a generally schematic view of an example of a sheetmaking machine;
FIG. 2 is a block diagram showing the process of the present invention involving applying an anti-aliasing filter to the minislice profile and then decimating the resulting intermediate profile to produce a control profile;
FIG. 3 is a block diagram of the anti-aliasing filter flow according to the present invention;
FIGS. 4a and 4b are graphs showing the effect of Hamming function window order N on the transition band and the attenuation, respectively;
FIGS. 5a and 5b are graphs showing the magnitude responses of a Hamming filter and an ideal low pass filter, respectively,
FIG. 6 is a graph showing the magnitude response of an anti-aliasing filter designed using the Hamming filter and ideal low pass filter of FIGS. 5a and 5b;
FIGS. 7a, 7b and 7c are impulse response graphs showing Hamming coefficients, ideal low pass filter coefficients and the resulting anti-aliasing filter coefficients, respectively, for a first example of designing a filter according to the present invention;
FIGS. 8a, 8b and 8c are impulse response graphs showing calculated Hamming coefficients, ideal low pass filter coefficients and the resulting anti-aliasing filter coefficients, respectively, for a second example of designing a filter according to the present invention; and
FIGS. 9a and 9b are graphs showing the magnitude responses of anti-aliasing filters using the coefficients of FIGS. 7c and 8c, respectively.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1, there is shown a sheetmaking machine for producing continuous sheet material. In the illustrated embodiment, the sheet making machine includes a feed box 10 which discharges raw material, such as paper pulp, onto a supporting web 13 trained between rollers 14 and 15. Further, the sheetmaking machine includes processing stages, such as a steambox 20 and calendering device 21 which operate upon the raw material to produce a finished sheet 18 which is collected on reel 22.
In conventional sheetmaking practice, the processing stages along the machine of FIG. 1 each include actuators for controlling parameters of sheet 18. In the illustrated embodiment, for instance, feed box 10 includes independently adjustable actuators 23 which control the quantity of material fed onto web 13 at adjacent cross-directional locations referred to as "slices". Similarly, steambox 20 includes actuators that control the quality of steam applied to sheet 18 at various slice locations. Also, calendering stage 21 can include actuators for controlling the compressive pressure applied to sheet 18 at various slice locations. In the following discussion, the various actuators are referred to as profile actuators as they affect the cross-directional profile of the sheet material being produced.
To provide control information for operating the profile actuators on the sheetmaking machinery of FIG. 1 at least one scanning sensor 30 is mounted on the sheetmaking machine to measure a selected sheet property, such as caliper or basis weight, during production of the sheet material. In the illustrated embodiment, scanning sensor 30 is mounted on a supporting frame 31 that extends across the sheetmaking machine in the cross direction. Further, scanning sensor 30 is connected, as by line 32, to a profile analyzer 33 for providing the analyzer with signals indicative of the magnitude of the measured sheet parameter at various cross directional measurement or data points. The signals form the high resolution profile. Profile analyzer 33 transforms the high resolution or mini-slice profile into a low resolution control profile. Profile analyzer 33 is also connected to the profile actuators at the processing stages of the sheetmaking machine for providing control signals to the actuators based on the low resolution control profile. For example, line 35 carries control signals from the profile analyzer 33 to profile actuators 23 at feedbox 10.
The process of the present invention is directed to performing the transformation of the high resolution profile to the low resolution profile in such a manner as to provide a faithful reproduction of the appropriate frequency components in the high resolution profile into the low resolution control profile. FIG. 2 is a block diagram showing the steps of the process of the present invention. In the process of the present invention, the datapoints, n, of the high resolution mini-slice profile 40 are filtered at 42 using an anti-aliasing filter function to create an intermediate profile 43. Then, the number of datapoints of the intermediate profile are reduced by an integer factor M at 44 to create the low resolution profile 45 to be used to control the parameter. The decimation factor M is based on the number of profile actuators. The technique shown at 44 is known as decimation or downsampling of the intermediate profile.
In the process of the present invention, the anti-aliasing filter step 42 is needed to ensure that no high frequency components in the high resolution profile are mapped into the low resolution control profile as phantom low frequency components. Applicant has developed an anti-aliasing filter that is particularly effective in accomplishing this goal. FIG. 3 is a block diagram detailing the anti-aliasing filter flow of the present invention.
The anti-aliasing filter 49 is constructed using a Hamming filter function 50 and an ideal low pass filter function 52. In accordance with standard terminology, the Hamming filter function is also referred to as a "window" function or simply a "window".
As shown in FIG. 3, the anti-aliasing filter is designed by first selecting an order N for Hamming window 50. FIGS. 4a and 4b are graphs that can be used to aid in the choice of window order. The graphs provide the user with an idea of the effect of choosing different window orders as the window order sets the width of the resulting filter's transition band and the attenuation of the stopband. The stopband defines the region where unwanted components are significantly attenuated.
The Hamming window response is convolved with an ideal low pass filter response as shown in FIG. 3. The Hamming window coefficients are determined according to the following equation: ##EQU1## where N=the window order of the Hamming function.
The coefficients for the ideal low pass filter are determined by the equation: ##EQU2## where ω c is the cutoff frequency defined as the frequency where magnitude is attenuated by fifty per cent. The cutoff frequency is related to the number of minislices per control slice (effectively, the number of datapoints n in the high resolution profile per datapoint in the final low resolution control profile). To avoid all chance of aliasing the cutoff frequency can be made equal to: ##EQU3## where Δω is the transition band of the anti-aliasing filter.
Choosing the cutoff frequency in the above manner ensures that no aliasing will occur. However, the width of the transition band Δω corresponding to the window order chosen must be known to determine ω c . Several other possible approaches may be used to determine the cutoff frequency of the anti-aliasing filter. One possibility would involve keeping the window order maximized to its largest value as the transition band will be at its narrowest and constant. Then ω c can be easily evaluated as discussed above. Alternatively, the cutoff frequency ω c can be set equal to the ratio of minislices per control zone. The drawback of this approach is that the width of the transition band may become a significant factor in some situations. Even if the Hamming window order is forty, the transition band may be too wide and the anti-aliasing filter could potentially allow some aliasing to occur. Regardless of which approach is taken, the anti-aliasing filter of the present invention will perform much better than applying only a rectangular window directly to the high resolution profile as done in conventional transformation schemes.
The anti-aliasing filter 49 of the present invention is constructed using the Hamming window coefficients and the coefficients from the ideal low pass filter. The anti-aliasing filter function f(n) is determined according to the following formula:
f(n)=w(n)h(n)
Hence, the coefficients of the anti-aliasing function are determined by multiplying together the Hamming window coefficients and the ideal low pass filter coefficients that were determined as described above.
The design of the anti-aliasing filter is automatic once the window order N is chosen as the coefficients for the Hamming window are based on N and the coefficients for the ideal low pass filter are based on the window order N and the number of minislices per control slice. Generally, a large N is better but this may be limited by computation or computer memory.
By way of example, FIGS. 5a, 5b are graphs showing the response of a 20the order Hamming function and an ideal low pass filter. FIG. 6 is a graph of an anti-aliasing filter constructed according to the present invention by convolving the Hamming window response of FIG. 5a and the low pass filter response of FIG. 5b.
As shown in FIG. 2, the anti-aliasing filter of FIG. 6 is applied to the n datapoints of the high resolution profile 40 to produce an intermediate filtered profile 42 that is then decimated to produce a final low resolution control profile 45.
Following are two examples of the manner in which the coefficients for the anti-aliasing filters according to the present invention are calculated. In the examples, the filter length is the number of weights in a window and window order is one less than the filter length.
EXAMPLE 1
In the first example, a filter of length 6 with a cutoff frequency of 0.5π is devised.
Therefore, the Hamming filter coefficients are:
w(n)=0.08δ[n]+0.3979δ[n-1]+0.9121δ[n-2]+0.9121δ[n-3]+0.3979δ[n-4]+0.08δ[n-5]
The ideal low pass filter coefficients are:
h(n)=-0.09δ[n]+0.1501δ[n-1]+0.4502δ[n-2]+0.4502δ[n-3]+0.1501δ[n-4]-0.09δ[n-5]
The resulting anti-aliasing filter coefficients are:
f(n)=-0.0072δ[n]+0.0597δ[n-1]+0.4106δ[n-2]+0.4106δ[n-3]+0.0597δ[n-4]-00072δ[n-5]
FIGS. 7a, 7b and 7c show the impulse responses of the Hamming filter, the ideal low pass filter and the resulting anti-aliasing filter, respectively.
EXAMPLE 2
In the second example, a filter of length 9 with a cutoff frequency of 0.4π is devised.
Therefore, the Hamming filter coefficients are:
w(n)=0.08δ[n]+0.2147δ[n-1]+0.54δ[n-2]+0.8653δ[n-3]+δ[n-4]+0.8653[n-5]+0.54δ[n-6]+0.2147δ[n-7]+0.08δ[n-8]
The ideal low pass filter coefficients are: ##EQU4##
The resulting anti-aliasing filter coefficients are: ##EQU5##
FIGS. 8a, 8b and 8c show the impulse responses of the Hamming filter, the ideal low pass filter and the resulting anti-aliasing filter, respectively.
FIG. 9a and FIG. 9b show the magnitude response of the anti-aliasing filters shown in FIGS. 7c and 8c, respectively. The response for the filter of FIG. 7c has a cutoff frequency of 0.5π while the response for the filter of FIG. 8c has a cutoff frequency of 0.4π. It can be seen that in order to meet the design specification for the first filter, there is much more attenuation in the passband than there is for the second filter. In order to have less attenuation in the passband, a high order of filter is required.
Although the present invention has been described in some detail by way of example for purposes of clarity and understanding, it will be apparent that certain changes and modifications may be practised within the scope of the appended claims.
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A process for transforming a plurality of data points n defining a high resolution profile for a parameter of a sheet material being manufactured into a low resolution profile for control of the parameter is disclosed. The process involves filtering the data points of the high resolution profile using an anti-aliasing filter function to create an intermediate profile and reducing the number of datapoints of the intermediate profile by an integer factor to create the low resolution profile to be used to control the parameter.
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This Application is a Continuation (Con.) of application Ser. No. 10/128,936 U.S. Pat. No. 6,693,837, filed Apr. 23, 2002.
TECHNICAL FIELD
The present invention is directed to dynamic random access memory (“DRAM”) devices. More particularly, the present invention is directed to a system and method allowing DRAM devices to more efficiently exit from a self-refresh state so that the DRAM device can resume processing valid commands more quickly.
BACKGROUND OF THE INVENTION
Most computers and other digital systems have a system memory which often consists of dynamic random access memory (“DRAM”) devices. DRAM devices are fairly inexpensive because a DRAM memory cell needs relatively few components to store a data bit as compared with other types of memory cells. Generally a DRAM memory cell consists of a transistor/capacitor pair whereas, in a static random access device (SRAM), each memory cell comprises four or more transistors. Thus, DRAM memory cells have fewer components than SRAM memory cells. As a result, DRAM arrays occupy far less area on a semiconductor substrate compared to SRAM arrays of the same size. Thus, DRAM devices are far less expensive to produce than SRAM devices. A large system memory can be implemented using DRAM devices for relatively low cost, making DRAM devices a very popular choice in many devices requiring a large memory capacity.
On the other hand, while DRAM devices are less expensive to produce than SRAM devices, DRAM devices suffer from the disadvantage that their memory cells must be continually refreshed because of the inherently transitory nature of their storage technology. Over time, the voltage stored across the capacitor dissipates as a result of current leakage. To offset this problem, each memory cell regularly must be refreshed within a maximum refresh interval by determining whether a high or low voltage was stored across that capacitor, and recharging the capacitor to that voltage. The refresh process, which basically involves reading a memory cell through a sense amplifier to recharge the memory cell's capacitor, is well known in the art, and it is reasonably simple and quick.
Notwithstanding how quick the refresh process might be, however, having to continually refresh all the memory cells in a DRAM memory array impedes the intended function of the memory: reading and writing data in response to processor directives. Even though memory cells are refreshed an entire row at a time, memory banks may be thousands of rows deep, and each row must be refreshed many times per second. Collectively, thousands upon thousands of refresh operations are required every second to preserve the contents of the memory cells in a DRAM device—thousands of operations during which the DRAM device is precluded from performing desired read and write functions. Moreover, unless the memory array is equipped with a dual accessing mechanism, a row cache device, or a functionally similar means, the array can be neither read from nor written to during a refresh cycle without interrupting or destroying the cycle. If the central processing unit or other controller initiates a memory read or write operation during a refresh cycle, the processor or controller needs to wait for completion of that refresh cycle along with any corresponding wait states or delay intervals. Clearly, waiting for refresh procedures slows the operational throughput of the computing system.
FIG. 1 depicts a conventional DRAM device 100 . The DRAM device 100 is accessed through the address lines 110 , the data lines 112 , and a number of control lines 120 - 132 . These control lines include CKE (clock enable) 120 , CK* (clock signal—low) 122 , CK (clock signal) 124 , CS* (chip select—low enable) 126 , WE* (write select—low enable) 128 , CAS* (column address strobe—low enable) 130 , and RAS* (row address strobe—low enable). The address lines 110 , data lines 112 , and control lines 120 - 132 , enable the system to read and write data to the actual memory banks 150 , as well as control the refreshing of the DRAM device 100 .
The control logic 160 controls the read, write, and refresh operations of the DRAM device 100 . The control logic 160 directs the operations of the DRAM device 100 as a function of the signals received at the control lines 120 - 132 . Numerous other elements of the DRAM device 100 are depicted in FIG. 1 , but the refresh counter 170 and the self-refresh control logic 180 are particularly relevant to this discussion.
The refresh counter 170 is an integral component in refreshing the DRAM device 100 . The refresh counter 170 maintains a count corresponding to the row number in the memory banks 150 that was last refreshed or, if a row refresh is in progress, the number of the row currently being refreshed. Once a command is received to refresh a row, the refresh counter 170 is incremented by one, and the row of the memory banks 150 corresponding to the updated count stored in the refresh counter 170 is refreshed. The refresh counter 170 thereby tracks what row is next to be refreshed, controlling the sequencing of row refreshes.
Tracking the count maintained by the refresh counter 170 , the rows of the memory banks 150 can be refreshed in either burst refresh or distributed refresh. Using burst refresh, all the rows of the memory banks 150 are refreshed in immediate succession, one after the other, for as long as it takes to refresh every row of the device. Operationally, the refresh counter 170 is incremented, the row indicated by the refresh counter 170 is refreshed, and this process repeats until each row of the memory banks 150 has been refreshed. Once all the rows have been successively refreshed, the DRAM device 100 once more is available for read and write operations until the memory banks 150 of the DRAM device 100 must again all be refreshed.
In a distributed refresh, one row of the memory banks 150 is refreshed at a time, then the DRAM device 100 is made available for useful operations until the next individual row of the memory banks 150 needs to be refreshed. As the designation “distributed” implies, this type of refresh distributes the time required to refresh every row in the memory banks 150 over the entire maximum refresh interval, instead of ceasing all read and write operations for the relatively long interval required to refresh every row in the memory banks 150 as in a burst refresh. Specifically, for each refresh command received, the refresh counter 170 is incremented, the row corresponding to the number indicated by the refresh counter 170 is refreshed, then the DRAM device 100 is made available for read and write operations until the next refresh command is received. This process repeats continuously. In a typical DRAM, having 4,096 rows and a maximum refresh interval of 64 milliseconds in its operational mode, a command to refresh one row would have to be issued approximately every 15 to 16 microseconds.
In addition, in a typical DRAM device, there are also two different types of refresh modes: auto-refresh and self-refresh. The first type, auto-refresh, is the command given to initiate a single refresh command. Whether the system employs burst refresh or distributed refresh to refresh its memory devices, issuance of an auto-refresh command initiates one refresh cycle for the entire memory bank or for a single row, respectively. Auto-refresh is, therefore, the “standard” refresh command used to refresh memory devices during normal operation. An auto-refresh command is issued to the DRAM device 100 by driving the CKE 120 and WE* 128 control lines high, and driving the CS* 126 , RAS* 130 and CAS* 132 control lines low.
Auto-refresh operates synchronously with the system clock. With the CKE 120 and WE* 128 control lines driven high, and the CS* 126 , RAS* 130 and CAS* 132 control lines driven low, the rising edge of the next clock signal initiates an auto-refresh of the next row of the memory banks 150 . As is known in the art, the rising edge of the next clock signal is that point where the clock signals received at the CK* 122 and CK 124 control lines cross. As previously described, the refresh counter 170 is incremented to indicate the next row in the memory banks 150 that is being refreshed or is next to be refreshed. Between refreshes in a system employing a distributed refresh mode, or once all the rows have been refreshed in a system using a burst refresh mode, the signals applied to the control lines can be driven to the states signaling read, write, and other valid commands. An interval t rfc , the time indicated by the device specification, should be permitted after the issuance of the auto-refresh command and the issuance of the next command.
By contrast, issuance of a self-refresh command places a DRAM device 100 in a continual, indefinite refresh cycle to preserve the data stored in the DRAM device 100 . A self-refresh command typically is issued during a period when useful read and write requests will not be forthcoming, for example, when a user has placed the computing system into a sleep or standby mode. A self-refresh cycle typically employs a distributed refresh cycle internally.
During a self-refresh cycle, because the system will not be called upon to perform read or write commands, current and voltage switching in the DRAM device 100 is reduced. This relatively stable condition tends to ameliorate electrical and thermal effects which contribute to current leakage from the capacitors of the memory cells. As a result, while the memory cells still need to be refreshed to preserve the integrity of the data stored therein, the memory cells do not need to be refreshed as frequently as during an operational state. During self-refresh, the contents of the memory cells can be preserved by refreshing a row less frequently than every 15 milliseconds as required in this example DRAM device 100 . In self-refresh state, the rows might not need to be refreshed for a period up to twice as long, or perhaps slightly longer, than is permitted during an operational state.
A self-refresh command is triggered by driving the CS* 126 , RAS* 130 and the CAS* 132 control lines low, driving the WE* 128 control line high, and, this time, driving the CKE 120 control line low. This command causes the self-refresh control logic 180 to periodically and repeatedly refresh every one of its rows, and also places all data, address, and control lines into a “don't care” state, with the exception of the CKE 120 control line. The CKE 120 control line being driven high takes the other control lines out of the “don't care” state, and signals the end of the self-refresh state. At that point, after a waiting interval described below, the system can then access the DRAM device 100 for read and write operations and/or to control the refreshing of the DRAM device through auto-refresh commands.
Although a self-refresh state is very similar to a repeating series of auto-refresh states, there is a critical difference: while a DRAM device 100 in an auto-refresh state is refreshed synchronously with the system clock, in a self-refresh state, the DRAM device is refreshed asynchronously and independently of the system clock. During a self-refresh state, the refreshing of the rows of the memory banks is controlled by the DRAM device's own, on-board self-refresh control logic 180 . The on-board self-refresh control logic includes its own clocking system (not separately shown in FIG. 1 ) which pulses the self-refresh cycles, as described, at a less frequent rate than the system clock pulses operational commands.
During self-refresh, the memory banks 150 are refreshed according to the DRAM device's 100 own clock, asynchronously of the system clock during self-refresh. As a result, the system may issue a self-refresh exit command at any point during the self-refresh cycle of the DRAM device 100 , either while a row is being refreshed or during a wait state between row refreshes. Accordingly, from the time the self-refresh exit command is issued until the DRAM device is available to process commands, the system must allow a waiting interval to pass. Waiting for this interval to pass will allow for the completion of the self-refresh of a row, if one was in progress as the time the self-refresh exit command was issued. If a self-refresh cycle was not in progress, the self-refresh control logic 180 will halt the self-refresh process and wait to make sure that no new refresh cycle begins once the self-refresh exit command has been received.
This waiting interval is denominated as t xsr , to represent the time needed to “exit self-refresh.” In either case, the system will not have any indication of whether a row refresh was in progress at the time the self-refresh exit command was issued, and the system must allow the interval t xsr to pass before issuing other commands. The passage of the interval t xsr is purely time wasted if a row refresh was not in progress when the exit self-refresh command was issued. Nonetheless, it is a necessary precaution because the self-refresh process operates asynchronously and independently of the system clock. The interval t xsr typically is equal to the time required to refresh one row, denominated as t rfc , to represent the time to “refresh complete,” plus one additional clock cycle to allow for the asynchonicity between the phase of the DRAM device 100 self-refresh clock and the system clock. Typically, this interval is on the order of 60 to 70 nanoseconds.
Certainly, potentially having to waste time just in case a row self-refresh was in progress is a concern for its own sake. However, a larger concern is the effect the asynchronicity between the self-refresh cycle and the system clock might have on the integrity of data stored in the DRAM device 100 . There is a possibility that rows of memory cells in the DRAM device 100 may not be refreshed within the maximum refresh interval and the contents of the memory cells in these rows may become corrupted. As previously described, the relatively stable state of the DRAM device 100 in self-refresh mode reduces current leakage in the DRAM device 100 because no commands are being processed that might cause unpredictable voltage and current fluctuations. Consequently, the maximum refresh interval for a DRAM device 100 in self-refresh mode is longer than that for a DRAM device 100 in operational mode, and the interval between row refresh cycles is also longer. Potential problems arise upon the transition from the relatively stable, slower-refreshing self-refresh state to the more volatile operational state and from the cumulative effect of numerous transitions between self-refresh and operational states.
FIG. 2 illustrates these concerns. The chart 200 visually depicts the switching of a DRAM device over time in response to self-refresh exit commands. Specifically, the device state graph 210 shows how the DRAM device switches between the self-refresh mode 220 and the operational mode 230 in response to receipt of self-refresh and self-refresh exit commands as represented by the switching between low and high states of the CKE signal line as depicted by the CKE signal 240 . As previously described, it is assumed that this DRAM device refreshes a row once every 40 microseconds while in self-refresh mode, and once every 15 microseconds while in operational mode. It is also assumed that, just at or prior to time t=0, a row was refreshed during the self-refresh state, incrementing the row counter to indicate the next row must be refreshed in 40 microseconds.
Before the next row is refreshed, however, at approximately time t=35 microseconds, the system issues a self-refresh exit command as represented by the CKE signal 240 driving high at 250 . In response, the self-refresh mode 220 is exited as represented by the device state graph 210 exiting self-refresh and returning to operational status 230 at 260 . Because the system clock and the DRAM device's on-board self-refresh clock operate asynchronously of each other, the system had no indication that the DRAM device was about to execute a row refresh operation at time t=40 microseconds. As a result, the row refresh operation was not executed, and as the DRAM device resumes the more volatile operational state, current leakage could affect the voltages stored in the memory cells and thereby undermine the integrity of the data stored. If the DRAM device has been in self-refresh mode for at least the time required to complete one complete self-refresh of each row in the DRAM device, assuming the device has 4,096 rows and self-refreshes one row every 40 microseconds, the next row to be refreshed has not been refreshed in nearly 164 milliseconds; this period is more than two and one-half times the maximum refresh interval of the DRAM device in its operational state.
To compound the problem, just before that row was to be auto-refreshed 15 microseconds after the DRAM device returned to its operational state 230 , the CKE signal 240 transitions low at 270 to direct the DRAM device back into self-refresh mode 220 at 280 . Upon returning to self-refresh mode 220 , the self-refresh clock will become active to refresh the next row in 40 microseconds at approximately time t=90 microseconds. However, before that refresh occurs, once more the CKE signal 240 transition high at 290 , directing the DRAM device to exit self-refresh mode 220 once again and resume operational status 230 . Charge leakage continues, and the integrity of the data stored in the next row of the DRAM device to be refreshed—and the succeeding rows which also have not been refreshed for a growing interval of time—becomes even more questionable.
This example, wherein the self-refresh mode is exited, entered, and exited again so rapidly is a somewhat extreme illustration for the sake of highlighting the problem. Notwithstanding, in an era presently becoming increasingly dominated by gigahertz-clocking devices and increasingly larger DRAM devices with thousands upon thousands of rows of memory cells to be refreshed, actual loss of memory contents upon mode changes is a very real concern. This is particularly true if the DRAM devices are used in slower-clocking systems where auto-refresh commands may be issued even less frequently.
At present, there is one predominant solution to the problem of one or more rows not being refreshed in a timely fashion as a result of a DRAM device switching between self-refresh and operational modes. Specifically, this solution is the standard observed by the Joint Electron Device Engineering Council (JEDEC). The JEDEC standard suggests that, upon issuing the command to exit the self-refresh mode, and after the self-refresh mode has exited but before the system issues any other commands, the system should be programmed to first issue an auto-refresh command. This solution addresses the problems described previously in that the next row of memory is immediately refreshed upon exiting self-refresh, hopefully preserving the integrity of the data stored in that row. Similarly, even if the DRAM device repeatedly and frequently transitions between self-refresh mode and operational mode, as in the case depicted in FIG. 2 , at least one row will be refreshed with each transition.
Unfortunately, the JEDEC suggestion has its shortcomings. First, because the JEDEC suggstion is a programming convention which depends on programmers actually and religiously including the mandated auto-refresh command in their programs. Accordingly, the JEDEC suggestion is often ignored by programmers, causing the problems previously described. Second, the JEDEC approach wastes time. Under the JEDEC approach, the system first must wait for the passage of the interval t xsr just in case a row was being self-refreshed at that moment the self-refresh exit command was issued; then, resumption of read and write operations is further delayed by the time it takes to complete an auto-refresh of the next row. At least one of those intervals represents a pure waste of time. If a row was being refreshed when the self-refresh command was issued, then auto-refresh of the next row—and the time required to complete it—was unnecessary. On the other hand, if a row was not being refreshed when the self-refresh command was issued, then waiting the interval t xsr for such a coincidental, hypothetical row refresh to complete was wasted.
FIG. 3A illustrates the time wasted using the JEDEC convention using a timing diagram of a system entering and exiting a self-refresh mode pursuant to this approach. Specifically, FIG. 3A shows the state of the CK 310 , CK* 315 , and CKE 320 signals, and the present command 325 . Between times T 0 330 and T 1 340 , the CKE signal 320 is driven low, directing the memory device into self-refresh mode which the memory device enters at T 1 340 . The self-refresh mode continues until between times Ta 0 350 and Ta 1 360 , when the CKE signal 320 is driven high, directing the memory device to exit the self-refresh state. In the event that a row refresh was being executed at the time the device was directed to exit the self-refresh state, the device is permitted a wait state to allow that refresh to be completed. The system issues a null, NOP command at Ta 1 360 allowing this interval to pass. After the conclusion of that transitional period t xsr , the memory device is potentially available for read and write operations at Tb 0 370 . However, in accordance with the JEDEC approach, before useful read and write operations should be conducted, the system first issues an auto-refresh command at Tb 0 370 to compensate for any refresh cycles that were lost while the memory device transitioned. In other words, after the self-refresh mode is terminated, the system must allow two intervals to pass upon exiting self-refresh: the waiting interval, t xsr , and the time required to perform an auto-refresh operation, t rfc .
In sum, devices currently used may not refresh rows of memory cells sufficiently rapidly upon switching between self-refresh and operational modes, and the contents of those memory cells could become corrupted. This problem currently is addressed by programming conventions. However, these programming conventions require that programmers actually implement the conventions, and they also waste time in mandating potentially unnecessary row refreshes at the conclusion of mandated transitional waiting intervals. It is to this concern that the present invention is directed.
SUMMARY OF THE INVENTION
Control logic is added to ensures refreshing of at least one row due to be refreshed while the self-refresh state exits and before the DRAM device resumes operational status. The added control logic avoids the possibility that rows will not be refreshed within the mandated refresh interval. Ensuring completion of the refresh of at least one row before exiting self-refresh eliminates a potentially wasted wait state followed by an interval being set aside for the system to the need for the system to manually direct an auto-refresh of at least one row. Alternatively, the added logic can be arrayed to refresh at least one row upon entering self-refresh, upon both entering and exiting self-refresh, or to perform a burst refresh of every row of the device before exiting self-refresh to ensure that no rows will go for too long a period without being refreshed as the self-refresh state is entered and exited.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a conventional memory device equipped with self-refresh circuitry.
FIG. 2 is a timing diagram illustrating the possible refresh problems of a conventional DRAM device upon exiting self-refresh.
FIG. 3A is a timing diagram showing the operation of a conventional DRAM device observing conventional protocols upon exiting self-refresh.
FIG. 3B is a timing diagram showing the operation of a DRAM device employing an embodiment of the present invention upon exiting self-refresh mode.
FIG. 4 is a block diagram of self-refresh control logic adapted to employ an embodiment of the present invention.
FIG. 5 is a block diagram of a computer system employing an embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
To avoid wasting so much time while still preserving memory integrity, a preferred embodiment of the present invention ensures that the next row of memory cells is refreshed during the interval t xsr after receipt of the self-refresh mode exit command, avoiding the time wasted on the auto-refresh cycle recommended by the JEDEC suggestion. In short, upon receipt of the self-refresh mode exit command, an embodiment of the present invention determines if a row is already being refreshed and, if not, the preferred embodiment disengages the memory device's on-board self-refresh clock and immediately initiates a refresh of the next row of memory cells. In other words, a preferred embodiment of the present invention has the advantage of the JEDEC suggestion in initiating a row refresh upon the transition between self-refresh and operational modes, but without wasting one of the time intervals required by the JEDEC suggestion. Furthermore, because under this preferred embodiment the DRAM device would include logic to execute this refresh upon self-refresh exit, this preferred embodiment of the present invention is not dependent upon programmers remembering to adhere to the JEDEC convention.
FIG. 3B shows how the preferred embodiment of the present invention eliminates the t rfc period, returning the memory device to operational status more quickly. The timing diagram of FIG. 3B depicts most of the same phases as FIG. 3 A. In the interest of brevity, these aspects have been provided with the same reference numerals, and an explanation of the repetitive phases will not be repeated.
The main difference between the timing diagram depicted in FIG. 3B as opposed to the timing diagram depicting a conventional approach depicted in FIG. 3A is that the t rfc period has been eliminated as a result of the application of the preferred embodiment of the present invention. Specifically, at time Ta 1 370 in FIG. 3B , the command being executed is not the autorefresh command executed during the corresponding interval in FIG. 3A , but instead is designated “VALID” to represent the preferred embodiment immediately refreshing the next row of memory cells. As a result, at time Tb 0 370 , instead of the system issuing an auto-refresh command to refresh the next row as shown in FIG. 3B , the preferred embodiment has already refreshed a row between times Ta 1 and Tb 0 , and is ready for a valid operational command.
It should be emphasized that, under both the prior art JEDEC approach and the preferred embodiment of the present invention, once the system issues the self-refresh exit command, the system must allow passage of the interval t xsr to allow for the asynchronicity between the system clock and the self-refresh clock within the DRAM device. However, because the preferred embodiment ensures that, even if a row was not already being refreshed upon issuance of the self-refresh exit command, a row will be refreshed during passage of the interval t xsr , there is no need for the system to perform an auto-refresh and wait the additional interval t rfc before resuming operations.
The preferred embodiment requires, as shown in functional block form in FIG. 4 , some additional elements being applied to the self-refresh control logic 400 . The transitional refresh controller 410 receives three signals and issues two signals. The row transitional refresh controller 410 receives a self-refresh engage signal 415 which indicates that the self-refresh command has been received, latched, and decoded. The refresh engage signal 415 also engages the self-refresh clock 430 . The self-refresh clock 430 , once engaged by the refresh engage signal 415 , continues to pulse the row refresh controller 420 with its clock pulse signal 480 until the CKE signal 440 is driven high, signaling the end of the self-refresh mode. The transitional refresh controller 110 also receives the CKE signal 440 , to monitor whether the system has issued a self-refresh mode exit command.
The transitional refresh controller 410 also monitors the row refresh active signal 450 generated by the row refresh circuitry 420 to determine whether a row already is being refreshed. If the row refresh active signal 450 indicates a row already is being refreshed when the CKE signal 420 is driven high, the transitional refresh controller 410 does nothing; the current row refresh is permitted to continue and conclude, then the self-refresh mode is exited. On the other hand, if the row refresh active signal 450 indicates a row is not being refreshed upon the CKE signal 440 being driven high, the transitional refresh controller 410 issues a self-refresh clock disengage signal 460 , and immediately issues a row refresh signal 470 to cause the next row of memory cells to be refreshed. The row refresh controller 420 can be triggered to refresh a row either by the transitional refresh controller 410 or the clock pulse signal 480 generated by the self-refresh clock 430 . The row refresh active signal 450 is also communicated to the refresh counter 170 ( FIG. 1 ) to cause the refresh counter 170 to be incremented.
Upon completion of the row being refreshed, the memory device is returned to operational mode as already is known in the art. In either case, because a row already has immediately been refreshed, there is no longer any need for the system to be programmed to perform an auto-refresh on the next row upon the memory device resuming operational mode.
As shown in FIG. 5 , a computer system 500 can take advantage of the present invention by incorporating DRAM devices 501 adapted with a preferred embodiment of the present invention as previously described. With reference to FIG. 5 , a computer system 500 including the DRAM 501 includes a processor 502 for performing various functions, such as performing specific calculations or tasks. In addition, the computer system 500 includes one or more input devices 504 , such as a keyboard or a mouse, coupled to the processor 502 through a memory controller 506 and a processor bus 507 to allow an operator to interface with the computer system 500 . Typically, the computer system 500 also includes one or more output devices 508 coupled to the processor 502 , such output devices typically being a printer or a video terminal. One or more data storage devices 510 are also typically coupled to the processor 502 through the memory controller 506 to store data or retrieve data from external storage media (not shown). Examples of typical data storage devices 510 include hard and floppy disks, tape cassettes, and compact disk read-only memories (CD-ROMs). The DRAM 501 is typically coupled to the memory controller 506 through the control bus 520 and the address bus 530 . The data bus 540 of the DRAM 501 is coupled to the processor 502 either directly (as shown) or through the memory controller 506 to allow data to be written to and read from the DRAM 501 . The computer system 500 may also include a cache memory 514 coupled to the processor 502 through the processor bus 507 to provide for the rapid storage and reading of data and/or instructions, as is well known in the art.
From the foregoing it will be appreciated that, although specific embodiments of the invention have been described herein for purposes of illustration, various modifications may be made without deviating from the spirit and scope of the invention. Just to name some examples, embodiments of the present invention also could preserve the integrity of data stored in memory by refreshing the next row upon entering self-refresh, upon entering and exiting self-refresh, or by refreshing all the rows in a burst refresh before transitioning between self-refresh and operational modes. Also, although this description of a preferred embodiment concerns a system in which the refresh counter is incremented and the next row in sequence is refreshed, the present invention could be used in a system where the row currently indicated by the refresh counter is refreshed before the refresh counter is updated. Similarly, the present invention could be used in a system where the refresh counter is decremented rather than incremented. In addition, the present invention could be used in a system where the refresh counter comprises a gray code counter, a conventional sequential counter, or any other type of counter. Accordingly, the invention is not limited except as by the appended claims.
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A system and method are disclosed to add logic to the self-refresh control logic presently employed in DRAM devices to ensure that, upon transitions between self-refresh mode and operational mode, at least one row of memory cells due to be refreshed is refreshed during the wait state following issuance of the transition command. Conducting this refresh during this existing wait state eliminates both the concern as to whether rows have been refreshed within the mandated refresh interval and the time required to execute an auto-refresh of at least one row upon completion of the transition.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application is a continuation of prior U.S. application Ser. No. 11/337,900, filed Jan. 23, 2006 now U.S. Pat. No. 7,137,970.
FIELD OF THE INVENTION
The present invention relates to test methods for assessing irritation of portions of skin and/or assessing inhibition and/or reduction of such irritation. More particularly, the present invention relates to test methods for assessing the inhibition and/or reduction of irritation of skin from fibrous structures, especially lotion-containing fibrous structures that come in contact with such irritated skin.
BACKGROUND OF THE INVENTION
Cold and allergy sufferers often develop irritation around the nostrils as a result of repeated and frequent rubbing of the skin site with facial tissues. This irritation is a combination of the inherent irritant properties of the tissue components (chemical irritation), and mechanical irritation from friction.
Over the years, formulators have tried to assess the irritation and/or the inhibition and/or reduction of such irritation by various products, such as topical lotions and creams.
A prior art test method comprised compromising a portion of skin with a chemical irritant and then directly applying a lotion to the irritated portion of skin.
Another prior art test method comprised compromising a portion of skin by tape stripping the portion of skin and then contacting the irritated portion of skin with a facial tissue in a one-wipe pass over the irritated portion of skin.
However, none of the existing prior art test methods are suitable for assessing skin irritation of cold sufferers because the irritation around one's nostrils during a cold is a combination of effects, including the inherent irritant properties of the tissue components (i.e., chemical irritants), and mechanical irritation from friction resulting from frequent and repeated rubbing of the irritated skin with a tissue.
Accordingly, there is a need for a test method that is capable of assessing the skin irritation present on the skin of a cold sufferer.
SUMMARY OF THE INVENTION
The present invention fulfills the need identified above by providing a test method that is capable of assessing irritation of portions of skin and/or assessing inhibition and/or reduction of such irritation.
In one example of the present invention, a method for assessing irritation of skin, the method comprising the steps of:
a. irritating a portion of skin by a first mode;
b. irritating the portion of skin by a second mode different from the first mode, wherein the second mode comprises rubbing a substrate on the portion of skin; and
c. assessing erythema and/or dryness of the portion of the skin; and
d. optionally, assessing objective instrumental measurements, is provided.
In another example of the present invention, a method for assessing irritation of skin, the method comprising the steps of:
a. irritating a portion of skin by a first mode comprising contacting the portion of skin with a chemical irritant;
b. irritating the portion of skin by a second mode different from the first mode; and
c. assessing erythema and/or dryness of the portion of the skin; and
d. optionally, assessing objective instrumental measurements, is provided.
Accordingly, the present invention provides a test method that is capable of assessing irritation of portions of skin and/or assessing inhibition and/or reduction of such irritation.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1A is a bar chart showing dryness data from two substrates tested according to one example of the present invention;
FIG. 1B is a bar chart showing erythema data from two substrates tested according to one example of the present invention;
FIG. 2A is a bar chart showing dryness data from two substrates tested according to one example of the present invention;
FIG. 2B is a bar chart showing erythema data from two substrates tested according to one example of the present invention;
FIG. 3A is a bar chart showing dryness data from two substrates tested according to one example of the present invention; and
FIG. 3B is a bar chart showing erythema data from two substrates tested according to one example of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Definitions
“Mode” as used herein means a specific way of doing something. In the present case, it is a specific way out of numerous ways of irritating a portion of skin.
“Irritation” or “irritate” or “irritating” as used herein means that a portion of skin exhibits signs of chafing and/or inflammation and/or abrasion.
“Chemical irritation” as used herein means that a chemical agent contacts a portion of skin such that it irritates the portion of skin.
“Physical irritation” as used herein means that a non-chemical agent contacts a portion of skin in such a way to cause irritation of the portion of skin. Nonlimiting examples of sources of physical irritation include tape stripping the portion of skin, rubbing a substrate across the portion of skin, rubbing a hand across the portion of skin, occluding the skin from an external environment, and subjecting the portion of skin to excessive wind.
“Mechanical irritation” as used herein means a physical irritation that is caused by a physical object contacting the portion of skin to cause irritation.
“Frictional irritation” as used herein means a mechanical irritation that is caused by a physical object, such as a substrate, repeatedly contacting the portion of skin in a rubbing manner to cause irritation.
“Substrate” as used herein means a physical object upon which and/or within which one or more additive ingredients may be deposited.
“Fibrous structure” as used herein means a substrate that comprises one or more fibers, natural and/or synthetic. Nonlimiting examples of fibrous structures include feminine care products (pads, tampons, wipes), adult incontinence products, sanitary tissue products (facial tissue, toilet tissue, paper towels, wipes), baby care products (diapers, wipes), fabrics and home care products (cleaning wipes, dusting wipes).
“Sanitary tissue products” as used herein means facial tissue, toilet tissue, paper towels and wipes.
“Erythema” as used herein means visually recognizable redness of the skin.
“Dryness” as used herein means visually recognizable powderiness or cracking of the skin.
Test Method
The test method of the present invention comprises a method for assessing irritation of skin.
The method comprises the steps of:
a. irritating a portion of skin by a first mode;
b. irritating the portion of skin by a second mode different from the first mode, wherein the second mode comprises rubbing a substrate on the portion of skin; and
c. assessing erythema and/or dryness of the portion of the skin; and
d. assessing objective instrumental measurements.
The step of irritating a portion of skin may comprise chemically irritating a portion of skin and/or physically irritating a portion of skin.
Nonlimiting examples of portions of skin suitable for use in the present invention include forearm skin. In one example, the portion of skin is the volar and/or flexor surface portion of the forearm. Two, three or more portions of skin on one forearm may be subjected to the test method of the present invention. The portions of skin may be any size. In one example, the size of the portion of skin is 4 cm×4 cm. Portions of skin may be 4 cm apart from the other on the forearm.
A nonlimiting example of chemical irritation of a portion of skin includes contacting the portion of skin with a skin irritant agent. Nonlimiting examples of suitable skin irritants include sodium lauryl sulfate and sodium laureth sulfate.
A nonlimiting example of physical irritation of a portion of skin includes tape stripping the portion of skin. In other words, applying a piece of tape to the portion of skin and then removing the tape such that the portion of skin becomes irritated.
Another nonlimiting example of physical irritation of a portion of skin includes occluding the portion of skin. One way of occluding comprises placing a patch, such as a Webril® patch, commercially available from Professional Medical Products Company) over the portion of skin. Tape, such as an occlusive, hypoallergenic tape, such as Blenderm® tape, commercially available from 3M Company, may be used to cover the patch and hold the patch in place on the portion of skin. The patch may also comprise a skin irritant to facilitate irritation of the skin.
The rubbing of the substrate across the portion of skin can occur in a back and forth manner, a circular manner and/or a multi-directional (two or more) manner and/or in a unidirectional manner, if the skin has been chemically irritated prior to rubbing.
The substrate may be a fibrous structure.
The fibrous structure may be embossed and/or may be pattern-densified.
The fibrous structure may be creped or uncreped.
The fibrous structure may comprise a nonwoven web.
The fibrous structure may comprise a cellulosic fiber containing web.
In one example, the substrate is a single- or multi-ply sanitary tissue product, specifically a sanitary tissue product comprising an additive ingredient, such as a lotion.
The additive ingredient may be present on a surface of the substrate. When the additive ingredient is a lotion and it is present on the surface of the substrate, a silicone may be present directly on the substrate and then the lotion may be present on top of the silicone. The lotion may be a transferable lotion, a minimally transferable lotion or a non-transferable lotion.
Nonlimiting examples of additive ingredients include chemical softening agents, dyes, colorants, surfactants, absorbents, permanent wet strength agents, temporary wet strength agents, antiviral agents, oils, nanotechnology agents, lotion compositions, skin benefits agents, skin healants, perfumes, especially long lasting and/or enduring perfumes, antibacterial agents, botanical agents, disinfectants, pharmaceutical agents, film formers, deodorants, opacifiers, astringents, solvents, cooling sensate agents such as camphor, thymol and menthol, and preservatives.
Nonlimiting examples of suitable chemical softening agents include silicones, quaternary ammonium compounds, petrolatum, oils, and mixtures thereof.
Nonlimiting examples of silicones include aminosilicones and/or cationic silicones.
In another example of the present invention, the method comprises the steps of:
a. irritating a portion of skin by a first mode comprising contacting the portion of skin with a chemical irritant;
b. irritating the portion of skin by a second mode different from the first mode;
c. assessing erythema and/or dryness of the portion of the skin; and
d. assessing objective instrumental measurements.
The methods of the present invention may include pretreatment steps prior to irritating a portion of skin. Nonlimiting examples of pretreatment steps include contacting a portion of skin with an additive ingredient, such as a lotion.
Assessing erythema and/or dryness of the portion of the skin can be done visually. For example, a panel of experts can visually grade erythema and/or dryness of a portion of skin. Suitable grading scales for both erythema and dryness are set out below in Tables 1 and 2, respectively.
TABLE 1
Erythema Grading Scale
0
No apparent cutaneous involvement
0.5
Faint, barely perceptible erythema or slight dryness
1
Faint, but definite erythema, definite dryness
1.5
Well-defined erythema or faint erythema with definite dryness
2
Moderate erythema; may have papules or deep fissures
2.5
Moderate erythema with barely perceptible edema;
may have a few papules
3
Severe erythema (beet redness); may have generalized papules
3.5
Moderate-to-severe erythema with moderate edema
4
Moderate-to-severed erythema and/or extending edema, may have
generalized vesicles or eschar formations
TABLE 2
Dryness Grading Scale
0
None
1
Patchy, slight powderiness with small scales
2
General, slight powderiness with small lifting scales
3
General, moderate powderiness with cracking and scales
4
General, heavy powderiness with cracking and lifting scales
5
Heavy cracking (possibly bleeding) and lifting scales
6
Severe cracking, with bleeding and sloughing of large scales
The step of assessing erythema and/or dryness by objective instrumental measurements may include evaluating the portion of skin with a transepidermal water loss instrument, commercially available from Cortex Technology, Denmark under the tradename TEWL, DermaLab® Evaporimeter. Participants may be conditioned in a temperature and humidity controlled room (73° F.±4° F. (about 23° C.±2.2° C.) and a relative humidity of 50%±10%) for approximately 20 minutes.
Even though the description above of this test method is directed to assessing irritation of skin, one can also measure lotion or additive (such as perfumes, preservatives, antiviral, antibacterial, skin healants, skin benefit agents, non-active agents) transfer during this test method by determining the amount of lotion or other additive that transfers from the substrate to the skin.
Additive Ingredients
Nonlimiting examples of additive ingredients that may be incorporated on and/or in the substrate include surface treating compositions including, but not limited to, nanotechnology agents, lotion compositions, skin benefit agents, perfumes, especially long lasting and/or enduring perfumes, antibacterial agents, antiviral agents, botanical agents, disinfectants, pharmaceutical agents, film formers, deodorants, opacifiers, astringents, solvents, cooling sensate agents, such as camphor, thymol and menthol.
A surface treating composition, for purposes of the present invention, is a composition that improves the tactile sensation of a surface of a substrate, such as a fibrous structure, perceived by a user whom holds the substrate and rubs it across the user's skin. Such tactile perceivable softness can be characterized by, but is not limited to, friction, flexibility, and smoothness, as well as subjective descriptors, such as a feeling like lubricious, velvet, silk or flannel.
The surface treating composition may or may not be transferable. Typically, it is substantially non-transferable.
The surface treating composition may increase or decrease the surface friction of the surface of the fibrous structure, especially the user contacting surface of the fibrous structure. Typically, the surface treating composition will reduce the surface friction of the surface of the fibrous structure compared to a surface of the fibrous structure without such surface treating composition.
Nonlimiting examples of suitable surface treating agents can be selected from the group consisting of: polymers such as polyethylene and derivatives thereof, hydrocarbons, waxes, oils, silicones, organosilicones (oil compatible), quaternary ammonium compounds, fluorocarbons, substituted C 10 -C 22 alkanes, substituted C 10 -C 22 alkenes, in particular derivatives of fatty alcohols and fatty acids (such as fatty acid amides, fatty acid condensates and fatty alcohol condensates), polyols, derivatives of polyols (such as esters and ethers), sugar derivatives (such as ethers and esters), polyglycols (such as polyethyleneglycol) and mixtures thereof.
In one example, the surface treating composition of the present invention is a microemulsion and/or a macroemulsion of a surface treating agent (for example an aminofunctional polydimethylsiloxane, specifically an aminoethylaminopropyl polydimethylsiloxane) in water. In such an example, the concentration of the surface treating agent within the surface treating composition may be from about 3% to about 60% and/or from about 4% to about 50% and/or from about 5% to about 40%. Nonlimiting examples of such microemulsions are commercially available from Wacker Chemie (MR1003, MR103, MR102). A nonlimiting example of such a macroemulsion is commercially available from General Electric Silicones (CM849).
Nonlimiting examples of suitable waxes may be selected from the group consisting of: paraffin, polyethylene waxes, beeswax and mixtures thereof.
Nonlimiting examples of suitable oils may be selected from the group consisting of: mineral oil, silicone oil, silicone gels, petrolatum and mixtures thereof.
Nonlimiting examples of suitable silicones may be selected from the group consisting of: polydimethylsiloxanes, aminosilicones, cationic silicones, quaternary silicones, silicone betaines and mixtures thereof.
Nonlimiting examples of quaternary ammonium compounds suitable for use in the present invention include the well-known dialkyldimethylammonium salts such as ditallowdimethylammonium chloride, ditallowdimethylammonium methylsulfate, di(hydrogenated tallow)dimethylammonium chloride. In one example, the surface treating composition comprises di(hydrogenated tallow)dimethylammonium chloride, commercially available from Witco Chemical Company Inc. of Dublin, Ohio as Varisoft 137®.
Nonlimiting examples of ester-functional quaternary ammonium compounds having the structures named above and suitable for use in the present invention include the well-known diester dialkyl dimethyl ammonium salts such as diester ditallow dimethyl ammonium chloride, monoester ditallow dimethyl ammonium chloride, diester ditallow dimethyl ammonium methyl sulfate, diester di(hydrogenated)tallow dimethyl ammonium methyl sulfate, diester di(hydrogenated)tallow dimethyl ammonium chloride, and mixtures thereof. In one example, the surface treating composition comprises diester ditallow dimethyl ammonium chloride and/or diester di(hydrogenated)tallow dimethyl ammonium chloride, both commercially available from Witco Chemical Company Inc. of Dublin, Ohio under the tradename “ADOGEN SDMC”.
For purposes herein, nanotechnology agents are defined as particles exhibiting average diameters of about 500 nm or less. In one example, particle size distributions of the nanotechnology agents in the present invention may fall anywhere within the range from about 2 nm to less than about 500 nm, alternatively from about 2 nm to less than about 100 nm, and alternatively from about 2 nm to less than about 50 nm. For example, a layer synthetic silicate can have a mean particle size of about 25 nanometers while its particle size distribution can generally vary between about 10 nm to about 40 nm. Alternatively, nanotechnology agents can also include crystalline or amorphous particles with a particle size from about 2 to about 100 nanometers, alternatively from about 2 to about 50 nanometers.
Inorganic nanotechnology agents generally exist as oxides, silicates, carbonates and hydroxides. Some layered clay minerals and inorganic metal oxides can be examples of nanotechnology agents. The layered clay minerals suitable for use in the present invention include those in the geological classes of the smectites, the kaolins, the illites, the chlorites, the attapulgites and the mixed layer clays. Typical examples of specific clays belonging to these classes are the smectices, kaolins, illites, chlorites, attapulgites and mixed layer clays. Smectites, for example, include montmorillonite, bentonite, pyrophyllite, hectorite, saponite, sauconite, nontronite, talc, beidellite, volchonskoite and vermiculite. Kaolins include kaolinite, dickite, nacrite, antigorite, anauxite, halloysite, indellite and chrysotile. Illites include bravaisite, muscovite, paragonite, phlogopite and biotite. Chlorites include corrensite, penninite, donbassite, sudoite, pennine and clinochlore. Attapulgites include sepiolite and polygorskyte. Mixed layer clays include allevardite and vermiculitebiotite. Variants and isomorphic substitutions of these layered clay minerals offer unique applications.
The layered clay minerals of the present invention may be either naturally occurring or synthetic. Example of suitable nanotechnology agents include natural or synthetic hectorites, montmorillonites and bentonites. Other examples include hectorites clays. Commercially available, and typical sources of commercial hectorites are the LAPONITEs from Southern Clay Products, Inc., U.S.A; Veegum Pro and Veegum F from R. T. Vanderbilt, U.S.A.; and the Barasyms, Macaloids and Propaloids from Baroid Division, National Read Comp., U.S.A.
The inorganic metal oxides of the present invention may be silica- or alumina-based nanotechnology agents that are naturally occurring or synthetic. Aluminum can be found in many naturally occurring sources, such as kaolinite and bauxite. The naturally occurring sources of alumina are processed by the Hall process or the Bayer process to yield the desired alumina type required. Various forms of alumina are commercially available in the form of Gibbsite, Diaspore, and Boehmite from manufactures such as Condea, Inc.
Boehmite alumina is a water dispersible, inorganic metal oxide having a mean particle size distribution of about 25 nanometers. Such product is commercially available, for example under the trade name Disperal P2™.
Natural clay minerals typically exist as layered silicate minerals and less frequently as amorphous minerals. A layered silicate mineral has SiO 4 tetrahedral sheets arranged into a two-dimensional network structure. A 2:1 type layered silicate mineral has a laminated structure of several to several tens of silicate sheets having a three layered structure in which a magnesium octahedral sheet or an aluminum octahedral sheet is sandwiched between two sheets of silica tetrahedral sheets.
A sheet of an expandable layer silicate has a negative electric charge, and the electric charge is neutralized by the existence of alkali metal cations and/or alkaline earth metal cations. Smectite or expandable mica can be dispersed in water to form a sol with thixotropic properties. Further, a complex variant of the smectite type clay can be formed by the reaction with various cationic organic or inorganic compounds. As an example of such an organic complex, an organophilic clay in which a dimethyldioctadecyl ammonium ion (a quaternary ammonium ion) is introduced by cation exchange and has been industrially produced and used as a gellant of a coating.
With appropriate process control, the processes for the production of synthetic nanoscale powders (i.e. synthetic clays) does indeed yield primary particles, which are nanoscale. However, the particles are not usually present in the form of discrete particles, but instead predominantly assume the form of agglomerates due to consolidation of the primary particles. Such agglomerates may reach diameters of several thousand nanometers, such that the desired characteristics associated with the nanoscale nature of the particles cannot be achieved. The particles may be deagglomerated, for example, by grinding as described in EP-A 637,616 or by dispersion in a suitable carrier medium, such as water or water/alcohol and mixtures thereof.
The production of nanoscale powders such as layered hydrous silicate, layered hydrous aluminum silicate, fluorosilicate, mica-montmorillonite, hydrotalcite, lithium magnesium silicate and lithium magnesium fluorosilicate are common. An example of a substituted variant of lithium magnesium silicate is where the hydroxyl group is partially substituted with fluorine. Lithium and magnesium may also be partially substituted by aluminum. In fact, the lithium magnesium silicate may be isomorphically substituted by any member selected from the group consisting of magnesium, aluminum, lithium, iron, chromium, zinc and mixtures thereof.
Synthetic hectorite was first synthesized in the early 1960's and is now commercially marketed under the trade name LAPONITE™ by Southern Clay Products, Inc. There are many grades or variants and isomorphous substitutions of LAPONITE™ marketed. Examples of commercial hectorites are LAPONITE B™, LAPONITE S™, LAPONITE XLS™, LAPONITE RD™ and LAPONITE RDS™. One embodiment of this invention uses LAPONITE XLS™ having the following characteristics: analysis (dry basis) SiO 2 59.8%, MgO 27.2%, Na 2 O 4.4%, Li 2 O 0.8%, structural H 2 O 7.8%, with the addition of tetrasodium pyrophosphate (6%); specific gravity 2.53; bulk density 1.0.
Synthetic hectorites, such as LAPONITE RD™, do not contain any fluorine. An isomorphous substitution of the hydroxyl group with fluorine will produce synthetic clays referred to as sodium magnesium lithium fluorosilicates. These sodium magnesium lithium fluorosilicates, marketed as LAPONITE™ and LAPONITE S™, may contain fluoride ions of up to approximately 10% by weight. It should be understood that the fluoride ion content useful in the compositions described herein can comprise any whole or decimal numeric percentage between 0 and 10 or more. LAPONITE B™, a sodium magnesium lithium fluorosilicate, has a flat, circular plate-like shape, and may have a diameter with a mean particle size, depending on fluoride ion content, that is any number (or narrower set of numbers) that is within the range of between about 25-100 nanometers. For example, in one non-limiting embodiment, LAPONITE B™ may be between about 25-40 nanometers in diameter and about 1 nanometer in thickness. Another variant, called LAPONITE S™, contains about 6% of tetrasodium pyrophosphate as an additive. In some instances, LAPONITE B™ by itself is believed, without wishing to be bound to any particular theory, to be capable of providing a more uniform coating (that is, more continuous, i.e., less openings in the way the coating forms after drying), and can provide a more substantive (or durable) coating than some of the other grades of LAPONITE™ by themselves (such as LAPONITE RD™). The coating preferably forms at least one layer of nanotechnology agents on the surface which has been coated, and is substantially uniform.
Inorganic metal oxides generally fall within two groups-photoactive and non-photoactive nanotechnology agents. General examples of photoactive metal oxide nanotechnology agents include zinc oxide and titanium oxide. Photoactive metal oxide nanotechnology agents require photoactivation from either visible light (e.g. zinc oxide) or from UV light (TiO 2 ). Zinc oxide coatings have generally been used as anti-microbial agents or as anti-fouling agents.
Non-photoactive metal oxide nanotechnology agents do not use UV or visible light to produce the desired effects. Examples of non-photoactive metal oxide nanotechnology agents include, but are not limited to: silica and alumina nanotechnology agents, and mixed metal oxide nanotechnology agents including, but not limited to smectites, saponites, and hydrotalcite.
A lotion composition may comprise oils and/or emollients and/or waxes and/or immobilizing agents The lotion compositions may be heterogeneous. They may contain solids, gel structures, polymeric material, a multiplicity of phases (such as oily and water phase) and/or emulsified components. It may be difficult to determine precisely the melting temperature of the lotion composition, i.e. difficult to determine the temperature of transition between the liquid form, the quasi-liquid from, the quasi-solid form and the solid form. The terms melting temperature, melting point, transition point and transition temperature are used interchangeably in this document and have the same meaning.
The lotion compositions may be semi-solid, of high viscosity so they do not substantially flow without activation during the life of the product or gel structures.
The lotion compositions may be shear thinning and/or they may strongly change their viscosity around skin temperature to allow for transfer and easy spreading on a user's skin.
The lotion compositions may be in the form of emulsions and/or dispersions.
A nonlimiting example of a suitable lotion composition of the present invention comprises a chemical softening agent, such as an emollient, that softens, soothes, supples, coats, lubricates, or moisturizes the skin. The lotion composition may sooth, moisturize, and/or lubricate a user's skin.
The lotion composition may comprise an oil and/or an emollient. Nonlimiting examples of suitable oils and/or emollients include glycols (such as propylene glycol and/or glycerine), polyglycols (such as triethylene glycol), petrolatum, fatty acids, fatty alcohols, fatty alcohol ethoxylates, fatty alcohol esters and fatty alcohol ethers, fatty acid ethoxylates, fatty acid amides and fatty acid esters, hydrocarbon oils (such as mineral oil), squalane, fluorinated emollients, silicone oil (such as dimethicone) and mixtures thereof.
Nonlimiting examples of emollients useful in the present invention can be petroleum-based, fatty acid ester type, alkyl ethoxylate type, or mixtures of these materials. Suitable petroleum-based emollients include those hydrocarbons, or mixtures of hydrocarbons, having chain lengths of from 16 to 32 carbon atoms. Petroleum based hydrocarbons having these chain lengths include petrolatum (also known as “mineral wax,” “petroleum jelly” and “mineral jelly”). Petrolatum usually refers to more viscous mixtures of hydrocarbons having from 16 to 32 carbon atoms. A suitable Petrolatum is available from Witco, Corp., Greenwich, Conn. as White Protopet® 1 S.
Suitable fatty acid ester emollients include those derived from long chain C 12 -C 28 fatty acids, such as C 16 -C 22 saturated fatty acids, and short chain C 1 -C 8 monohydric alcohols, such as C 1 -C 3 monohydric alcohols. Nonlimiting examples of suitable fatty acid ester emollients include methyl palmitate, methyl stearate, isopropyl laurate, isopropyl myristate, isopropyl palmitate, and ethylhexyl palmitate. Suitable fatty acid ester emollients can also be derived from esters of longer chain fatty alcohols (C 12 -C 28 , such as C 12 -C 16 ) and shorter chain fatty acids e.g., lactic acid, such as lauryl lactate and cetyl lactate.
Suitable fatty acid ester type emollients include those derived from C 12 -C 28 fatty acids, such as C 16 -C 22 saturated fatty acids, and short chain (C 1 -C 8 and/or C 1 -C 3 ) monohydric alcohols. Representative examples of such esters include methyl palmitate, methyl stearate, isopropyl laurate, isopropyl myristate, isopropyl palmitate, and ethylhexyl palmitate. Suitable fatty acid ester emollients can also be derived from esters of longer chain fatty alcohols (C 12 -C 28 and/or C 12 -C 16 ) and shorter chain fatty acids e.g., lactic acid, such as lauryl lactate and cetyl lactate.
Suitable alkyl ethoxylate type emollients include C 12 -C 18 fatty alcohol ethoxylates having an average of from 3 to 30 oxyethylene units, such as from about 4 to about 23. Nonlimiting examples of such alkyl ethoxylates include laureth-3 (a lauryl ethoxylate having an average of 3 oxyethylene units), laureth-23 (a lauryl ethoxylate having an average of 23 oxyethylene units), ceteth-10 (acetyl ethoxylate having an average of 10 oxyethylene units), steareth-2 (a stearyl ethoxylate having an average of 2 oxyethylene units) and steareth-10 (a stearyl ethoxylate having an average of 10 oxyethylene units). These alkyl ethoxylate emollients are typically used in combination with the petroleum-based emollients, such as petrolatum, at a weight ratio of alkyl ethoxylate emollient to petroleum-based emollient of from about 1:1 to about 1:3, preferably from about 1:1.5 to about 1:2.5.
The lotion compositions of the present invention may include an “immobilizing agent”, so-called because they are believed to act to prevent migration of the emollient so that it can remain primarily on the surface of the fibrous structure to which it is applied so that it may deliver maximum softening benefit as well as be available for transferability to the user's skin.
Immobilizing agents include agents that are may prevent migration of the emollient into the fibrous structure such that the emollient remain primarily on the surface of the fibrous structure and/or sanitary tissue product and/or on the surface treating composition on a surface of the fibrous structure and/or sanitary tissue product and facilitate transfer of the lotion composition to a user's skin. Immobilizing agents may function as viscosity increasing agents and/or gelling agents.
Nonlimiting examples of suitable immobilizing agents include waxes (such as ceresin wax, ozokerite, microcrystalline wax, petroleum waxes, fisher tropsh waxes, silicone waxes, paraffin waxes), fatty alcohols (such as cetyl, cetaryl, cetearyl and/or stearyl alcohol), fatty acids and their salts (such as metal salts of stearic acid), mono and polyhydroxy fatty acid esters, mono and polyhydroxy fatty acid amides, silica and silica derivatives, gelling agents, thickeners and mixtures thereof.
One or more skin benefit agents may be included in the substrate. Nonlimiting examples of skin benefit agents include zinc oxide, vitamins, such as Vitamin B3 and/or Vitamin E, sucrose esters of fatty acids, such as Sefose 1618S (commercially available from Procter & Gamble Chemicals), antiviral agents, anti-inflammatory compounds, lipid, inorganic anions, inorganic cations, protease inhibitors, sequestration agents, chamomile extracts, aloe vera, calendula officinalis , alpha bisalbolol, Vitamin E acetate and mixtures thereof.
Nonlimiting examples of suitable skin benefit agents include fats, fatty acids, fatty acid esters, fatty alcohols, triglycerides, phospholipids, mineral oils, essential oils, sterols, sterol esters, emollients, waxes, humectants and combinations thereof.
The skin benefit agent may be alone, included in a lotion composition and/or included in a surface treating composition. A commercially available lotion composition comprising a skin benefit agent is Vaseline® Intensive Care Lotion (Chesebrough-Pond's, Inc.).
Nonlimiting Example of Present Invention
Samples to be evaluated are obtained. Participants for the study are selected. Participants were excluded from the study if: 1) they were currently participating in any other clinical study, 2) they had participated in any type of research study involving the forearms within the previous twenty-one days, 3) they had allergies to soap, detergent, perfume, cosmetics, and/or toiletries, 4) they were taking anti-inflammatory corticosteriods or other medications that may interfere with test results, 5) they had had eczema or psoriasis within the past six months, 6) they had been diagnosed with skin cancer within the previous twelve months, 7) they were pregnant or lactating, or 8) they had cuts, scratches, rashes or any condition on their inner forearms that may prevent a clear assessment of their skin.
Participants are given an Olay® Sensitive Skin Care Bar for all bathing and showering needs to be used beginning with their enrollment into the study and until their participation in the study is complete. Instruct participants to avoid scrubbing the inner forearm areas and allow the soap and water to flow over the areas without washing. In addition, they are required to refrain from using lotions, creams, ointments, oils and/or moisturizers on the forearm areas.
Two to three test sites are identified and demarcated on each volar surface of the forearm. Test sites are measured 4 cm×4 cm, and were 4 cm apart. Each site is treated with a different sample. The samples are randomized, and the technician conducting the test is not aware of the test sample identity. Treatments at the test sites include a 24-h occluded patch of 0.3 ml of a solution of SLS, and wiping (rubbing) the test samples in a back and forth motion a specified number of times.
For the sample wipes, each sample is folded up to five times, and wiped 10 times in a back and forth movement (20 passes). The test sample is then refolded and the wiping repeated with a fresh area of the sample. New samples are used, as needed until the total number of back and forth wipes is completed. The SLS is patched using a Webril® patch (Professional Medical Products Company) covered by an occlusive, hypoallergenic tape (Blenderm®, 3M Company).
Scoring of the test sites is done at baseline (prior to any treatment) and before and after either patching with SLS or wiping with the test samples. When SLS patching is conducted, the patches are removed 30-60 minutes before grading. In all studies, visual scoring is conducted by expert graders under a 100 watt incandescent daylight bulb. If a test site exhibits an erythema grade of “2” or higher, that test site receives no further treatment.
EXAMPLE
Example 1
Facial Tissues Comprising Lotion
Test sites on the flexor surfaces of the forearms of 19 subjects (participants) were wiped with the lotion-containing samples (tissues) on day 1 using a total of 200 wipes (400 passes) in order to pretreat the portion of skin with lotion. This was followed by a 24-h occlusive patch with 0.25% SLS (sodium lauryl sulfate). Visual scoring of erythema and dryness was conducted. Scoring of the test sites was done prior to any treatment, immediately after the sample wipes (post sample wipes), 30 minutes after removal of the SLS patch (post-SLS patch, 24-h post wipe), and 24 hours after removal of the SLS patch (post-SLS patch, 48-h post wipe). The group mean scores (+/− standard error) for dryness (a) and erythema (b) were determined for each scoring timepoint. Post-baseline average treatment comparisons were performed using analysis of variance (“ANOVA”). All other treatment comparisons were performed using the stratified Cochran Mantel Haenszel (“CMH”) test. For Sample 1, the concentration of lotion on the sample was 0.668 mg/cm 2 . Since Sample 2 is a currently marketed competitor's product, the lotion concentration is unknown. As shown in FIG. 1 :
Sample 1 is statistically lower than tissue Sample 2 (with lotion) (p<0.05).
Example 2
Facial Tissues Comprising Lotion
Test sites on the flexor surfaces of the forearms of 18 subjects were pretreated by 24-h patch with 0.25% SLS. After patch removal, test sites were wiped with the test samples (tissues) using a total of 200 wipes (400 passes). Visual scoring of erythema and dryness of the test sites was done prior to any treatment, 30 minutes after removal of the SLS patch, immediately after the sample wipes (post sample wipe), and at 24 and 48 hours after the sample wipes (post-sample wipe, 24-h, and post-sample wipe, 48-h). The change from post-SLS baseline was determined for each subject, then the average over all subjects was calculated. The post-baseline average was calculated using the average of all post-baseline visits for each subject, then calculating the average over all subjects. Treatment comparisons for erythema at 24-h, 48-h, and the change in post-baseline average were performed using ANOVA on ranks. For Sample 1, the concentration of lotion was 0.668 mg/cm 2 . Since Sample 2 is a currently marketed competitor's product, the lotion concentration is unknown. As shown in FIG. 2 :
Sample 1 is statistically lower than Sample 2 (without lotion) (p<0.05).
Sample 2 is statistically lower than Sample 1 (without lotion) (p<0.05).
Sample 2 is statistically lower than Sample 1 (without lotion) (p<0.05).
Sample 1 is statistically lower than Sample 2 (with lotion) (p<0.05).
Example 3
Facial Tissues Comprising Lotion
Test sites on the flexor surfaces of the forearms of 15-18 subjects were pretreated by 24-h patch with 0.25% SLS. After patch removal, test sites were wiped with the test samples using a total of 200 wipes (400 passes). Visual scoring of erythema and dryness of the test sites was done prior to any treatment, 30 minutes after removal of the SLS patch, immediately after the sample wipes, and at 24, 48 and 72 hours after the sample wipes. The change from post-SLS baseline was determined for each subject, then the average over all subjects was calculated. The post-baseline average was calculated using the average of all post-baseline visits for each subject, then calculating the average over all subjects. Erythema post-baseline average comparisons were performed using ANOVA. All other treatment comparisons were performed using ANOVA on ranks. For Sample 1, the concentration of lotion was 0.668 mg/cm 2 and the concentration of lotion for Sample 2 was 0.815 mg/cm 2 . Both samples had 3000 ppm of silicone on them. As shown in FIG. 3 :
Sample 1 is statistically lower than Sample 2 (without silicone) (p<0.05).
Sample 1 is statistically lower than Sample 2 (without silicone) (p<0.05).
Sample 2 is statistically lower than tissue Sample 1 (without silicone) (p<0.05).
Example 4
Feminine Pads Comprising Lotion
Test sites on the flexor surfaces of the forearms of 19 subjects (participants) were wiped with the lotion-containing samples (feminine pads). On day 1 using a total of 120 wipes in order to pretreat the portion of skin with lotion. Different test products were used. This was followed by a 24-h occlusive patch with 0.25% SLS (sodium lauryl sulfate). Visual scoring of erythema and dryness was conducted. Scoring of the test sites was done prior to any treatment, immediately after the sample wipes (post sample wipes), 30 minutes after removal of the SLS patch (post-SLS patch, 24-h post wipe), and 24 hours after removal of the SLS patch (post-SLS patch, 48-h post wipe). The group mean scores (± standard error) for dryness (a) and erythema (b) were determined for each scoring timepoint. Objective instrumental measurements were taken using but not restricted to DermaLab® evaporimeter instrument will be used to assess transepidermal water loss (TEWL) at the test sites including the upper arm control site following all visual grading evaluations.
Post-baseline average treatment comparisons were performed using analysis of variance (“ANOVA”). All other treatment comparisons were performed using the stratified Cochran Mantel Haenszel (“CMH”) test.
For all of Examples 1-3, the post-baseline average was calculated using the average of all post-baseline visits for each subject, then calculating the average over all subjects. If there were missing visits for a subject, that subject was not included in the calculation of the post-baseline average.
Additionally, in those experiments where SLS patching occurred prior to treatment with the lotion, the results are presented as the change in group mean. The change in group mean was calculated by determining the change from post-SLS baseline for each subject, then calculating the average over all subjects. In some cases, not all test subjects completed the entire test. In these instances, the scores recorded for the dropped subjects were removed from the calculation of the change in group mean for that timepoint.
All p-values were unadjusted for multiple comparisons.
All documents cited in the Detailed Description of the Invention are, in relevant part, incorporated herein by reference; the citation of any document is not to be construed as an admission that it is prior art with respect to the present invention. To the extent that any meaning or definition of a term in this written document conflicts with any meaning or definition of the term in a document incorporated by reference, the meaning or definition assigned to the term in this written document shall govern.
The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Instead, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as “40 mm” is intended to mean “about 40 mm”.
While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
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Test methods for assessing irritation of portions of skin and/or assessing inhibition and/or reduction of such irritation are provided.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention pertains to accouterments for projectile firing devices, such as bows, although it could also be adapted for use with other kinds of projectile firing devices, such as firearms. A force is exerted on such a firing device in a given direction when the projectile is fired. In the case of a bow, the archer experiences a "kick" wherein the bow feels as if it jumps forward, and the archer must maintain firm control to hold the bow steady or perhaps even avoid dropping it. This can adversely affect not only the accuracy, but even the force, of the archer's shot, and, of course, it greatly affects the archer's comfort. The present invention has been shown to dramatically minimize the "kick" experienced by the archer.
2. Description of the Background
A number of devices have been proposed either for controlling bow kick or for dampening bow vibrations. Some of these simply consist of elongate dead weights which may conveniently be mounted on a fitting provided on the front of most bows, so that the elongate dead weight extends forward horizontally from the bow in use.
An "hydraulic stabilizer" has been offered for sale under the name "Pro King."
British Patent No. 1,296,201 discloses a stabilizer which appears to be intended primarily for use in dampening the vibrations set up by the bow string upon its release. In one embodiment of this device, there is provided a chamber partially filled with liquid in which a spherical element is centered, lengthwise of the chamber, apparently for movement therealong, between two compression springs.
U.S. Pat. Nos. 4,660,538 and No. 4,779,602 likewise disclose compensators or stabilizers having relatively movable parts, reciprocable in a horizontal direction, with the movable parts being the outer or casing-like portions of the devices. Springs are provided to bias the movable members to a given starting position.
U.S. Pat. No. 4,245,612 discloses a device in which generally cylindrically-shaped annular weights are removably mounted in a casing and held by a compression spring. It would appear that these weights may not be intended to move relative to the casing in use, e.g. since a scent-impregnated cylinder is interposed between and abutting the weights and the opposite end of the casing.
U.S. Pat. No. 3.683,883 discloses various forms of stabilizers using magnetized weights, while U.S. Pat. No. 3,342,172 discloses still another "shot cushioning" means for a bow.
SUMMARY OF THE INVENTION
The present invention provides a compensator which is believed to provide better results than the aforementioned prior art, and more specifically, preliminary field tests of the device according to the invention have indicated that its efficacy is quite outstanding.
The compensator of the present invention comprises an elongate casing adapted to permit the casing to be mounted on a bow or other projectile firing device with the length of the casing generally parallel to the direction of the force which is exerted on the firing device when the projectile is fired. The casing has interior walls of constant transverse cross-sectional configuration along a significant portion of its length.
A weighted piston member is disposed in the casing and reciprocable lengthwise of the casing. The piston member has a length, along a significant portion of which the transverse cross-sectional configuration of the piston member mates with that of the constant portion of the interior walls of the casing. The clearance between the piston member and the constant portion of the interior walls of the casing is sufficiently small to maintain the piston member generally parallel to the casing, but sufficiently large to allow free reciprocation of the piston member along the casing.
It has been found that improved results are achieved if the end of the piston member which is rearmost with respect to the direction of the force on the projectile firing device is closed and aerodynamically shaped to facilitate movement of the piston toward the opposed end of the casing, the other end of the piston preferably being adapted to offer greater resistance to movement of the piston toward its respective end of the casing.
Said other end of the piston is preferably hollow and opens longitudinally through the other end of the piston member. The hollow may be defined by a skirt.
Even further improvements are experienced if the skirt is laterally perforated and/or if the casing is partially filled with a liquid such as an hydraulic-type oil. Performance is also believed to be improved by providing a one-way valve in association with the open end of the piston member allowing fluid flow outwardly from the hollow. Such a valve may be held against the open end of the piston member by a compression spring cooperative between the valve and the casing.
Indeed, compression springs or other cushioning means are preferably provided at least between the piston and the aforementioned one end of the casing, and preferably between both ends of the piston member, respectively, and the adjacent ends of the casing. In such case, the same spring can be used to cushion the movement of the piston member toward the other end of the casing and also to hold the valve against the end of the piston, as previously described.
It is a principal object of the present invention to provide an improved reactive force compensator for a projectile firing device.
A corollary object of the present invention is to provide such a compensator in which a weighted piston reciprocable within a horizontally elongated casing is of an improved configuration.
Still another object of the present invention is to provide cushioning means, a liquid volume, and/or a one-way valve, in association with such improved piston member.
Still other objects, features and advantages of the present invention will be made apparent by the following description, the drawings and the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic side view of a bow showing a compensator according to the present invention mounted thereon and illustrating the orientation of the compensator and its parts relative to the bow in use.
FIG. 2 is an enlarged longitudinal cross-sectional view through the compensator of FIG. 1.
FIG. 3 is a transverse cross section taken on line 3--3 of FIG. 2.
DETAILED DESCRIPTION
FIG. 1 shows a side view of a bow 10 comprising a riser section 14 and limbs 18, between the outer ends of which is strung the string 12. The riser section 14 includes a central grip area 16 configured for engagement by the archer's hand. Below the grip area 16, riser section 14, on its forward side, is provided with a threaded female fitting, as is well known in the art. To this fitting there is removably, and more specifically threadedly, mounted a compensator 20 according to the present invention.
Referring now jointly to FIGS. 1, 2 and 3, compensator 20 comprises a casing including an elongate cylindrical tube-like portion 22 and a pair of dome-like end closures 24 and 26 which are fixedly secured to respective opposite ends of cylindrical portion 22 in any suitable manner, preferably one which seals the connection. For example, the parts 22, 24 and 26 of the casing can be formed of a suitable rigid plastic, and the closures 24 and 26 can be interference fitted, bonded, or otherwise sealingly fixed to the cylindrical portion 26.
The casing is adapted to be mounted so that it projects generally horizontally forward from the bow 10 in use, as shown in FIG. 1, and with one end, specifically the end closed by closure 26, rearmost, near the riser section 14 of the bow. It will be appreciated that, in use, when the bow string 12 is drawn back, the archer exerts a forward force on the grip area 16 of the bow. When the bow string is released, the archer feels a kick or tendency for the bow to jump forward, because a force generally represented by the vector F acts on the bow. It will be seen that, when mounted in the manner described, i.e. with closure 26 closest to the bow and the compensator 20 extending horizontally forward therefrom, compensator 20 lies generally parallel to the force F, and with the one end of the compensator adjacent closure 26 rearmost with respect to the direction of the force F. As used herein, the compensator will be considered "generally parallel" to the force F if its lengthwise direction has at least a substantial component which is parallel to the force F.
The manner in which the casing is adapted to be so mounted on the bow is shown best in FIG. 2. Closure 26 has a central endwise bore 28. After closure 26 had been fixed to the adjacent end of cylindrical portion 22 of the casing, a sealing washer 30 is placed inside the casing adjacent to and coaxial with bore 28. Then, a screw 32 is placed through the aligned openings of the washer 30 and the bore 28, from the inside of the casing outward, so that the head of the screw bears against the washer 30 and helps to tighten the seal. Another washer 34, which is curved to match the configuration of the closure 26, is placed about the shank of screw 32 externally of closure 26, followed by a lock nut 36.
It can be seen that the end of screw 32 protrudes beyond nut 36 thereby providing a threaded male member which can be connected to the aforementioned fitting on the bow 10 either directly or with a nipple or the like.
After assembly of the parts associated with closure 26 as described above, the other parts of the compensator can be emplaced within the casing from the other end prior to final closing and sealing by closure 24. These internal parts include a weighted piston 38. "Weighted" will be used herein to refer generically to pistons which inherently have sufficient weight to cause the necessary reciprocation along the casing as well as to pistons to which weight is somehow added.
It will be appreciated that the casing has internal walls which have a constant transverse cross-sectional configuration along a significant portion of the length of the casing, specifically a circular transverse cross-sectional configuration along cylindrical portion 22. The piston member has a length extending generally parallel to that of the casing, and along a significant portion of which the transverse cross-sectional configuration of the piston member mates with that of the constant portion of the interior walls of the casing. In this case, the transverse external configuration of the piston is circular and is of constant diameter except for the aerodynamically formed head end of the piston to be described more fully below. Also, the clearance between the piston member 38 and the portion 22 of the casing is sufficiently small to maintain the piston member generally parallel to the casing, but sufficiently large to allow free reciprocation of the piston member along the casing. Thus, piston member 38 moves like a true piston, remaining in parallel alignment with the casing, by way of contrast, for example, to the spherical element disclosed in British Patent No. 1,296,201.
The end 40 of piston member 38 closest to the mounting end of the casing, i.e. the end carrying closure member 26, is closed and the adjacent portion of the piston member solid, providing the bulk of the weight of the piston. The solid portion of the piston represents slightly more than half its length and extends through a substantial part of the aforementioned constant diameter part of the piston member. As previously mentioned, the one end 40 is aerodynamically configured, like a bullet head, to facilitate movement of piston member 38 toward the mounting end of the casing.
The other end of piston member 38 is preferably configured to offer greater resistance to movement of the piston member toward the other end of the casing, i.e. the free or outer end. More specifically, it has been found that better results are obtained if this other end of the piston is defined by a cylindrical skirt 42 which defines an internal hollow 44 of the piston opening endwise therethrough.
It has further been found that even better results are obtained if the skirt 42 is laterally perforated. In the preferred embodiment shown, the perforations are in the form of twelve bores or ports, nine of which are shown at 46 in FIG. 2. The ports are arranged in sets of four, each set being spaced lengthwise along the skirt 44 from the next, and the ports in each set being circumferentially spaced from each other by 90°. It is believed to be particularly beneficial to incline the ports, as shown, toward the blind end of the piston member 38 from the outer diameter to the inner diameter of the skirt 44. In a preferred embodiment, the angle of inclination of the ports 46 with respect to the axis of the piston member is 45°.
The endwise opening defined by skirt 44 has associated therewith a one-way valve 48, which can be a flapper type, or any other conventional type valve. The valve 48 could be mounted to the skirt 44, but as shown, is held against the outer end of skirt 44 by a compression spring 50 interposed between valve 48 and the end of the casing defined by closure 24. Valve 48 is arranged so as to allow fluid flow from the interior of the skirt to the exterior.
In addition to holding the valve 48 against the open end or skirt end of the piston member 38, compression spring 50 also serves to cushion movements of piston 38 toward the free or outer end of the casing in use. A similar spring 52 coacts between the mounting end of the casing and the closed end 40 of the piston member 38, through an intervening disk-shaped plate 54, to similarly cushion movements of piston member 38 toward the inner or connection end of the casing in use.
Before closing with member 24, the casing has emplaced therein a volume of liquid 56. The volume should not completely fill the free space in the casing unoccupied by other parts of the apparatus, but should fill at least well over half of that space. An example of a suitable liquid is a lightweight oil or hydraulic fluid. The aforementioned clearance between the piston member 38 and the tubular portion 22 of the casing should be sufficient to allow some fluid flow lengthwise across the piston.
The lengths of the piston and casing should preferably be chosen, bearing in mind the space taken up by other parts such as the springs 50 and 52, so that the piston will have a travel of at least about 1-1/2 inches in use, but preferably somewhat greater travel.
The size and weight of the apparatus can be varied to provide for the requirements of different archers and/or different bows. The device can also be adapted for use on other types of projectile firing devices, e.g. for use on firearms to compensate for recoil. The primary changes which would have to be made in the latter case would be that the means of mounting the apparatus on, for example, a rifle, would have to be changed, and the orientation of mounting would be reversed, since the recoil force for which compensation is desired is rearward with a rifle, rather than forward as with a bow.
Whether intended for use with bows, firearms, or perhaps even other types of projectile firing devices, various modifications might be made over the preferred embodiment described above. Accordingly, it is intended that the scope of the present invention be limited only by the claims which follow.
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A reactive force compensator is provided for a projectile firing device, such as a bow or gun, on which a force is exerted in a given direction when the projectile is fired. The compensator comprises an elongate casing adapted to permit the casing to be mounted on the projectile firing device with the length of the casing parallel to the direction of said force. A weighted piston member is disposed in the casing and adapted to reciprocate therein while remaining parallel thereto. The piston preferably has an aerodynamic end, disposed rearmost with respect to said force, and a more resistive end disposed forwardmost with respect to the force. Preferably, the latter end is defined by a hollow opening endwise through the piston member.
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CROSS-REFERENCE TO RELATED APPLICATION
This application is a divisional of application Ser. No. 12/466,471, filed May 15, 2009, the disclosure of which is hereby incorporated in its entirety by reference herein.
BACKGROUND
U.S. Pat. No. 5,993,350 to Lawrie et al. provides a powertrain system for a hybrid vehicle. The hybrid vehicle includes a heat engine, such as a diesel engine, and an electric machine, which operates as both an electric motor and an alternator, to power the vehicle. The hybrid vehicle also includes a manual-style transmission configured to operate as an automatic transmission from the perspective of the driver. The engine and the electric machine drive an input shaft which in turn drives an output shaft of the transmission. In addition to driving the transmission, the electric machine regulates the speed of the input shaft in order to synchronize the input shaft during either an upshift or downshift of the transmission by either decreasing or increasing the speed of the input shaft. Operation of the transmission is controlled by a transmission controller which receives input signals and generates output signals to control shift and clutch motors to effect smooth launch, upshifts, and downshifts of the transmission.
U.S. Pat. No. 6,019,699 to Hoshiya et al. provides a drive control system for a hybrid vehicle that prevents a delay in the application of a one-way clutch in a transmission. In this drive control system, an electric motor and an internal combustion engine are coupled to the input side of a transmission having at least one gear stage to be set by applying a one-way clutch. The drive control system comprises: a detector for detecting a coasting state in which the one-way clutch is released in a deceleration state set with the gear stage; and, an input speed raising device for driving the electric motor when the coasting state is detected, so that the input speed of the transmission may approach the synchronous speed which is the product of the gear ratio of the gear stage to be set by applying the one-way clutch and the output speed of the transmission.
SUMMARY
A method for controlling a hybrid electric powertrain includes, in response to a request to increase a powertrain braking force on at least one of a plurality of traction wheels, (i) commanding at least one clutch to increase a gear ratio of a transmission, and (ii) during clutch stroke, commanding an electric machine to act as a generator such that the electric machine applies a braking force to at least one of the traction wheels.
A hybrid electric vehicle includes a plurality of traction wheels, an engine, and a transmission mechanically connected with the engine and including at least one clutch to alter a gear ratio of the transmission. The vehicle also includes an electric machine mechanically connected with at least one of the traction wheels, and a controller. The controller is configured to, in response to a request to increase a powertrain braking force on at least one of the traction wheels, (i) command the at least one clutch to increase the gear ratio of the transmission and (ii) during clutch stroke, command the electric machine to act as a generator such that the electric machine applies a braking force to at least one of the traction wheels.
A hybrid electric vehicle includes a plurality of traction wheels, an engine, and a transmission mechanically connected with the engine and including at least one clutch to alter a gear ratio of the transmission. The vehicle also includes an electric machine mechanically connected with at least one of the traction wheels, a power storage unit, and a controller. The controller is configured to, in response to a request to increase a braking force on at least one of the traction wheels, (i) command the electric machine to act as a generator such that the electric machine applies a braking force to at least one of the traction wheels until a state of charge of the power storage unit achieves a desired threshold, and (ii) command the at least one clutch to increase the gear ratio of the transmission after the state of charge of the power storage unit achieves the desired threshold.
While example embodiments in accordance with the invention are illustrated and disclosed, such disclosure should not be construed to limit the invention. It is anticipated that various modifications and alternative designs may be made without departing from the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of an example configuration of a hybrid electric vehicle.
FIG. 2 is a block diagram of another example configuration of a hybrid electric vehicle.
FIG. 3 is an example plot of transmission output torque generated in response to a request for a manual pull-in down shift.
FIG. 4 is an example plot of electric machine torque generated in response to a request for a manual pull-in down shift.
FIG. 5 is an example plot of net electric machine and transmission output torque generated in response to a request for a manual pull-in down shift.
FIG. 6 is an example plot of on-coming transmission clutch pressure command generated in response to a request for a manual pull-in down shift.
FIG. 7 is an example plot of off-going transmission clutch pressure command generated in response to a request for a manual pull-in down shift.
FIG. 8 is an example plot of engine speed during a manual pull-in down shift.
DETAILED DESCRIPTION
A driver of a hybrid electric vehicle may execute a manual pull-in downshift when, for example, travelling down a steep grade to achieve additional deceleration and minimize brake wear. The transmission may be downshifted into a lower gear via synchronous clutches or a coast clutch such that negative torque (braking torque) is transmitted to the driveline.
A delay in achieving the desired negative driveline torque during a manual pull-in may occur in hybrid electric drivetrains (and other drivetrain configurations). This delay can be up to one second as measured from the driver command or PRNDL position movement until torque increases in the halfshafts. Delay may result from the need to stroke the oncoming transmission clutch. Delay may also result from the need to ensure that the engine does not exceed its speed limit if the transmission is downshifted. The drivetrain may wait until the vehicle speed is reduced so that when the transmission is downshifted, the engine speed will not exceed its limit.
Certain embodiments disclosed herein may reduce/eliminate delays in achieving a desired negative driveline torque after the initiation of a request for a manual pull-in. As an example, an electric machine may be requested to provide negative driveline torque while a mechanical driveline is requested to perform a manual pull-in (e.g., stroke the oncoming clutch, bring the engine up to synchronous speed and transfer torque to the new ratio), provided the engine speed is less than a desired threshold for the desired gear. If the engine speed is greater than the desired threshold, the request to shift may be delayed until the engine speed is less than the desired threshold. Once the new gear is available, electric torque may be reduced as the mechanical torque is increased to provide generally consistent vehicle deceleration.
As another example, the electric machine may be requested to provide negative driveline torque (possibly while the mechanical driveline remains off) until an associated battery reaches a desired state of charge. (As apparent to those of ordinary skill, the electric machine acts as a generator while providing negative driveline torque. Electrical energy generated by the electric machine may be stored in the battery.) The mechanical driveline may then be requested to perform a manual pull-in, and electric torque reduced and mechanical torque increased as described herein.
Referring now to FIG. 1 , an automotive vehicle 10 may include a drivetrain 12 . The drivetrain 12 may include tire/wheel assemblies 14 n ( 14 a , 14 b , 14 c , 14 d ), an engine 16 , electric machine 18 (e.g., electric rear axle drive), and power storage unit 19 (e.g., battery). The drivetrain 12 may also include a crank integrated starter/generator (CISG or other electric machine) 20 , transmission 22 , front differential 24 , and front half shafts 26 . As apparent to those of ordinary skill, components immediately adjacent to each other are mechanically connected. The drivetrain 12 may further include a rear differential 28 , rear half shafts 30 , and a rear prop shaft 32 .
The transmission 22 may include an input 34 mechanically connected with the engine 16 , an output 36 mechanically connected with the tire/wheel assemblies 14 a , 14 b via the front differential 24 , one or more gears 38 , and one or more clutches 40 arranged in a known fashion.
As known in the art, the CISG 20 may be used to start or stop the engine 16 ; the engine may generate motive power to drive the tire/wheel assemblies 14 a , 14 b via the transmission 22 , front differential 24 , and front half shafts 26 . As also known in the art, the electric machine 18 may act as a motor to generate motive power to drive the tire wheel assemblies 14 c , 14 d via the rear prop shaft 32 , rear differential 28 , and rear half shafts 30 ; the electric machine 18 may also act as a generator to generate electrical power for storage by the power storage unit 19 . Either or both of the engine 16 and electric machine 18 may be used to generate motive power to drive the tire/wheel assemblies 14 n.
One or more controllers 42 may be in communication with the electric machine and/or transmission 22 . The controllers 42 may submit torque commands/requests to the electric machine 18 such that, for example, the electric machine consumes electrical power to generate a propulsion force for the tire/wheel assemblies 14 c , 14 d , or consumes mechanical power to generate a braking force (negative torque) for the tire/wheel assemblies 14 c , 14 d . The controllers 42 may submit commands/requests to the transmission 22 such that, for example, a speed ratio of the transmission 22 (e.g., the ratio of the speed of the input 34 to the speed of the output 36 ) changes via application of the clutches 40 to the gears 38 in a known fashion. As discussed below, these commands may be coordinated to provide negative driveline torque in response to a request for a manual pull-in downshift with little or no delay.
Referring now to FIG. 2 , numbered elements that differ by 100 relative to FIG. 1 have similar descriptions to the numbered elements of FIG. 1 . The drivetrain 112 of FIG. 2 includes a power transfer unit 136 , front prop shaft 138 , and a coupling 140 . As known in the art, these additional components may (i) permit the engine 116 to drive any of the tire/wheel assemblies 114 n and (ii) permit the electric machine 118 to drive any of the tire/wheel assemblies 114 n . Of course, other drivetrain configurations are also possible.
Referring now to FIGS. 3 through 8 , the operation of an engine, electric machine, transmission clutches, and controllers (such as the engines 16 , 116 , electric machines 18 , 118 , clutches 40 , 140 , and controllers 42 , 142 illustrated in FIGS. 1 and 2 ) are described with reference to several operating modes that occur in response to a request for a manual pull-in downshift. While there are five such operating modes in the embodiments of FIGS. 3 through 8 , any suitable number of operating modes may be used.
FIG. 3 depicts conventional transmission output torque to a driveline during a manual pull-in downshift. That is, transmission output torque first overshoots (after some delay) and then undershoots its final target value. With the addition of offsetting electric machine torque to the driveline as depicted in FIG. 4 , the net torque output of the electric machine and transmission to the driveline as depicted in FIG. 5 has reduced overshoot and undershoot, as well as reduced delay.
Mode 1 : The strategy enters Mode 1 at the initiation of a manual pull-in downshift request. A controller may command an electric machine to provide negative torque (i.e., act as a generator). This torque may continue to ramp to a calibrateable value of maximum torque, which may be a function of vehicle speed.
The strategy may exit Mode 1 after the controller receives notification that a transmission is ready to downshift (increase its gear ratio) via, for example, a shift ready flag or any other known technique. If the engine speed is such that it will not exceed its limit when downshifted, this may occur immediately. If the engine speed is such that it will exceed its limit when downshifted, the strategy may wait until the engine speed decreases to a suitable value before the shift ready flag is set. In other embodiments, the shift ready flag may be set when a state of charge of a power storage unit achieves a threshold value (assuming engine speed, if the engine is on, is such that it will not exceed its limit when downshifted).
Mode 2 : The electric machine torque command initiated in Mode 1 may continue (e.g., ramp until a calibrateable value is achieved, and then hold), if it has not already achieved the calibrateable value during Mode 1 . The controller may command an on-coming transmission clutch pressure to a high value to fill the clutch then cut back to a calibrateable value needed to start the shift as known in the art. The controller may command an off-going transmission clutch pressure to a reduced calibrateble value as also known in the art.
The strategy may exit Mode 2 at the expiration of a timer, detection of the torque phase, and/or detection of the shift start in a known fashion.
Mode 3 : The controller commands the on-coming transmission clutch pressure to increase and the off-going transmission clutch pressure to decrease in a coordinated manner as known in the art. The controller holds the electric machine torque at its current commanded value until a drop in engine speed (which corresponds to a peak in transmission output torque) is detected. (As known in the art, the described coordinated activity of the on-coming and off-going clutches causes a dip in engine speed if this coordination is biased towards a flare condition. If this coordination is biased towards a tie-up condition, the engine speed will, of course, rise and the transmission output torque will become more negative.) The controller may then command the electric machine to provide positive torque (i.e., act as a motor). (Alternatively, this command may be initiated after the strategy exits Mode 3 .) This torque may continue to ramp to a calibrateable value of maximum torque, which may be a function of vehicle speed
The strategy may exit Mode 3 when a speed ratio of the transmission has achieved a desired value, e.g., 5% of the final value.
Mode 4 : The controller may control the on-coming clutch through, for example, an open or closed loop profile, and command the off-going clutch to a pressure below its stroke pressure. The controller may command the electric machine back to, for example, zero torque (or other target value) as a function of percent shift complete. Commanding the electric machine torque to offset the inertia torque of the input to the transmission may provide a smoother shift. Keeping the electric machine torque at zero (or negative torque) may provide an elevated negative torque feel that may be desired when a manual pull-in shift is requested. Thus, this feel may be calibrated based on the particular vehicle application, and may also be calibrated for each shift type. For example, if the shift occurs immediately after the request, the driver may desire the extra inertia torque feel. If the shift occurs after several seconds to obtain better brake regeneration, the driver may not desire any torque feel as it would be delayed from the shift request.
The strategy may exit Mode 4 when the speed ratio of the transmission has achieved a desired value, e.g., 90% of the final value.
Mode 5 : This is the end mode and provides the completion of the shift event. As known in the art, the controller may command the on-coming transmission clutch pressure to a maximum and the off-going transmission clutch pressure to a minimum, etc.
While embodiments of the invention have been illustrated and described, it is not intended that these embodiments illustrate and describe all possible forms of the invention. The words used in the specification are words of description rather than limitation, and it is understood that various changes may be made without departing from the spirit and scope of the invention.
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A method for controlling a hybrid electric powertrain includes, in response to a request to increase a powertrain braking force on at least one of a plurality of traction wheels, (i) commanding at least one clutch to increase a gear ratio of a transmission, and (ii) during clutch stroke, commanding an electric machine to act as a generator such that the electric machine applies a braking force to at least one of the traction wheels.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a Divisional Application of U.S. patent application Ser. No. 12/352,110 filed on Jan. 12, 2009, now issued as U.S. Pat. No. 8,226,401, which is herein incorporated by reference in its entirety.
FIELD OF THE INVENTION
The present invention relates to gum manufacturing methods and systems and more particularly relates to the forming and conditioning of gum products as a precursor to dividing the gum into individual slab, stick or pellet type units.
BACKGROUND OF THE INVENTION
The process of making and packaging gum products involves a significant amount of machinery. For example, a substantially automated system and method for making slab/stick type gums, is shown in U.S. Pat. No. 6,254,373 entitled Gum Processing and Packaging System, which is assigned to the predecessor of interest of the present assignee. As shown in the '373 Patent, a process and apparatus for the continued production and processing and packaging of a final slab/stick type chewing gum is disclosed. The product is extruded as a continuous tape or ribbon and is eventually flattened into an approximate final cross-sectional size and shape and then inserted into a final gum sizing apparatus. Thereafter, the continuous strip of final chewing gum product is scored, cut into individual pieces and individually wrapped by a standard packaging machine. The present invention is directed towards improvements in the state of the art over such prior systems and equipment as shown in the '373 Patent.
BRIEF SUMMARY OF THE INVENTION
The present invention is directed toward improvements in the conditioning of chewing gum product to attempt to reach the optimal temperature, viscosity, and moisture content for quality and processing reasons, particularly when rolling and/or scoring the chewing gum product in sheet form. Such uniformity better insures that the correct amount of gum is in each individual unit of gum and that the shape, size and consistency is substantially the same. Achieving such uniformity and high volume production with such automation are a significant advantage for cost and quality reasons.
A first patent aspect of the present invention is directed toward gum manufacturing machinery comprising a gum loafing machine have an inlet receiving finished gum product and a forming die providing an outlet proximate a knife that is adapted to generate loaves of finished gum product. A gum conditioner is arranged downstream of the gum loafing machine that has a conveyor running through an environmental enclosure with a temperature control. The conveyor is adapted to convey the loaves of finished gum through the environmental enclosure.
According to the above aspect, the conveyor of the gum conditioner may include at least three conveyors arranged in a stacked vertical configuration with two different operational modes. In a first operational mode, the second conveyor runs in a first direction conveying loaves in a serpentine path over substantially the entire length of the second and third conveyors. In a second operational mode, the second conveyor runs in a second direction opposite the first direction to convey loaves in a cascading path thereby substantially bypassing the length of the second and third conveyors. As such, the residence time of the conveyor can be greatly varied by utilizing more or less of the overall gum conditioning conveyor length as may be desired (speed controls and speed changes to the conveyors may be additionally employed).
Another different feature which may be employed with the first above aspect is that the gum loafing machine may be employed to prepare a generally uniform shape and thickness of the finished gum product to facilitate more uniform conditioning and avoid the otherwise non-uniform and irregularly shaped thicknesses that may be output, for example from a gum mixing extruder that forms the finished gum product. The size of the loaves may be optimized for conditioning as opposed to a form that is necessarily suitable for rolling operations. Further, after the finished gum product is loafed and conditioned within the gum conditioner, a second forming extruder may be employed having a die adapted to form a continuous ribbon from the individual loaves to facilitate further downstream rolling of the sheet by rollers that progressively reduce a thickness of the continuous gum ribbon for subsequent gum dividing operations. As such, conditioning may occur in one form, while rolling and scoring is accomplished in a different form.
Another aspect of the present invention is directed toward gum manufacturing machinery comprising a gum mixer (e.g. at least one of a mixing extruder and a batch mixer) that receives a plurality of gum ingredients and mixes the gum ingredients into a finished gum product. A first forming extruder is arranged downstream of the gum mixer and receives the finished gum and forces the finished gum through a first forming die to generate a substantially uniform output shapes sufficient for conditioning. A gum conditioner is arranged downstream of the first forming extruder and has a conveyor running through an environmental enclosure with a temperature control. The conveyor is adapted to convey the substantially uniform output through the environmental enclosure. Further, and after such conditioning, a second forming extruder is arranged downstream of the gum conditioner that has a second forming die. The second forming extruder forces the finished gum through the second forming die to form a continuous gum ribbon. Rollers are subsequently arranged downstream of the forming extruder to progressively reduce a thickness of a the continuous gum ribbon for subsequent gum diving operations.
A feature according to the above aspect is that a first forming extruder may provide a discontinuous output such as separate loaves to facilitate conditioning whereas the second forming extruder produces the ribbon to facilitate rolling operations.
A further aspect of the present invention is directed toward a method of manufacturing gum comprising of mixing a plurality of gum ingredients into a finished gum; forming the finished gum into a substantially uniform output shape; conditioning the formed finished gum in a controlled temperature environment for a residence time; forming a continuous gum ribbon; progressively reducing the thickness of the continuous gum ribbon; and dividing the gum ribbon into individual pieces of gum.
It is an advantage of this method and further feature that different gum batch recipes for different finished gum products may be run through the same gum line. For example, the method may further comprise running a first gum mixture at a first predetermined residence time for conditioning in a controlled temperature environment; and running a second gum mixture different than the first gum mixture using the same gum line as for the first gum mixture but at a second residence time different than the first residence time for the first gum mixture. This can be further facilitated by use of a conveyor having multiple vertically spaced conveyors with two different operational modes for generating a serpentine path and a cascading path as described previously. Significantly different conditioning residence times may therefore be employed for different gum batch recipes.
Other aspects, objectives and advantages of the invention will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings incorporated in and forming a part of the specification illustrate several aspects of the present invention and, together with the description, serve to explain the principles of the invention. In the drawings:
FIG. 1 is a schematic diagram of an embodiment of gum manufacturing machinery illustrating one operating mode with a cascading path of loaves through a gum conditioner in accordance with an embodiment of the present invention;
FIG. 1A shows a schematic diagram of an alternative embodiment for mixing gum that may be substituted for the mixing extruder shown in FIG. 1 ;
FIG. 2 is another schematic diagram of the embodiment shown in FIG. 1 but illustrated in a different operational mode with loaves spending a longer residence time with a serpentine path through the gum conditioner as illustrated; and
FIG. 3 is a flow diagram illustrating a process for handling and processing finished gum product in accordance with an embodiment of the present invention.
While the invention will be described in connection with certain preferred embodiments, there is no intent to limit it to those embodiments. On the contrary, the intent is to cover all alternatives, modifications and equivalents as included within the spirit and scope of the invention as defined by the appended claims.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the FIGS. 1-2 , gum manufacturing machinery generally indicated at 10 for handling and processing finished gum product 12 is illustrated with, methodology of running through such machinery diagramed in FIG. 3 .
The gum manufacturing machinery 10 generally includes a gum mixer which as illustrated in FIG. 1 may take the form of a gum mixing extruder 14 ; or alternatively as shown in FIG. 1A a batch mixer 16 . Each of these may be used to produce a finished gum product 12 . For example as illustrated in FIG. 1 , the gum mixing extruder 14 includes a plurality of gum ingredient inputs 20 along its length for receipt of gum base and other gum ingredients such as flavorings, sugars, sweeteners, fillers, various agents, and the like. These inputs 20 are arranged along the length of a single mixing screw 22 having different screw mixing elements for input and mixing at different stages during the mixing process. For example, gum mixing extruders or other gum mixers are disclosed for example in U.S. Provisional Patent Application Nos. 61/016,016; 61/036,626; and 61/045,764, which are assigned to the present assignee, the disclosures of which are hereby incorporated by reference in their entireties. The output from the gum mixing extruder 14 is a finished gum product 12 that is readily suitable for consumption and chewing as it includes the water soluble sweeteners and flavorings desired by the consumer as well as the underlying chewable gum base to facilitate chewing. As illustrated, the output from a gum mixing extruder 14 may be generally irregular or otherwise non-uniform in shape in that it often will be output in an uneven stream of material having a non-uniform thickness of material. The same can be said of the output of a batch mixer 16 in that it is generally irregularly shaped without a consistent thickness. Thus, by producing finished gum product 18 , it may generate a non-uniform output 24 as diagrammed in FIG. 3 .
Given that the temperature of the finished gum product is not yet suitable or optimal for rolling activities, and that the temperature may need to be cooled or otherwise adjusted to allow the material to set sufficiently, it can be appreciated that the non-uniform output 24 is not conducive to generating uniform conditioning of the finished gum product. As such, a feed conveyor 26 feeds the uneven output 12 into a loafing machine 28 (also referred to herein as a loafing extruder) that forms discrete loaves of finished gum product as in step 27 in FIG. 3 . The loafing machine 28 may include a forming extruder 30 that forces the finished gum product through a forming die, thereby forming a uniform extrusion 33 as in FIG. 3 , that is periodically cut off into separate loaves 34 with finished gum product loaves being indicated at 36 in FIGS. 1-2 . To facilitate the cutting operation 34 , a knife 32 is used that periodically moves laterally across the forming die to cut and slice off individual loaves 36 .
An output conveyor 38 picks up the loaves cut off from the forming extruder 30 and runs at a slightly faster pace so as to space the individual loaves 36 at regular intervals as they are output from the forming extruder 30 and cut off by knife 32 . The forming extruder 30 includes only a single input and does not provide for input or mixing of additional ingredients into the finished gum product at this stage. Instead the loafing machine 28 and forming extruder 30 is merely employed to generate a relatively uniform and consistent thickness of material to facilitate more even conditioning of the finished gum product downstream.
As illustrated, the individual loaves 36 generally take the shape of the extruding die at the output of the forming extruder 30 and may have separate loaves integrally connected by thin webs that may be produced by teeth on the extruding die as illustrated. The loaves may have a slight parallelogram shape or be of slight shape variations in width and length, but the thickness of the individual loaves 36 is preferably between about ½ and 2 inches thick (vertically) with the length and width being between about 6 inches and 18 inches. The length and width dimensions are not as critical or important as it is the minimum thickness in one dimension that controls heat transfer. Thus, the minimum thickness dimension is of importance as this determines the relative residence time necessary for achieving sufficiently uniform viscosity and temperature for forming a thin ribbon to facilitate subsequent rolling and scoring operations.
The output conveyor 38 feeds the individual loaves 36 into a gum conditioner 40 that conditions the loaves of finished gum product 42 . More specifically, the gum conditioner 40 adjusts or otherwise conforms the temperature of the finished gum product 12 and attempts to obtain a substantially uniform temperature throughout. The gum conditioner 40 is arranged downstream of the gum loafing machine 28 for receiving the output thereof and includes three vertically stacked conveyors including a top conveyor 44 , an intermediate conveyor 46 and a bottom conveyor 48 that are all substantially contained and run through an environmental enclosure 50 , such as a long enclosed tunnel. Each of the conveyers 44 , 46 , 48 is contained in the environmental enclosure 50 , such that the gum product carried thereon is subjected to the temperature and humidity controlled environment within the enclosure 50 .
The gum conditioner 40 includes a temperature control, a humidity control and a residence time control. The temperature and humidity control can set and/or adjust the temperature and humidity within the environmental enclosure such that it may be different than that of the room in which the machinery is contained. The residence time control is provided with a wide degree of residence time variability in part due to speed adjustment but also due to a unique aspect presented by the arrangement of three conveyors, 44 , 46 and 48 and the operational mode variance as illustrated when comparing FIGS. 1 and 2 . As a result, a residence time can be predetermined and set and/or adjusted based upon the gum batch recipe 52 as indicated in FIG. 3 .
Typically, and depending upon the finished gum product, the raw output of the gum mixing extruder 14 will generally produce a gum output having an average temperature between 40 and 50° C. Within the environmental enclosure 50 of the gum conditioner 40 a generally uniform temperature is controlled to move the finished gum temperature to a substantially consistent and desirable temperature. Specifically, the environmental enclosure 50 may include a controlled temperature between 40° C. and about 50° C.; and a humidity of between about 20 and about 40%. Typically the temperature and humidity will be set at predetermined set points within those ranges depending upon the gum recipe and batch that is being run through the gum line at any particular instant.
As for the residence time, the embodiment provides for a wide control possibility in residence time based on speed control and operational mode. In one embodiment, the residence time may be as fast as about two minutes and as slow as about 20 minutes to provide for a minimal residence time or a very long residence time depending upon the gum batch recipe to appropriately provide the gum in best condition for later processing, such as rolling and scoring into sheets. The conditioner preferably has a residence time control variance of at least 10 minutes during operation thereof that is at least about 1 minute and less than about 30 minutes.
As can be seen in comparing FIGS. 1 and 2 , the gum conditioner 40 has two different operational modes. As shown in FIG. 2 , a first operational mode is provided in which the loaves follow a serpentine path substantially over the entire length of the intermediate and bottom conveyors, 46 and 48 . By having to travel the entire length of the lower two conveyors, the residence time is increased by virtual of the distance over which the finished gum product loaves must travel. However, if such a long residence time is not desired or needed, the distance can be short circuited as shown in FIG. 1 where a second operational mode is provided in which the loaves substantially bypass the length of the second and third conveyors. In this operational mode, the intermediate conveyor 46 runs in an opposite direction as that shown in FIG. 2 to prevent the loaves from reversing direction and instead the loaves cascade over the conveyors with a cascading path, thereby to substantially bypassing the length of the second and third conveyors. As shown, the second intermediate conveyor 46 has a portion that overlaps the top conveyor 44 to receive loaves that vertically drop down from the top conveyor onto the intermediate conveyor and likewise the bottom conveyor 48 has ends that overlap both of the ends of the intermediate conveyor for receipt of loaves that drop down on either the front or back end of the intermediate conveyor depending upon which operational mode is employed.
Depending upon the gum recipe batch being run on the gum line, upon exiting the gum conditioner, the finished gum loaves may have a temperature of between about 40 and 50° C. However, residence time is important and formula dependent to develop crystal structure and/or otherwise set up the firmness of the gum product, even if little or no temperature change occurs. At this point, the loaves are also set up enough with a sufficiently uniform viscosity to facilitate further processing such as rolling and scoring.
Accordingly at this point, a further conveyor 54 feeds the finished gum product loaves (at step 56 in FIG. 3 ) into a second downstream forming extruder 58 . The forming extruder 58 includes a forming die that is thin and elongated such that it produces a continuous finished gum product ribbon (at step 57 in FIG. 3 ) suitable for subsequent rolling and scoring operations. Specifically, the forming extruder 58 may include twin screws that break up the loaves and force the loaves through an elongate and thin forming die to produce the ribbon 60 .
Upon exiting the forming extruder 58 , the continuous gum ribbon 60 may be subject to a dusting operation 62 in which a duster 64 sprinkles powdered sweetener on the surface of the continuous gum ribbon 60 so as to prevent sticking and to facilitate better processing during subsequent rolling and scoring operations. It is understood that while such dusting will add some component to the eventual packaged gum, a “finish gum product” is considered to be produced at the very first step illustrated in the output of the gum mixing extruder 14 and the dusting at this point is primarily a processing aid adding only some additional component to the gum.
After passing through the duster 64 , the gum ribbon 60 is processed and run through a series of progressive rollers 66 that roll the continuous ribbon sheet to a uniform reduced thickness 68 . Once the gum ribbon 60 is progressively rolled to the desired thickness, then a scoring roller 70 may be employed as well as a lateral dividing roller 72 . These rollers 70 , 72 score and divide the gum ribbon 60 into individual scored sheets 74 as indicated at step 76 in FIG. 3 .
From here, the scored sheets 74 are conveyed to a further gum conditioner 78 having a conveyor 80 and an environmental enclosure in the form of a tunnel 82 to facilitate cooling of the individual scored sheets to stiffen the gum material of the sheets sufficiently prior to stacking so as to maintain shape rather than allow material creep. The gum conditioner 78 conditions individual sheets 84 sufficient to facilitate stacking of sheets 86 where the sheets can be stacked and stored in a conditioning room 88 . The stacked sheets are then stored in the conditioning room 90 at a lengthy interval to fully condition the gum sheets and achieve a sufficiently cool temperature until such time that the sheets are ready to be divided into individual gum pieces such as stabs or sticks and then packaged as indicated in step 92 in FIG. 3 .
All references, including publications, patent applications, and patents cited herein are hereby incorporated by reference to the same extent as if each reference were individually and specifically indicated to be incorporated by reference and were set forth in its entirety herein.
The use of the terms “a” and “an” and “the” and similar referents in the context of describing the invention (especially in the context of the following claims) is to be construed to cover both the singular and the plural, unless otherwise indicated herein or clearly contradicted by context. The terms “comprising,” “having,” “including,” and “containing” are to be construed as open-ended terms (i.e., meaning “including, but not limited to,”) unless otherwise noted. Recitation of ranges of values herein are merely intended to serve as a shorthand method of referring individually to each separate value falling within the range, unless otherwise indicated herein, and each separate value is incorporated into the specification as if it were individually recited herein. All methods described herein can be performed in any suitable order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of any and all examples, or exemplary language (e.g., “such as”) provided herein, is intended merely to better illuminate the invention and does not pose a limitation on the scope of the invention unless otherwise claimed. No language in the specification should be construed as indicating any non-claimed element as essential to the practice of the invention.
Preferred embodiments of this invention are described herein, including the best mode known to the inventors for carrying out the invention. Variations of those preferred embodiments may become apparent to those of ordinary skill in the art upon reading the foregoing description. The inventors expect skilled artisans to employ such variations as appropriate, and the inventors intend for the invention to be practiced otherwise than as specifically described herein. Accordingly, this invention includes all modifications and equivalents of the subject matter recited in the claims appended hereto as permitted by applicable law. Moreover, any combination of the above-described elements in all possible variations thereof is encompassed by the invention unless otherwise indicated herein or otherwise clearly contradicted by context.
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Gum manufacturing machinery and method of manufacturing gum is illustrated in which a gum loafing machine generates loaves of finished gum that are then subsequently run through a gum conditioner to more uniformly set the temperature and viscosity of the gum material prior to further processing. Upon achieving the appropriate conditioning level, a further forming extruder may be used to generate a continuous gum ribbon for subsequent rolling and scoring operations. The gum conditioner may include vertically stacked conveyors that have different operational modes including a first mode that provides a serpentine path for a long residence time and a second mode that provides a cascading path that avoids or bypasses much of the length of some of the conveyors to provide a shorter residence time. The gum manufacturing machinery may be used in an adjustable manner so as to accommodate difference gum recipes for different batches of gum product.
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[0001] This patent application is a divisional of U.S. patent application Ser. No. 10/247,272 which was filed on Sep. 19, 2002
FIELD OF THE INVENTION
[0002] The present invention relates to the field of Quantum Electronics, and more particularly to the elemental basis of laser technology, and can be used to develop tunable mid-infrared (mid-IR) solid state lasers.
[0003] Primarily, the invention can be used in cases where monochromatic laser emissions tunable in the middle-infrared spectral region are required for solving problems in various fields of science and technology, such as laser spectroscopy, trace gas analysis, photo chemistry, photo biology, medicine, and wavelength specific military applications, among others.
BACKGROUND OF THE INVENTION
[0004] There is a growing demand for affordable mid-infrared sources for use in a variety of applications including atmospheric sensing (global wind sensing and low altitude wind shear detection), eye-safe medical laser sources for non-invasive medical diagnostics, eye-safe laser radar and remote sensing of atmospheric constituents, optical communication, and numerous military applications such as target designation, obstacle avoidance and infrared counter measures. These applications rely on the existence of “spectroscopic fingerprints” of numerous organic molecules in the mid-IR range.
[0005] Recent research advances have spurred considerable effort in the development of practical mid-IR sources. This work has included direct generation in semiconductors using InAsSbP/InAsSb/InAs, 1 and quantum cascade lasers 2 . Mid-IR wavelengths have also been generated using nonlinearities in Optical Parametric Oscillators 3 and difference frequency generators. 4,5 All of these approaches yield tunable sources in the mid-IR and all suffer some fundamental problems that limit their use as robust low cost mid-IR source. Furthermore, to date, all of these sources have limited output powers that preclude their use in higher power applications such as remote sensing.
[0006] In contrast to the relatively large body of work using the approaches described above, there has been relatively little investigation of the potential for direct oscillation from divalent transitional metal ions (TM 2+ ) placed in the asymmetric (T d ) lattice sites of the wide bandgap binary and mixed ternary II-VI semiconductor crystals. The lack of work on direct emission of chromium doped (or other transitional metal doped) sources in the mid-IR has one primary cause. Long wavelength TM emissions are quenched by multi-photon processes in conventional laser host media such as oxide and fluoride crystals, resulting in extremely low room-temperature quantum efficiency of fluorescence.
[0007] Recently, mid-IR laser activity near 2-4 μm was reported for Cr:ZnS 6,7,8,9,10 , Cr:ZnSe 6,7,11,12,13,14,15,16,17,18 , Cr:Cd 1-x Mn x Te 19 , Cr:CdSe 20 , and Fe 2+ :ZnSe 21 crystals. These TM doped II-VI compounds have a wide bandgap and possess several important features that distinguish them from other oxide and fluoride laser crystals. First is the existence of chemically stable divalent TM dopant ions, which substitute Zn 2+ or Cd 2+ host ions, with no need for charge compensation. An additional feature of the II-VI compounds is their tendency to crystallize in tetrahedrally coordinated structures. As opposed to the typical octahedral coordination at the dopant site, tetrahedral coordination gives smaller crystal field splitting, placing the dopant transitions further into the IR. Finally, a key feature of these materials is a poor phonon spectrum that makes them transparent in a wide spectral region, decreases the efficiency of non-radiative decay and gives promise to a high yield of fluorescence at room temperature.
[0008] In terms of merit for high average power applications, it is known that some of chalcogenides (e.g. ZnS and ZnSe) feature excellent thermo-mechanical properties, having thermal shock resistance values comparable to and coefficient of thermal conductivity better than such thermo-mechanically robust materials as YAG crystals. Given the attractive thermo-mechanical, spectroscopic properties of TM 2+ , and nice overlap of the Cr 2+ absorption and emission Er and Tm fiber lasers as well as of stained layer InGaAsP/InP and, theoretically, InGaNAs/GaAs diode lasers, directly fiber or diode-pumped wide band semiconductor crystals doped with TM ions can be considered as very promising and effective systems for medicine, remote sensing, trace gas analysis, and high power wavelength specific military applications.
[0009] The studies of TM 2+ doped II-VI materials showed that in terms of spectroscopic and laser characteristics these media are very close mid-IR analogues of the titanium-doped sapphire (Ti—S). It is anticipated that, similarly to the Ti—S laser, TM 2+ doped chalcogenides will be lasing in the near future with a great variety of possible regimes of oscillations, but with an additional significant advantage of being directly pumpable with radiation of InGaAsP or InGaNAs diode arrays.
[0010] During the last 2-7 years several groups, including the inventors, have actively explored analogues TM 2+ crystal hosts for tunable lasing in CW, free-running long pulse, Q-switched and mode-locked regimes of operation. So far the most impressive results—room temperature operation, >60% lasing efficiency, 3.7 W of output power, more than 1000 nm range of tunability—have been obtained using Cr 2+ :ZnSe crystals. Based on these results, it appears that Cr doped ZnS and ZnSe crystals possess a unique combination of technological, thermo- mechanical, spectroscopic, and laser characteristics that make them potentially low cost, affordable mid-IR laser sources.
[0011] However, in these spectroscopic and laser studies of TM 2+ :II-VI materials there was no indication that microchip lasers and chip-scaled integrated lasers could be designed on the basis of TM doped II-VI hosts. Microchip lasing requires several specific factors in addition to standard factors required for any laser media. These additional factors are high optical density and high gain of thin layers (usually <1-2 mm) of active material, which is translated into high cross sections of absorption and emission, combined with a high doping levels of active ions at which there is still no concentration quenching of fluorescence and no degradation of the optical quality of the host material.
[0012] Also unknown in the prior art is a design of “spatially dispersive” cavities for realization of flexible laser modules easily reprogrammable from monochromatic to ultrabroadband and multiline regimes of operation.
[0013] U.S. Pat. Nos. 5,461,635 and 6,236,666 taught the approach of superbroadband (SBL) or multiwavelength system 22,23,24,25 based on spatial separation of different wavelengths in a single laser cavity. The optical components of the cavity maintain distinct gain channels in the active zone of semiconductor chip, reduce cross talk, suppress mode competition, and force each channel to lase at a specific stabilized wavelength. By designing this cavity structure appropriately, the system creates its own microcavities each lasing at different wavelengths across the complete gain spectrum of the active material. The system is ideal from the point of view of control of laser wavelengths generated in a common laser cavity and allows the obtaining of very small and controllable wavelength spacing. This approach allows the construction of a laser that emits a plurality of narrow spectral lines that can be easily tailored to any pre-assigned spectral composition within the amplification spectrum of the gain medium. This approach has been demonstrated for the emission of thirty lines in laboratory conditions and the stability and line width measurements are extremely promising. Conventional tunable laser systems used for remote sensing are appropriate only for single element analysis. Proposed simple, flexible and easily reprogrammable laser modules open new opportunities for simultaneous multi-element gas tracing analysis. It appears that TM doped II-VI hosts and, specifically, chromium doped ZnS and ZnSe crystals featuring broad amplification spectra are ideal active media for superbroadband and multiline lasing.
[0014] Finally, the prior art has not taught utilization of acousto-optic, electro-optic, photorefractive and birefringent properties of II-VI crystals in one integrated microchip system combining active medium, acousto- or electro-optic modulator, filter, other passive components of the cavity such as waveguide grating, or birefringent filter.
SUMMARY OF THE INVENTION
[0015] The present invention contemplates a new class of middle-infrared microchip lasers based on transitional metal (TM 2+ =Ti, V, Cr, Mn, Fe, Co, Ni, and Cu) doped binary II-VI crystals having formula MeZ, where Me being Zn, Cd, Ca, Mg, Sr, Ba, Hg, Pb and Z being S, Se, Te, O and their mixtures as well as mixed ternary chalcogenide matrixes having formula MeX 2 Z 4 with X being Ga, In, Al. A particular embodiment of this invention is microchip laser based on Cr 2+ doped ZnS, ZnSe, CdS, and CdSe crystals. The microchip laser is the most compact and simplest diode or fiber laser pumped solid state laser with a typical dimension of 0.5-1 mm 3 . The main advantages of the proposed microchip lasers will be the ability to be fabricated with collective fabrication processes allowing low cost mass production with good reproducibility and reliability as well as simplicity, allowing its utilization without any optical alignment and maintenance.
[0016] The following steps are germane to the practice of the invention. Growing (Chemical, Physical Vapor Transport or other methods) or purchasing II-VI host crystal materials from commercial vendors followed by cutting them into polished wafers of thickness 0.1-3 mm.
[0017] Introducing transitional metal (e.g. Cr) thin film of controllable thickness on the crystal facets at the stage after crystal growing by means of pulse laser deposition, plasma sputtering, cathode arc deposition, or other methods,
[0018] Thermal annealing of the crystals under simultaneous action of electric field for effective thermal diffusion of the dopant into the crystal volume with a temperature and exposition time providing highest concentration of the dopant in the volume without degrading laser performance due to scattering and concentration quenching,
[0019] Polishing microchip facets,
[0020] formation of microchip laser by means of direct deposition of mirrors on flat and parallel polished facets of a thin TM:II-VI wafer.
[0021] The microchip laser thus fabricated can utilize direct diode or fiber laser pumping with a level of power density providing formation of positive lens and corresponding cavity stabilization as well as threshold population inversion in the laser material.
[0022] The present invention by taking advantage of acousto-optic, electro-optic, photorefractive and birefringent properties of II-VI crystals also contemplates an integrated microchip system combining active medium, acousto- or electro-optic modulator, filter, other passive components of the cavity such as waveguide grating, or birefringent filter.
[0023] The present invention further contemplates microchip lasers integrated into “spatially dispersive” cavities for realization of flexible laser modules easily reprogrammable from monochromatic to ultrabroadband and multiline regimes of operation.
[0024] The advantages of the present invention will be further appreciated from the drawings and from the detailed description provided below.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] The herein described features of the present invention, as well as others which will become apparent, are attained and can be understood in more detail by reference to the following description and appended drawings, which form a part of this specification. It is to be noted, however, that the appended drawings illustrate only exemplary embodiments of the invention and therefore not be considered limiting of its scope, for the invention may admit other equally effective embodiments.
[0026] FIG. 1 is a flow chart of an embodiment of a three-stage method for producing transitional method doped wafer according to the present invention that will be further diced into numerous microchip active elements.
[0027] FIG. 2 is a graph of room temperature absorption and emission spectra of Cr 2+ :ZnS (A) and Cr 2+ :ZnSe (C) crystals prepared according to the invention, measured at 300K, and plotted in cross-sectional units, and corresponding emission lifetime temperature dependences (B, D).
[0028] FIG. 3 is a graph of room temperature absorption and emission spectra of Cr 2+ :CdS (A) and Cr 2+ :CdSe (C) crystals prepared according to the invention, measured at 300K, and plotted in cross-sectional units, and corresponding emission lifetime temperature dependences (B, D).
[0029] FIG. 4 is a graph of saturation of ground state absorption in Cr 2+ :ZnS crystal. Solid curve is a result of calculation with Frantz-Nodvic equation.
[0030] FIG. 5 is a block-diagram of experimental nonselective hemispherical cavity used for Cr 2+ :ZnS gain switched lasing.
[0031] FIG. 6 is a graph of output-input energies of Cr 2+ :ZnS gain switched laser in hemispherical cavity with 10% output coupler. The measured slope efficiency is 9.5%.
[0032] FIG. 7 is a block-diagram of experimental selective hemispherical cavity with CaF 2 prism dispersive element used for Cr 2+ :ZnS tunable gain switched lasing.
[0033] FIG. 8 is a graph of Cr 2+ :ZnS tuning curve with CaF 2 prism selector. The tuning is limited by the coatings of available cavity optics. Currently tunability from 2050 to 2800 nm is achieved.
[0034] FIG. 9 is a block diagram of experimental set-up for Cr 2+ :ZnS CW lasing under Er fiber laser excitation in external hemispherical cavity.
[0035] FIG. 10 is a graph of output-input characteristics of the Cr 2+ :ZnS continuous wave laser in hemispherical cavity under 1.55 μm Er-fiber laser pumping with different output couplers; (●) T=20%, and (▪) T=2% correspond to minimum threshold adjustment; (▴) T=2%-adjustment to maximum output power.
[0036] FIG. 11 is a block diagram of Cr 2+ :ZnS and Cr 2+ :ZnSe gain switched microchip lasers with no mirrors deposited on the crystal facets.
[0037] FIG. 12 is a graph of output-input energies for gain switched ZnSe microchip laser with no mirrors deposited on the crystal facets. (▴ and ● represent different excitation spots on the crystal).
[0038] FIG. 13 is a block diagram of experimental set-up for Cr 2+ :ZnS and Cr 2+ :ZnSe CW lasing under Er fiber laser excitation in microchip configuration.
[0039] FIG. 14 is a graph of output-input characteristics of the Cr 2+ :ZnS and Cr 2+ :ZnSe continuous wave microchip lasers under 1.55 μm Er-fiber laser pumping.
[0040] FIG. 15 is a graph of output-input curve of the optimized Cr 2+ :ZnS continuous wave microchip laser under 1.55 μm Er-fiber laser pumping.
[0041] FIG. 16 is a graph of the mode structure of the microchip lasers (A) and coupled cavity (B) microchip lasers (with external etalons) for Cr 2+ :ZnS and Cr 2+ :ZnSe crystals.
[0042] FIG. 17 is a block diagram of experimental set-up for microchip output beam divergence measurements combined with a graph of spatial distribution of the output radiation of Cr 2+ :ZnS (red) and Cr 2+ :ZnSe (green) lasers at a distance of L=330 mm from the output laser surfaces.
[0043] FIG. 18 is a block diagram of “spatially dispersive” cavity made from stand alone components for realization of flexible laser module easily reprogrammable from monochromatic to ultrabroadband and multiline regimes of operation.
[0044] FIG. 19 is a block diagram of a chip scale integrated multiline TM:II-VI laser.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0045] In the preferred embodiment, the Cr 2+ :ZnS crystals are prepared by a three-stage method according to a flow chart depicted in FIG. 1 . At the first stage, undoped single crystals are synthesized by a chemical transport reaction from gas phase using an iodine gas transport scheme, preferably in a quartz tube 20mm in diameter and 200mm in length placed in a two heating zone furnace. Powder obtained by a joint ignition of initial components serves as raw material. Temperatures in the zones of raw material and crystallization are approximately 1200° C. and 1100° C. respectively. I 2 concentration is in the range of 2-5 mg/cm 3 . High optical quality unoriented ingots, preferably Ø2×cm 3 , are cut and ground to slabs of 5×5×3 mm size.
[0046] At the second stage and third stages, introduction of chromium (or other transitional metal) into the crystalline host is performed by thermal diffusion (third stage) from a then film deposited, preferably, by the pulse laser deposition method (second stage). Plasma spluttering or other thin-film deposition methods could also be sued. Thermal annealing can be carried out in sealed ampoules under a pressure of, preferably, approximately 10 −5 torr and temperature of approximately 830° to approximately 1100° C. over 3 to 20 days. In some cases to provide more effective thermo-diffusion it was performed under simultaneous action of electric field of 1-30 kV/cm magnitude with positive terminal being applied to Cr film and negative—to the Ag electrode deposited on the opposite surface of the wafer. Polished samples of 1-3 mm thickness and up to 5 mm aperture can then be produced.
[0047] The room-temperature absorption and fluorescence spectra of the studied Cr 2+ :ZnS and Cr 2+ :ZnSe crystals are given in cross section units in FIGS. 2A and 2C , respectively. The absorption spectra were measured using a (Shimadzu UV-VIS-NIR-3101PC) spectrophotometer. The fluorescence spectra were measured using an (Acton Research ARC-300i) spectrometer and a liquid nitrogen cooled (EGG Judson J10D-M204-R04M-60) InSb detector coupled to amplifier (Perry PA050). This InSb detector-amplifier combination featured a temporal resolution of 0.4 μs. The fluorescence spectra were corrected with respect to the spectral sensitivity of the recording system using a tungsten halogen calibration lamp (Oriel 9-2050). As an excitation source we used CW Erbium doped fiber laser (IPG Photonics, ELD-2), modulated at 800 Hz. It is noteworthy that Cr 2+ :ZnSe crystals did not exhibit any polarization dependence of the absorption and the difference due to the polarization dependence of the absorption and fluorescence spectra for Cr:ZnS did not exceed 10% at room temperature. This allowed us to treat the studied crystal in the first approximation as optically isotropic.
[0048] The luminescence kinetics of the crystals were measured at 1950, 2100, 2400, and 2600 nm across a broad temperature range using D 2 and H 2 Raman-shifted Nd:YAG laser excitation at 1560 and 1907 nm. Within the 0.4 μs accuracy of measurements there was no difference in the lifetime of luminescence for different wavelengths of excitation and registration. FIG. 2B shows that the emission lifetime drops only slightly for ZnS, i.e. from 5.7 to 4.3˜s, between 14 and 300° K and is practically unchanged for ZnSe ( FIG. 2D ). This shows that quenching is not important below 300° K.
[0049] The spontaneous-emission cross-sections σ em (λ) ( FIGS. 2A and 2C ) were obtained from fluorescence intensity signal I(λ) using the Fuchtbauer-Ladenburg equation:
σ em ( λ ) = λ 5 I λ ( λ ) A 8 π n 2 c ∫ I λ ( λ ) ⅆ λ , ( 1 )
where A is the spontaneous emission probability from the upper laser level, and n is the index of refraction.
[0050] To derive the absorption cross-section magnitude from the ″absorption spectrum, one needs to know the Cr 2+ concentration. Unfortunately, the absolute dopant concentration is neither uniform nor accurately known in the case of diffusion doping. We therefore used the reciprocity method for the broadband transition:
σ a ( λ ) = σ em ( λ ) g 2 g 1 exp ( hc / λ - E ZFL kT ) ( 2 )
[0051] in conjunction with measured absorption spectra to calculate the absorption cross-section in FIG. 2A , C, making use of the known ground and upper level degeneracies g 1 =3 and g 2 =2, respectively. Here E ZFL is the energy of the zero phonon line of the corresponding transition, k is the Boltzmann constant, and T is the temperature. We also assumed that the Jahn-Teller splitting of both upper ands lower levels can be neglected, as it is less or comparable to kT at room temperature. Our value for the peak absorption cross-section of σ a =1.6×10 −18 cm 2 at λ=1690 nm for Cr 2+ :ZnS agrees reasonably well with the value of σ a =1.0×10 −18 cm 2 known in the prior art and obtained using the absorption coefficient and the known concentration of Cr 2+ .
[0052] Similar graphs of room temperature absorption and emission spectra of Cr 2+ :CdS (A) and Cr 2+ :CdSe (C) crystals prepared according to the invention, measured at 300K, and plotted in cross-sectional units, and corresponding emission lifetime temperature dependences (B, D) are displayed in FIG. 3 .
[0053] One of the important potential applications of TM:II_-VI crystals is the passive Q-switching of the resonators of solid state lasers (e.g. Cr 2+ :ZnS crystals for passive Q-switching of Er:glass lasers). Experiments on saturation of Cr 2+ :ZnS absorption were performed under 1.56 μm excitation. The radiation of a D 2 -Raman-shifted YAG:Nd laser with a pulse duration of 5 ns and pulse energy of up to 20 mJ and repetition rate of 10 Hz was used. Saturation experiments utilized a 2.5 mm thick Cr 2+ :ZnS crystal with initial transmission of T=0.43 at 1.56 μm. The pump radiation was focused on the sample by a 26.5 cm lens and the dependence of the crystal transmission as a function of pumping energy density was measured by means of the sample Z-scanning. Spatial energy distributions of the pump radiation were determined by a standard knife-edge method. The effective radius of the pumping beam was measured at the 0.5 level of maximum pump intensity of radiation.
[0054] As one can see from FIG. 4 , the active absorption changes more than 1.4 times under increasing of pump energy fluence from W=0.8×10 18 to 6.7×10 18 photon/cm 2 . Since the pump pulse duration (5 ns) is much shorter than the relaxation time of Cr 2+ :ZnS saturable absorber (4.5 μs) the saturation behavior was analyzed in terms of energy fluence with a modified Frantz-Nodvik equation for a four level slow absorber. According to this equation the crystal transmission depends on pump energy fluence, “W”, and absorption cross section as follows:
T = 1 z ln ( 1 + T 0 ( e z - 1 ) ) , ( 3 )
where z=W σ ab , T o -initial crystal transition at W=0, and σ abs -absorption cross section (cm 2 ). Equation (3) was solved numerically, and from the best fit to the experimental results ( FIG. 4 , solid line), the value of σ abs (λ=1.56 μm) was estimated to be 0.7×10 18 cm 2 . Taking into account the ratio of absorption at 1.56 μm and in the maximum of absorption band (λ=1.7 μm, see FIG. 2 ) the peak absorption cross section was determined to be 1.4×10 18 cm 2 , which is in a very good agreement with the value of cross section estimated in the current study from spectroscopic measurements.
[0055] The Cr 2+ concentration in the crystal was 3.5×10 18 cm −3 . This satisfactory agreement of σ abs values determined from spectroscopic and saturation measurements indicates negligible excited state absorption losses for Cr 2+ :ZnS at 1.56 μm and the wavelength of Er:glass laser oscillation (1.54 μm). Hence, Cr 2+ :ZnS crystals feature a relatively high cross section of absorption 0.7×10 −18 cm 2 at 1.56 μm compared with 7×10 −21 cm 2 for Er:glass. This value is practically two times larger than 0.27×10 −18 cm 2 cross section value for Cr 2+ :ZnSe known in the prior art and in conjunction with negligible excited state absorption losses reveal possible application of Cr 2+ :ZnS crystals as a promising saturable absorber for resonators of Er:glass lasers. In addition to this it is advantageous to utilize for solid state laser Q switching and mode-locking Cr 2+ :ZnS crystals with dichroic mirrors deposited on their faces. These mirrors are supposed to be transparent at the wavelength of solid state laser (e.g. Er-glass laser) oscillation and reflective in the region of Cr 2+ :ZnS lasing. In this coupled cavity configuration Cr 2+ :ZnS element will serve simultaneously as passive Q-switch or mode-locker, as a load for solid state laser, and as an active element. Due to stimulated processes in Cr 2+ :ZnS one can expect that the effective time of depopulation of Cr 2+ :ZnS excited levels will be much faster than for regular arrangement without coupled cavity. It will result in a shorter pulsed duration in a Q-switch regime and even possibility of mode-locked operation.
[0056] A block-diagram of experimental nonselective hemispherical cavity used for Cr 2+ :ZnS gain switched lasing is depicted in FIG. 5 . Laser experiments were performed using the 1.5607 μm output from a D 2 Raman cell pumped in the backscattering geometry by the 1.064 μm radiation of a Nd:YAG laser. An optical diode was placed before the Raman cell to prevent possible damage of Nd:YAG laser optics by amplified backscattered 1.06 μm radiation. Pump pulses from the Raman cell had pulse duration of 5 ns at FWHM; output energy reached 100 mJ and was continuously attenuated by a combination of a half-wave plate and a Glan prism. Amplitude stability of the pump pulses was about 5%. The hemispherical cavity consisted of the input mirror deposited on the facet of the ZnS crystal and output mirror with 20 cm radius of curvature. Output mirrors had either 10-20% transmission in the spectral region 2.05-2.5 μm, or 20-30% transmission in the spectral region 1.95-2.5 μm. Both mirrors had their peak reflectivity at 2.360 μm. Length of the cavity was 18.5 cm. Pump radiation was focused on the crystal with a 26.5 cm lens placed 22.5 cm before the crystal providing a good match for the pump caustics and the cavity mode size (200 μm). Low doped samples (3-4 cm −1 at 1.7 μm) of 1.7 mm thickness were utilized. The second facet of the crystal was anti-reflection (AR) coated in the lasing region and was fully reflective at the wavelength of pumping, providing a double pass pumping scheme. A Ge filter was used to separate residual pump light from the Cr 2+ :ZnS laser beam.
[0057] Room temperature laser operation was realized with a threshold of 170 μJ and slope efficiency of 9.5% with respect to the pump energy when output coupler R 2.360 μm =90% was utilized. The laser had an output linewidth of approximately 90 nm (FWHM), centered at 2.24 μm and maximum output energy reached 100 μJ. A graph of output-input energies of Cr 2+ :ZnS gain switched laser in hemispherical cavity is depicted in FIG. 6 . Further increase of the pump energy resulted in optical damage of the input mirror. The laser performance of the diffusion doped Cr 2+ :ZnS crystals is expected to be improved by optimization of crystal quality, doping technology and optimization of the output coupler.
[0058] With the R 2.360 μm =80% mirror laser operation was obtained with a threshold of 250 μJ. This allowed a Findlay-Clay calculation of the losses within the cavity 29 . With the crystal length of 1.7 mm and σ abs =0.8×10 −18 cm 2 the losses in the cavity were calculated to be 14.7%. It is felt that this can also be improved by the optimization of the crystal preparation techniques.
[0059] In the wavelength tuning experiment, depicted in FIG. 7 , a hemispherical cavity of the length 19.7 cm was utilized. Wavelength tuning was realized using a CaF 2 Brewster prism as the dispersive element placed 5 cm from the output coupler. The focusing lens and crystal remained at the positions that were used in the nonselective cavity. The output coupler was the 20 cm, R 2.360 μm =90% mirror that was used in the nonselective cavity. This arrangement provided a nice match of the cavity waist and pump beam spot (˜200 μm) in the crystal.
[0060] The pump source was operating at 1.5607 μm with the pulse energy of about 600 μJ and 5 ns pulse duration in a TEM 00 mode. This pump energy was about three times larger than the threshold pump energy level. The Cr 2+ :ZnS laser output was directed through a CaF 2 lens to a 0.3 m “SpectraPro” monochromator with a PbS detector for wavelength measurements. FIG. 8 demonstrates a continuous wavelength tuning that was realized over the 2.05-2.40 μm spectral region.
[0061] The output of the chromium laser oscillation had a linewidth of approximately 30 nm (FWHM). The peak efficiency of the tunable output was centered at 2.25 μm. The tuning limits were due to coatings of the cavity optics and not the emission spectrum of Cr 2+ :ZnS crystal. The use of proper broadband coatings could potentially increase the tuning range to 1.85-2.7 μm.
[0062] The laser output linewidth could be further narrowed by means of a Littrow or Littman configured grating tuned cavity.
[0063] A block diagram of experimental set-up for Cr 2+ :ZnS CW lasing under Er fiber laser excitation in external hemispherical cavity is depicted in FIG. 9 . Pump source was an Erbium Doped Fiber Laser (ELD-2, IPG Photonics). This laser delivers 2W of single mode CW non-polarized radiation at 1550 nm and was equipped with an optical isolator to prevent any possible feedback from the ZnS and ZnSe laser system. The fiber core was 5 μm in diameter. For external non-selective resonator laser experiments, the hemispherical cavity consisted of the flat input mirror and output mirror with 20 cm radius. The input mirror crystal had 99.5% reflectivity in the spectral region from 2.2 to 2.5 μm. The output mirrors had either 2-20% transmission in the spectral region 2.2-2.5 μm, or 20-30% transmission in the spectral region 1.95-2.5 μm. Both output mirrors had their peak reflectivity at 2.360 μm. The antireflection coated chromium doped ZnS crystal with a thickness of 1.1 mm and an absorption coefficient of 5 cm −1 at the pump wavelength was utilized. The crystal was mounted on an optical contact to the input flat dichoric mirror made from the YAG crystal for the sake of effective dissipation of heat. The pump radiation of the Er fiber laser was first collimated with a microscope objective in a parallel pencil of light having 1 mm in diameter, and than focused with a second 15 mm focal length objective into the crystal through the input mirror. The output laser parameters were different when the cavity was adjusted to minimum threshold and maximum output power. The output-input dependences for ZnS:Cr 2+ continuous wave lasing under Er fiber pumping for two different output couplers and for different cavity adjustments to the minimum threshold and maximum output power are depicted in FIG. 10 .
[0064] The minimum threshold values were measured to be 100 mW and 200 mW of absorbed pump power for output couplers with 2% and 20% transmission, respectively. An output power of 63 mW near 2370 nm at an absorbed pump power of 0.6 W was demonstrated with an output coupler with 2% transmission for maximum output power adjustment. The maximum slope efficiency “η” with respect to the absorbed pump power was 18% in this experiment. The round trip passive losses “L d ” in the cavity were estimated to be of 3.7% from the Findley-Clay analysis. The limiting slope efficiency of studied crystal was estimated to be 51% from a Caird analysis of inverse slope efficiency versus inverse output coupling using equation
1 η = 1 η 0 ( 1 + L d T ) , ( 4 )
where η is the slope efficiency, η o is the limiting slope efficiency, and T is the mirror transmission. This value is close to the quantum defect of 65% for the studied crystal.
[0065] A block diagram of Cr 2+ :ZnS and Cr 2+ :ZnSe gain switched microchip lasers with no mirrors deposited on the crystal facets is depicted in FIG. 11 . Gain switched microchip laser experiments were performed with Cr 2+ doped ZnSe and ZnS. The crystal used were 0.5-3 mm thick with polished but uncoated parallel faces and had coefficient of absorption of k˜6 cm −1 at 1.77 μm. Pumping was from the 1.56 μm output of a D 2 Raman shifted Nd:YAG operating at 10 Hz with a pulse duration of about 5 ns and 1.5 mm beam diameter. Output-input energies for pulsed ZnSe microchip lasing for different lasing spots are shown in FIG. 12 . Threshold input energy was found to be 7 mJ. A maximum slope efficiency of 6.5% and maximum output power of 1 mJ were obtained for a microchip without mirrors, when positive feedback was only due to the Fresnel reflections. The spectral range of the free-running laser output was from 2270 to-2290 nm.
[0066] A block diagram of experimental set-up for Cr 2+ :ZnS and Cr 2+ :ZnSe CW lasing under Er fiber laser excitation in microchip configuration is displayed in FIG. 13 . For microchip laser experiments both Cr 2+ :ZnS and Cr 2+ :ZnSe crystals were studied. The crystals were polished flat and parallel (parallelism of ˜10″) to 1.1 and 2.5 mm thickness, respectively. The mirrors were directly deposited on the parallel polished facets of a thin wafer of laser material. Input and output dichroic mirrors had 0.01 and 3.5% transmission over 2300-2500 nm spectral region, respectively, and their transmission at 1550 nm pumping wavelength was 75%. Two different pump arrangements were utilized. The first one was identical to the pump conditions for the Cr 2+ :ZnS CW lasing in hemispherical cavity when the pump radiation of the Er fiber laser was first collimated with a microscope objective in a parallel pencil of light having 1 mm in diameter, and then focused with a second 15 mm focal length objective into the crystal through the input mirror. The second pump arrangement was provided without any additional optics by means of the microchip laser mounting at a close (˜20 um) distance from the tip of the pump Er-fiber laser. In both cases the rather large value of the temperature derivative of the refraction index for ZnS and ZnSe crystals (˜5 times larger than for YAG crystal) played a constructive role by means of creating a strong positive lens and providing effective stabilization of the microchip cavity. FIG. 14 shows the output power of the Cr 2+ :ZnS and Cr 2+ :ZnSe microchip laser plotted as a function of absorbed pump power.
[0067] In a focused pump beam arrangement a laser threshold of 120 mW and a slope efficiency of 53% with respect to the absorbed pump power were realized for Cr 2+ :ZnS microchip laser. High, close to theoretical limit of 65%, slope efficiency of the microchip laser indicates a good quality of the used crystal. The maximum output power of optimized Cr 2+ :ZnS microchip laser reached 150 mW as demonstrated in FIG. 15 .
[0068] In the case of ZnSe microchip lasing in a focused pump beam arrangement a laser threshold of 190 mW and a slope efficiency of 20% with respect to the absorbed pump power were demonstrated. The maximum output power reached 100 mW.
[0069] For the second pump arrangement, when the microchip lasers were directly coupled to the fiber tip laser thresholds of 150 mW and 240 mW and slope efficiencies of 36 and 14% with respect to the absorbed pump power were realized for Cr 2+ :ZnS and Cr 2+ :ZnSe microchip lasers, respectively. The maximum output power of the Cr 2+ :ZnS microchip laser was practically unchanged while it dropped for Cr 2+ :ZnSe by a factor of 1.6 in comparison to the focused pump arrangement. This can be explained by the excessive length and corresponding mismatch in the mode size and pump beam profile of the ZnSe microchip.
[0070] The output spectrum in free-running laser operation covered the spectrum range from 2280 to 2360 and from 2480 to 2590 for ZnS and ZnSe microchip lasers, respectively. At maximum pump power the output spectrum of the Cr 2+ :ZnSe laser consisted of more than 100 axial modes with a free spectral range Δν=0.8 cm −1 . The typical output spectra of the microchip lasers are depicted in the “A” traces of FIG. 16 . Due to a smaller crystal thickness, the free spectral range of the Cr 2+ :ZnS microchip laser was Δν=2 cm −1 and the output spectrum consisted of about 50 axial modes. We attempted to arrange mode control of the microchip lasers by means of a coupled cavity arrangement, with an additional external mirror. The coupled microchip and mirror produced the spectral structure shown in the “B” traces of FIG. 16 . In these experiments the number of axial modes decreased to 18-24 modes (each line in FIG. 16B consists of 3 longitudinal modes) for both lasers. This can be further decreased to a single longitudinal mode oscillation in a double cavity configuration using a narrowband output coupler. This experiment demonstrates a feasibility of the microchip single longitudinal mode lasing using a selective output coupler in a combination with the external etalon.
[0071] FIG. 17 displays a block diagram of experimental set-up for microchip output beam divergence measurements combined with a graph of spatial distribution of the output radiation of Cr 2+ :ZnS (red) and Cr 2+ :ZnSe (green) lasers at a distance of L=330 mm from output laser surfaces. As one can see, a 18 mrad FWHM of the intensity profile was measured for the Cr 2+ :ZnS laser. It is slightly less than that for Cr 2+ :ZnSe laser ( 25 mrad). Taking thermal effects, that are responsible for cavity stabilization, into account, the divergence difference may be explained by a lower dn/dT in Cr 2+ :ZnS crystal (+46×10 −6 K −1 in ZnS vs. +70×10 −6 K −1 in ZnSe).
[0072] The proposed approach of superbroadband/multiwavelength (SBML) system is based on spatial separation of different wavelengths in a single laser cavity. In that regard the teachings of U.S Pat. Nos. 5,461,635 and 6,236,666 are incorporated herein by reference. The basic optical scheme of the laser transmitter is shown in FIG. 18 .
[0073] The laser operates as follows. Emission from the spatially separated channels of the active medium passes through the intracavity lens into the off-axis mode suppression element, aperture A, which together with the spatially filtered pump radiation divides active zone of the gain waveguide into a number of channels and separates from the amplified emission of individual channel only part of it that is spread parallel to the resonator axis. This separated radiation is diffracted on the diffraction grating. The Littrow mount grating works as a retroreflector in the auto-collimating regime in the first order of diffraction and returns part of radiation back to the aperture. The off-axis mode suppression element, aperture, in turn extracts from the diffracted radiation only the radiation of the main laser modes. Secondary laser modes, which diverge from the optical axes, are expelled from the process of generation. Hence, the aperture should simultaneously select the fundamental transverse modes for all existing channels in the cavity. The radiation of the main laser modes, each with a distinct wavelength, is collimated by the focusing lens and directed back to the active medium. As FIG. 18 shows, the optical components of the cavity maintain distinct gain channels in the active zone of active element, reduce cross talk, suppress mode competition, and force each channel to lase at specific stabilized wavelength. This approach allows the construction of the laser that emits a plurality of narrow spectral lines that can be easily tailored to any pre-assigned spectral composition within the amplification spectrum of the gain medium. We believe that TM doped II-VI hosts and, specifically, chromium doped ZnS and ZnSe crystals featuring broad amplification spectra are ideal active media for superbroadband and multiline lasing.
[0074] There are different schemes that can provide single longitudinal mode operation of Ii-VI microchip laser coupled to external etalon cavity in combination with narrowband output coupler, fiber grating butt- coupling, external grating, hybridly coupled phase array demultiplexer, and waveguide grating mirror.
[0075] FIG. 19 displays further chip scale integration of multiline TM:II-VI laser. This integrated optical chip is made on II-VI substrate. The chip consists of several sections. The right section has multiple V-grooves etched in II-VI substrate and is provided for connection with fiber lasers or fiber coupled diode lasers. Central section consists of multiple waveguides (e.g. made by ion exchange or ridge technology) and provides delivery of the pump radiation to the active section. The active section consists of multiple II-VI waveguides doped with TM 2+ and can be further combined with dispersive element such as a tapered grating. Tapered grating, for example, can be provided by exposing active waveguides with UV interference pattern. Utilization of tapered grating provides an autocollimation regime of retroreflection for different wavelengths for each individual active waveguide giving rise to a multifrequency regime of oscillation. Due to electro-optic properties of II-VI materials it is possible to integrate Mach-Zehnder or electro-reflection internal modulator with the active section of the same waveguide (not shown on the Figure). Output multifrequency radiation can be coupled to an output fiber.
[0076] There are many other possible schemes of utilization of acousto-optic, electro-optic, photorefractive and birefringent properties of II-VI crystals in one integrated microchip system combining active medium, acousto- or electro-optic modulator, filter, other passive components of the cavity.
[0077] While our invention has been disclosed in various forms, this disclosure is not to be construed as limiting the invention solely to these forms, rather the invention is limited solely by the breadth of the claims appended hereto.
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24. I. Moskalev, S. Mirov, V. Fedorov, T. Basiev, G. Grimes, E. Berman, “External cavity multiline semiconductor laser for WDM applications” in In-Plane Semiconductor Lasers V, Like J. Mawst and Ramon Martinelli, Editors, Proc. SPIE 4287, 128-137 (2001).
25. T. T. Basiev, P. G. Zverev, V. F. Fedorov, S. B. Mirov (April 1997) Multiline, superbroadband and sun-color oscillation of LiF:F 2 − color center laser, Applied Optics, 36, 2515-2522 (1997).
26. G. Grebe and H. J. Schulz, “Luminescence of Cr 2+ centers and related optical interactions involving crystal field levels of chromium ions in zinc sulfide”, Z. Naturforsch 29a 1803-1818 (1974).
27. C. S. Kelley and F. Williams, Phys. Rev. B, 2, 3-8 (1970).
28. A. V. Podlipensky, V. G. Shcherbitsky, N. V. Kuleshov, V. P. Mikhailov, V. I. Levchenko, and V. N. Yakimovich, “Cr 2+ :ZnSe and Co 2+ :ZnSe saturable-absorber Q switches for 1.54-μm Er:glass lasers,” Opt. Lett. 24/14, 960-962 (1999).
29. D. Findlay and R. A. Clay, “The Measurement of Internal Losses in 4-Level Lasers”, Phys. Lett 20/3, 277-278 (1966).
30. J. A. Caird, S. A. Payne, P. R. Staver, A. J. Ramponi, L. L. Chase, W. F. Krupke, IEEE J. Quantum Electron QE-24, 1077 (1988).
31. J. Izawa, H. Nakajima, H. Hara, Y. Arimoto, “A tunable and longitudinal mode oscillation of a Tm, Ho:YLF microchip laser using an external etalon,” Optics Commun., 180, 137-140 (2000).
32. N. Vasa, P. Husayin, M. Kidosaki, T. Okada, M. Maeda, T. Mizunami, “Fiber grating butt-coupled cw Cr 3+ :LiSrAlF 6 laser performance,” in Conference on Lasers and Electro - Optics , Vol. 6, 1998, OSA Technical Digest series (Optical Society of America, Washington D.C., 1998) pp. 67-68.
33. D. V. Thourhout, A. V. Hove, T. V. Caenegem, K. Vandeputte, P. Vandaele, I. Moerman, X. Leijtens, M. K. Smit, R. Baets, “Realization of a Phased-Array Multi-Wavelength laser using hybridly integrated PICs”, in 2000 Electronic Components and Technology Conference, 1266-1271, 2000.
35. I. Avrutsky, R. Rabady, “Waveguide grating mirror for large-area semiconductor lasers”, Opt. Letts., 26, 989-991 (2001).
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A method of fabrication of laser gain material and utilization of such media includes the steps of introducing a transitional metal, preferably Cr 2+ thin film of controllable thickness on the ZnS crystal facets after crystal growth by means of pulse laser deposition or plasma sputtering, thermal annealing of the crystals for effective thermal diffusion of the dopant into the crystal volume with a temperature and exposition time providing the highest concentration of the dopant in the volume without degrading laser performance due to scattering and concentration quenching, and formation of a microchip laser either by means of direct deposition of mirrors on flat and parallel polished facets of a thin Cr:ZnS wafer or by relying on the internal reflectance of such facets. The gain material is susceptible to utilization of direct diode or fiber laser pumping of a microchip laser with a level of power density providing formation of positive lens and corresponding cavity stabilization as well as threshold population inversion in the laser material. Multiple applications of the laser material are contemplated in the invention.
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CROSS REFERENCE TO RELATED APPLICATION
This application claims the benefit of U.S. Provisional Application No. 60/004,793, filed Oct. 2, 1995, entitled, "High Density Perforating Gun System," further identified by Attorney Docket No. 0750F-016.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to through tubing perforation guns used to support explosive charges in a borehole to form perforations through which water, petroleum or minerals are produced.
2. Background Information
This invention is an improvement to phased, through tubing, perforating systems in that it allows for a high shot density of directional shaped charges in a phased orientation between about 135 and 145 degrees.
Standard sizes for perforating systems for completing wells in 7 inch casing range from 47/16ths inches outside diameter to 51/4th inches outside diameter. The typical wall thickness for the carrier tube is from 3/8ths of an inch to 7/16ths of an inch. The most common perforating gun systems for gravel pack completions in 7 inch casing have 41/2 inch outside diameters with 12 shots per foot. The systems are typically phased with 135 degrees rotation between shots and therefore will have eight rows of shots in the casing. The standard size hole that the most common perforating guns make in the casing is about 0.70 of an inch in diameter. There is a need to perforate the casing with a higher shot density than 12 shots per foot. It is desirable to shoot as many holes per foot as possible into the casing, so long as the size of each hole does not drop below 0.70 of an inch in diameter. It is also desirable to be able to shoot a shaped charge made of zinc alloy so that the undesirable debris from the system is reduced. This need should be fullfilled with a perforation gun that achieves a high density of perforations in a manner that does not weaken the performance of the gun or the structural integrity of the gun or the casing.
SUMMARY OF THE INVENTION
The general object of the invention is to provide a gun for well perforating that overcomes the various disadvantages of the prior art devices. The present invention is a 41/2 inch diameter, 18 shot per foot gun that produces an actual hole size in the casing of at least 0.70 of an inch in diameter with a zinc alloy charge case or steel charge case. This performance is accomplished by shooting sequentially with a phasing of between about 135 and 145 degrees between shots with a shaped charge liner diameter of 1.690 inches or larger. This 135 to 145 degree phasing provides for 18 rows of shot in the casing. The present invention produces 50 percent more flow area than the conventional 41/2 inch, 12 shot per foot system in a 7 inch diameter casing.
The 135 to 145 degree phasing makes the 18 shot per foot shot density possible with the given liner size and carrier tube inside diameter. It minimizes the loss in casing strength since the holes made in the casing by the shaped charges are about 12 inches apart vertically, as opposed to the prior art 135 degree phasing which results in a vertical separation between shots of only about 5.33 inches.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross-sectional view showing a shaped charge positioned in a perforating gun;
FIG. 2 is a schematic assembly of a plurality of shaped charges mounted in a charge holder tube in a high shot density fashion according to the invention; and
FIG. 3 is a side elevational view of the carrier tube with a plurality of apertures phased between 135 and 145 degrees to receive shaped charges.
DETAILED DESCRIPTION OF THE INVENTION
Referring initially to FIG. 1 of the drawings, numeral 11 illustrates a tubular high density perforating gun system of the present invention with a carrier housing tube 17 having an interior annular surface 15 and an exterior annular surface 13. The outside diameter of the carrier housing tube 17 is preferably between 47/16ths and 51/4th inches. The charge holder tube 19 has an exterior annular surface 21 and an interior annular surface 23 that forms a concentric cylinder and is generally coaxial with the carrier housing tube 17 and is located within the carrier housing tube 17. The diameter of the annular outside surface 21 of the charge holder tube 19 is such that an annular space 25 is created between the annular outer surface 21 of charge holder tube 19 and the annular inner surface 15 of the carrier housing tube 17.
The numeral 27 designates a shaped charge having a frusto-conical charge case 29 with an interior surface 31. The charge case 29 is preferably manufactured from a zinc alloy with similar composition and properties as ZA-5 (No. 5) described in publications by the American Die Casters Association and commercially available. A frusto-conical charge liner 43 has an explosive material retaining wall 33 with an exterior surface 35. Charge liner 43 is attached at its base 34 to the base 36 of the charge case 29 and extends into the conical space of the charge case 29. The diameter of the base 34 of the charge liner 43 is at least about 1.690 inches. A firing plate 37 with an exterior surface 39 forms the nose of the explosive material retaining wall 33 of the charge liner 43. Shaped explosive 41 is located in the area prescribed by the interior surface 31 of the charge case 29, the exterior surface 35 of the explosive material retaining wall 33, and the exterior surface 39 of the firing plate 37. An annular fastener ring 45 is located near the base 36 of the charge case 29 and extends radially outward.
Located at the nose of the charge case 29 is a plurality of ears 47 which extend outwardly from the charge case 29 in a parallel fashion to receive a primer cord 49. The length from the base 34 of the charge liner 43 to the ears 47 is such that the axis (not shown) of the primer cord 49 is located slightly off center, preferably about 20/1,000ths of an inch, of the charge holder tube 19, thereby allowing a snug fit of the primer cord 49 within the ears 47 when the primer cord 49 is put in tension upon assembly. The primer cord 49 is conducively attached to an electrical means (not shown) to sequentially fire the shaped charges 27. This off center assembly of the primer cord 49 in tension assures an electrically conducive contact between the primer cord 49 and the shaped explosive 41 and alleviates the need for clips or additional means of retaining the primer cord 49 in contact with the shaped explosive 41. This off center assembly of the primer cord 49 also prevents loss of performance of the shaped charges 27 due to charge interference or nonsequential firing.
A carrier housing tube bore 51, with an axis (not shown) which is perpendicular to the axis of the carrier housing tube 17, is located on the carrier housing tube 17 of the perforating gun 11, and has a diameter slightly less than that of the base 34 of the charge liner 43. The carrier housing tube bore 51 extends to a depth about half way through the carrier housing tube 17 from the outside edge 13 of the carrier housing tube 17 leaving a selected unbreached portion 54 in the carrier housing tube 17.
Referring now to FIG. 2 and FIG. 3 in the drawings, a plurality of shaped charges 27, in schematic here, are shown assembled in the charge holder tube 19 in phase between about 135 and 145 degrees. In the preferred embodiment, a plurality of apertures 52 are milled with a phasing between about 135 and 145 degrees through a tube, preferably a drawn over mandrel (DOM) tube, by a multiple axes laser milling machine or any other device known in the art for milling apertures in tubes. Fastener ring slots 53 are cut by a laser milling machine, or any other device known in the art, into the the top and bottom edges of the apertures 52 in the charge holder tube 19 to receive the fastener ring 45 of the shaped charges 27.
The shaped charges 27 are inserted into the charge holder tube 19 and held in place by the fastener rings 45 with a pressure fit into the fastener ring slots 53. The primer cord 49 is fed through the ears 47 of the charge case 29. The charge holder tube 19 with the attached shaped charges 27, located in phase about the charge holder tube 19 between about 135 and 145 degrees, and at a shot density of at least 18 shots per foot, is inserted into the carrier housing tube 17 and attached thereto by connector means (not shown).
The carrier housing tube bores 51 are milled into the carrier housing tube 17 in phase between about 135 and 145 degrees by means commonly known in the art. The carrier housing tube bores 51 are aligned with the charge liners 43 such that the unbreached portions 54 of the carrier housing tube 17 are located in front of the charge liners 43. The thus assembled perforating gun 11 is then attached to an upper end connector (not shown) for mounting on a conveyance sub (not shown) to raise or lower and position the perforating gun 11 at the selected position in the well adjacent to the geological formation to be perforated.
Upon detonation, the unbreached portion 54 of the carrier housing tube 17 is burned through first. Perforations are made through the casing and the diameter of at least selected perforations in the casing is at least 0.70 inches.
In an alternate embodiment, the high density perforating gun 11 has a carrier housing tube 17 with an outside diameter between about 61/2 and 71/2 inches. The base 34 of the charge liner 43 has a diameter of at least about 2.500 inches. The shaped explosives 41 of this alternate embodiment are configured such that the diameter of at least selected perforations is at least 1.00 inch, and the shot density is at least 18 shots per foot.
It should be apparent from the foregoing that an invention having significant advantages has been provided. The high density perforating gun system 11 is configured to enable the orientation of shaped charges 27 in phase between about 135 and 145 degrees as shown in FIGS. 1-3 in which the carrier housing tube 19 is used to position the shaped charge 27 and others like it to form perforations in the casing and into the geological formation. Moreover, the high density perforating gun system 11 when constructed as indicated above, allows at least 18 shots per foot into the geological formation in a manner that does not weaken the performance of the perforating gun 11 or the structural integrity of the gun assembly or the casing.
While the invention is shown in only one of its forms, it is not just limited but is susceptible to various changes and modifications without departing from the spirit thereof.
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A high density perforating gun having a carrier housing tube and an interior charge holder tube through which are mounted zinc alloy shaped charges in a phased relationship between about 135 and 145 degrees. The 135 to 145 degree phased relationship provides for an 18 shot per foot perforating gun system. The shaped charges of selected length are inserted into the carrier housing tube and held in place by fastener rings fitted to fastener ring slots. The nose ends of the shaped charges are fitted with ears to receive a detonating cord. This positions the primer cord in tension and generally coaxially with the carrier housing tube to prevent charge interference and assure sequential detonation.
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BACKGROUND OF THE INVENTION
The subject invention discloses a method and means of tufting in which different pile heights may be obtained on conventional tufting machines by a modified yarn feed process. With more particularity, in conventional tufting, standard needles are driven through a backing layer by one of many types of needle drives to enable loops of yarn to be deposited in the backing layer and held in place by a looper positioned below the backing layer as the tufting needles withdraw. Each needle receives a single strand of yarn and the size of the loop formed will be determined by the amount of yarn fed during the tufting cycle.
Presently, two-pile height (or additional pile heights) tufting is known; however, the systems utilized for such tufting are quite complex. Typically, all yarn being delivered to the different needles is delivered by one of a number of feed rolls, each of such rolls being driven by magnetic clutches which connect each of the feed rolls to one of a number of shafts. The shafts are set to run at different speeds and thus, the feed roll speed is varied by controlling the clutches. Such machinery with large clutches and associated gears is quite cumbersome and, accordingly, patterns for the carpets are limited to a realistic number of repeats across the width of each tufted carpet.
Typically, there are ten such repeats across a standard width of carpet which means that the same pattern will be repeated in ten different places across the carpet. Since in each pattern one needle will function identically to a corresponding needle in each of the other repeats, yarns for each of these needles which produce identical patterns will be fed by a common feed roll. Thus, from any one feed roll, yarn will be fed to needles positioned across the width of the carpet. For example, if there are 1200 needles and 10 repeats, the chosen pattern would be 120 needles wide with needles Nos. 1, 121, 241, 361, 481, 601, 721, 841, 961, and 1081, all extending to the same feed roll since each of these needles represent or will tuft the first row of each of the ten repeating patterns.
It can be appreciated that the yarn strands which extend from a single feed roll to needles at different locations will be of different lengths which gives rise to tensioning problems. In present patterning machines where varying pile height capability is present, the deficiency in supplying yarn of varying tensions is partially overcome by carefully routing yarns from each feed roll to the respective needles in such a manner that the visible effect caused by the relative distance factors is minimized. Tubing commonly used for this type of routing is known as scramble tubes. Even with the use of scramble tubes, it is difficult to achieve the yarn tension control in a high-low patterning machine on the order of that achieved by a conventional non-patterning machine where the yarns can be fed directly from the feed roll to the needles without having to be routed in different directions as for example, some yarns in the two pile height patterning machine end up being routed diagonally from one end of the machine to the other.
A second detrimental aspect to present day, conventional high-low patterning is attributable to the fact that the clutch response is not instantaneous and since the distances from the feed roll may be as great as the width of the carpet, the pile height change does not occur completely until several cycles after the clutches are switched. It will be recognized that with this deficiency, the achievement of a clear pattern is difficult.
In conventional patterning high-low machines, in an effort to eliminate the difference in tension stretch in the yarns, accordingly, to produce a better defined pattern, rolls commonly known as pull rolls are utilized and located below the scramble tube bank. Presumably, all of the yarn is placed under tension in such a manner that the tension is presumably equalized. In practice, the result is far from an optimum one and weak yarns are likely to break at a weak point or a bad splice in the yarn.
Furthermore, with conventional patterning tufting machines, the limitation of a number of repeats, for example, 10, obviously limits the type of patterns which can be tufted. In machines heretofore used, there has been no commercially feasible way to control the height of each tuft of each tufting needle throughout the carpet.
Various principles utilized and some of the apparatus discussed herein are the subject matter of copending Application Ser. No. 699,905. Somewhat related subject matter is disclosed in co-pending Application Ser. Nos. 699,904 and 700,413.
SUMMARY OF THE INVENTION
In accordance with the subject invention, the apparatus and method disclosed herein provide a means of improving upon yarn feed for conventional high-low pattern tufting. Cumbersome, complex machinery used in the past can be eliminated and, because of a more direct path of yarn travel, many of the disadvantages of present day high-low pattern tufting which cause the production of poor quality carpets can be eliminated.
In place of the feed roll patterning concept and the requisite divergent yarn feeding, the subject invention utilizes a yarn pulling and clamping technique which is facilitated by individually actuatable band driven pullers which engage the yarn and meter and feed it directly to needles without the necessity of scramble tubes and pull rolls.
In a preferred embodiment, for each needle, a first yarn puller extends from a band-like member that is continuously driven by an oscillating shaft and upon each reciprocation of the band-like member, a length of yarn is drawn from the yarn creel. This yarn length may then be selectively advanced by any one of a plurality of yarn pullers which will advance only the desired amount of yarn. In the preferred embodiment, two such yarn pullers are shown and they are controlled in such manner that the deactuation of one yarn puller causes the actuation of the other yarn puller so that one of two pile heights will always be selected. Once this selection has been made, the yarn is clamped to prohibit additional yarn from being pulled from either the creel or a first yarn pocket where the yarn puller deposits the yarn drawn from the creel. Upon release of further clamping means, the selected, metered length of yarn can then be advanced to the tufting needle with the yarn under uniform tension with other yarns.
Further in accordance with the subject invention, the yarn pullers may be driven by thin band-like members, preferably constructed of steel, which are in turn driven by adjustable-stroke oscillatory shafts. These can be on the order as disclosed in co-pending Application U.S. Ser. No. 699,905. The bands extend tangentially from their respective shafts and are restrained in groove-like structure so that the path of the band is kept straight once it leaves the shaft. The yarn puller or plunger elements are secured to the bands at ends remote from the band end which is engageable by the oscillating shaft.
In the case of the yarn puller which initially pulls yarn from the creel (since this is a continually reciprocating puller) the band is continuously engaged by the oscillating shaft.
In the case of the selectable yarn metering pullers, if two such pullers are used, they may be connected to bands which are engageable with their respective shafts and which may be driven into or allowed to disengage from their respective shafts by the same control means. This may be a plunger which reciprocates to the right and left as driven by a solenoid or other means. Accordingly, upon receiving a pulse, the solenoid may cause the plunger to engage one of the bands with its oscillating shaft. Upon deenergization of the solenoid, the plunger will return to its rest position and, in so doing, will cause the first band to disengage with its driving shaft while causing a second band to be driven into engagement with its oscillating shaft. The shafts oscillate continually but only drive the bands when the bands are driven into engagement by the solenoid plunger means.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more detailed understanding of the invention, reference is made in the following description to the accompanying drawings in which:
FIG. 1 is a schematic view showing conventional tufting apparatus, together with the improved yarn feeding system;
FIG. 1A is an isometric view showing a yarn clamp;
FIG. 2 is an isometric cut-away view showing an oscillatory member and band actuation structure;
FIG. 3 is a cross-sectional plan view of the mechanism of FIG. 2 with a solenoid plunger in a deactuation position;
FIG. 4 is a cross-sectional plan view of the mechanism of FIG. 2 with the solenoid plunger shown in its actuating position;
FIG. 5 is an isometric view showing band structure utilized in the subject invention;
FIG. 6 is an isometric view showing shaft structure together with a solenoid actuation means;
FIG. 7 is an isometric cut-away view showing housing structure together with shaft and plunger receptacles and the yarn channel;
FIG. 8 is a cut-away cross-sectional view taken along lines 8--8 of FIG. 9;
FIG. 9 shows the subject yarn feeding and metering system and is the first of a series of sequential drawings showing feeding and metering steps;
FIG. 10 is the second of a series of sequential views;
FIG. 11 is the third of a series of sequential views; and
FIG. 12 is the fourth of a series of sequential views.
DETAILED DESCRIPTION
With reference to FIG. 1, conventional tufting equipment is shown schematically to which has been added the yarn feeding and metering system herein disclosed. The yarn feeding and metering components are shown schematically housed in unit housing 10. A feeding shaft 11 and two metering shafts, 12 and 13, are shown. A yarn passageway 14 extends from the creel (not shown) at the top of the figure to a point in closer proximity to the tufting station. Plunger channels 15, 16 and 17 are shown extending from shafts 11, 12 and 13, the purpose for which will be described subsequently. A solenoid actuator 19 is shown which, through appropriate linkage, will cause bands (not shown) to be engaged by shafts 12 and 13 as will also be described subsequently. Clamps 20, 21 and 22 are shown positioned along yarn passageway 14 and are used to clamp yarn extending through the passageway at intervals throughout the yarn feeding and metering process.
The remainder of the tufting unit of FIG. 1 represents a conventional tufting machine in which yarn S extends to the needle in much the same fashion as would be found in conventional non-patterning machines. A frame 30 is shown supporting the needle structure. A needle stroke shaft 32 is journalled within frame structure 30 and an eccentric 34 is secured to shaft 32 and actuates connecting rod 36. The connecting rod 36 is secured to push rod 38 which, in turn, is secured to needle 40. A needle yarn guide 42 forms the lowermost guide for the yarn strand S and additional yarn guides 44, 46 and 48 are shown as being secured to frame structure 30.
A backing layer L onto which yarn is tufted is fed to take-up roll 50 over backing guide 52 from feed roll 54 and idler roll 56. Feed roll 54 is driven by the ratchet 58 and pawl 60 drive which is controlled through linkage 61 by eccentric 62. A backing support 64 is shown, below which looper 66 is positioned to engage loops as they are tufted by needle 40. The looper 66 is driven by eccentric 70 through linkage 68.
While not shown, it is to be understood that a motor through suitable transmission apparatus will drive the various drive mechanisms such as eccentrics 70, 62 and 34 which drive various portions of the apparatus.
Having briefly described elements of the subject invention generally, these elements and their components will now be described in detail.
Yarn pullers or metering members which reciprocate within channels 16 and 17 are driven by bands which are engaged by shafts 12 and 13. As will be seen from FIG. 9, band-like member or ribbon 24 is engageable with shaft 12 and drives puller or plunger 28 in channel 16 and band-like member or ribbon 25 is engageable with shaft 13 and drives puller or plunger 29 in channel or pocket 17.
With reference to FIG. 1A, a clamp 20 is shown and it is to be understood that the same structure may be used for clamps 21 and 22. Clamp 20 comprises an inner solid cylindrical member 72 through which diametric bores 74 are made for yarn strands S. An outer cylindrical sleeve 76 has bores 78 alignable with the bores 74 of the inner solid cylindrical member 72. Relative motion between member 72 and sleeve 76 will cause the yarn to be clamped although movement cannot be so great as to shear the yarn strands. Each of the yarn strands S is fed through a separate feeding unit to a different needle 40 as will be clear from the following description.
With reference to FIGS. 2-4, the mechanism which causes the engagement of band 24 (which drives the puller in channel 16) by means of oscillating drive shaft or tube 12 is shown. The band or ribbon is contained in channel 18 and while it may slide, it will not bend when subjected to compression forces. As will be seen from FIGS. 5 and 9, the band or ribbon 24 extends to plunger 28 which is in the stationary channel 16 (see FIG. 1) below the oscillatory shaft 12. The band or ribbon 24 thus extends upwardly from plunger 28 around the shaft 12 for approximately 180° and terminates in a shoe 114. As can be seen from the partial view in FIG. 2, shaft 12 closely fits within a cavity formed in housing 10 and groove 18 which carries band 24 in actually the shallowest of three grooves or notches in shaft 12. Shoe 114 is positioned within intermediate groove 116 which extends partially around the shaft. A third deeper notch or groove 118 has a purpose which will be described subsequently.
The shoe 114 may be welded, soldered or otherwise attached to band or ribbon 24. A drive spring 120 is welded or soldered or otherwise attached to the base of shoe 114 and extends along part of the distance of shoe 114. It will be noted that the ribbon or band 24 has a portion of its center cut out to give a lanced out tab 122, (see FIG. 5). The shoe 114 has a cavity 124 in which is contained a compressible pin 126 which bears against drive spring 120 and which extends through the lanced out portion of band or ribbon 24. The compressible pin 126 may be constructed of a rubber-like substance. A stop member 128 is rigidly secured to and embedded within housing structure 10. The left tip of actuation pin 100 is shown in its non-energized position in FIGS. 2 and 3. When plunger or actuation pin 100 is as shown in FIGS. 2 and 3, the ribbon or band-like member 24 is held out of action due to the interference of lanced out tab 122 with surface 130 of housing 10. The band or ribbon 24 is prevented from being driven in a clockwise direction by stop member 128 as can be seen in FIGS. 2 and 3.
When a particular pile height is to be selected and hence the band or ribbon 24 of that unit is to be actuated, the plunger or actuation pin 100 is advanced thus unlatching spring 122 from surface 130. As spring 122 is unlatched, it applies pressure to the compressible pin 126 which, in turn, depresses the drive spring 120. As can be seen best in FIG. 3, the drive spring 120 is attached to only one end of shoe 114 and thus can be driven outwardly from the shoe by compressible pin 126 if permitted by the notch structure of shaft 12. As the shaft oscillates, it will reach the position as shown in FIG. 3 at which time the compressible pin 126 will force the lower end of drive spring 120 into engagement with notch 118. As the shaft 12 reverses, drive spring 120 will be driven in the counterclockwise direction, thus driving band member 24. As the band or ribbon 24 advances the lanced out portion or tab 122 of the ribbon or band 24 becomes trapped within groove 18 formed between the shaft and the stationary housing 10 (as seen in FIG. 4) with the drive spring 120 being held in its drive position.
Thus, as can be seen in FIG. 4, the band or ribbon 24 is driven as far as the oscillatory motion of the shaft carries it since the drive spring 120 is engaged in the driving or deepest notch 118. As this counterclockwise motion of band 24 occurs, it will be appreciated that plunger 28 of FIG. 9 is driven downwardly within pocket or plunger channel 16 and will, as will be described, be engaging yarn.
As the shaft 12 oscillates in a clockwise direction, surface 155 of shaft 12 engages surface 157 of shoe 114 whereby band 24 will be returned to its unactuated position and if actuation pin 100 has been deactivated by the solenoid means, then the lanced out tab 122 will be permitted to return to its position where it abuts against surface 130. Compressible pin 126 will, accordingly, be permitted to release its pressure against drive spring 120 which will return to its non-driving position in juxtaposition against shoe 114 and out of engagement with notch 118. Thus, the next time the shaft 12 oscillates in a counterclockwise direction, the band 24 will remain in its stationary non-actuated position. On the other hand, if the same height is to be called for a second time in succession, the solenoid is left alone and the actuation pin or plunger 100 remains in the position as shown in FIG. 4 thus causing the band 24 to be driven by oscillating shaft 12 for a second cycle.
With reference to FIG. 5, the bands 24 and 25 are shown in isometric views and are shown attached to yarn pullers or plungers 28 and 29, respectively. Engagement elements such as shoe 114, drive spring 120 and lanced out tab 122 are shown by identical numerals on each of the bands 24 and 25.
With reference to FIG. 6, shafts 12 and 13 are shown in isometric views together with the solenoid actuation unit. The solenoid 92 is shown operatively connected to plunger or actuation pin 100 by intermediate elements 94, 96 and 98. As can be seen, the actuation pin 100 is placed so that when in the off condition, the plunger 100 is biased by spring 102 to the right to cause engagement with the structure to the right. This means band 25 will be forced into engagement with shaft 13. When the solenoid 92 is actuated, the spring biasing 102 will be overcome and actuation pin 100 will disengage from the structure to the right and cause the engagement of band 24 with shaft 12 to the left of the plunger 100. As can be seen from the perspective in FIG. 6, actuation pins 100 can be placed side-by-side although each succeeding unit is independently actuable through its own solenoid unit.
With reference to FIG. 7, a portion of housing 10 is shown. In particular, cavity 200 which houses clamp 21 and cavity 202 which houses clamp 22 are each along yarn passageway 14. Plunger channels 16, 17 intersect passageway 14 and house plungers 28 and 29 respectively. Each plunger channel or pocket 16 and 17 has a vertical groove 208 and 210, respectively. The edges of bands 24 and 25 are inserted and confined within the vertical grooves 208 and 210, respectively to confine the bands in a linear direction as they extend tangentially outward from the shafts 12 and 13, respectively. By restraining bands 23, 24 and 25 as will be discussed, the oscillatory motion of the shafts can be translated to reciprocable motion of plungers 27, 28 and 29. Shafts 12 and 13 are housed in cavities 212 and 214, respectively, while plunger 100 reciprocates in cavity 216 which extends upwardly as well to house linkage member 98.
With reference to FIG. 8, a cross-sectional view is taken in channel 15 looking down from the above plunger 27. As can be seen, the band 23 is secured within channels to prevent any bending or deformation of the band.
With reference to FIG. 9, a more detailed view of the yarn feeding and metering apparatus is disclosed. Yarn comes from a creel (not shown) to the left of the apparatus and extends through passageway 14 (through the housing) to guides 44, 46 and 48 (see FIG. 1) and subsequently to the needles 40. As can be seen in FIG. 9, oscillating shaft 11 drives band 23 to which plunger 27 is connected. Since plunger 27 reciprocates to draw a length of yarn from the creel for each cycle, it is not necessary to have an engaging mechanism as disclosed in FIGS. 2-4 since the band 23 may be held in continuous engagement with oscillating shaft 11 by any convenient means of attachment such as rivet, screw or other common fastener. To the right of shaft 11, shafts 12 and 13 are shown which are adjustable in their oscillatory amplitude to carry out the metering function. Bands 24 and 25 are shown extending to yarn plungers or pullers 28 and 29, respectively. The yarn pullers or metering members 28 and 29 are designed to penetrate downwardly to different levels, thereby providing different metering capabilities and, accordingly, a different height pile is obtained depending upon which unit is chosen. As will be seen, when plunger 28 is chosen, it will descend to a previously adjusted level so that most of the yarn pulled from the creel by plunger 27 is used. On the other hand, when plunger 29 is chosen and descends, shaft 13 would normally be adjusted to utilize only part of the yarn in pocket 15 and, accordingly, on the next descent of plunger 27, a lesser amount need be pulled from the creel. The clamps 20, 21 and 22 are important in the operation of the feeding and metering of yarn and the clamps are in closed positions when marked by an X as clamps 21 and 22 are shown in FIG. 9.
With further reference to FIG. 9, when solenoid 92 is in the off position, the plunger 100 is biased to the right to engage band 25 with shaft 13, thus actuating plunger 29. Since plunger 29 has been designated as the metering means for the shorter pile, then the short pile will be chosen until such time as the solenoid is actuated, and plunger 100 is pulled to the left to engage band 24 with shaft 12, thus causing the selection of the unit which was chosen to provide the longer pile height.
With further reference to FIG. 9, it is to be further understood that the metering and feeding of two different lengths of yarn occurs during two successive machine cycles. Since the design of the yarn feed can be made on gauge, every needle has its own independently controlled feed and, accordingly, there are no pattern restrictions.
It is to be further understood that yarn plunger 27 always pulls from the creel and stores a length of yarn which may be somewhat greater than that needed by plunger 28 which is the highest pile plunger. This assures that when the clamp isolating pocket 15, i.e., clamp 21, from the meter pockets 16 and 17 is released and the tension goes to zero, there will always be enough yarn to transfer to the metering pockets 16 or 17 at zero tension.
Clamp 20 or the creel clamp serves to isolate the creel and its tension from the metering pockets 16 and 17. It is unclamped when the creel puller or plunger 27 is moving downward and clamped when puller 27 is moving upward.
The center clamp 21 has two primary functions. It isolates the yarn on its downstream side so that the creel puller 27 pulls yarn only from upstream (the creel) and does not allow the tension of creel pulling into the metering section. Secondly, it releases yarn pulled from the creek only after creel clamp 20 is clamped.
The feed clamp 22 prevents yarn from being pulled from the needles 40 while being transferred from the creel pocket 15 to either of the metering pockets 16, 17 and also is timed for proper release of metered yarn to needles after the meter clamp 21 is clamped.
FIG. 9 is now to be viewed as the first figure of sequential drawings FIGS. 9-12. As can be seen in FIG. 9, the creel pulling is almost complete as creel puller or plunger 27 reaches its full descent. Clamp 20 is off or unclamped to allow the yarn to be pulled from the creel while clamp 21 is clamped to prevent yarn from being pulled from the metering and needle areas toward creel puller 27. The center meter (high pile) is to be selected for high pile and thus, the solenoid 92 is actuated.
With reference to FIG. 10, clamp 20 is on in its clamping position and yarn creel puller or plunger 27 ascends. Clamp 21 is turned off while clamp 22 remains on. Plunger 28 descends pulling the yarn from creel pocket 15 into the metering pocket 16.
With reference to FIG. 11, clamp 21 is turned on while clamp 22 is off to permit the yarn metered in pocket 16 to be pulled on through by the needles. Also, since clamp 21 is on, yarn puller 27 may now descend to draw the next length of yarn from the creel as clamp 20 has now been released.
FIG. 12 shows clamp 20 back on the plunger 27 raised. Clamp 21 has been released and the low pile has been selected for the next tuft and thus, plunger 29 has descended since solenoid 92 is deactuated causing band 25 to be engaged by oscillating shaft 13. The actuation of the solenoid can be made at any time after the position reached in FIG. 10 but before the position reached in FIG. 11.
Accordingly, the many advantages of the subject system can now be appreciated. The pile height change now will occur in the system disclosed herein without the gradual tapering that has been a problem in other high-low patterning systems used to date. It is not necessary to effectuate changes through clutches and therefore it is of no concern that responses to clutches are not instantaneous and that full changes do not occur completely until several cycles after the clutches are switched.
The tension in the above-disclosed system can be held to a more uniform state since the distance from the metering area to the needles remains the same for all yarns. With the subject system, there is no need to utilize feed rolls with yarns stretched through scramble tubes to all areas of the tufting machines to enable pattern repeat.
Additional compensatory apparatus such as pull rolls, which are used to eliminate any discrepancies in yarn tension are not needed with the system disclosed herein. Furthermore, and of particular importance, is that with the present apparatus disclosed herein, there are no pattern restrictions. The entire machine will have only three drive tubes with shafts, i.e., 11, 12 and 13, and every needle has its own independently controlled feed which may be so controlled for every needle stroke. This enables wider variations in patterning without the necessity of predetermined repeats.
It will be understood that solenoid 92 receives control signals for selective actuation of plungers or yarn pullers 28, 29. Pattern information such as recorded on tape, drums or other media is converted into electrical or other type signals which are then transmitted to the solenoids 92 in synchronism with the operation of the machine.
It should be noted that with respect to the construction of the band-like member and the oscillating shaft, the smaller the shaft is, the thinner the band must be. Since the band should not take permanent deformation, Hook's Law of Stress should not be surpassed. While hardened stainless steel is preferred for the band-like member, plastic bands and other metal bands can be used as well, so long as they do not take permanent deformation. As an example, it has been found that stainless steel bands on the order of 1/100 of an inch in thickness are acceptable for the operations discussed herein using a five inch drive shaft.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and accordingly, reference should be made to the appended claims, rather than to the foregoing specification as indicating the scope of the invention.
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A method of and apparatus for feeding yarn to needles of a conventional tufting machine in which the yarn is controlled to permit the feeding of at least two different lengths per needle to produce pile tufts of varying heights. A series of yarn pullers and clamps are utilized to draw and meter the yarn from the creel. Different pullers are utilized to provide the varying pile heights. The pullers or plungers may be driven by band-like members which are engageable upon selection with a continuously oscillating shaft.
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RELATED APPLICATION
This application is a continuation-in-part of Ser. No. 739,886, filed Nov. 8, 1976, which in turn is a continuation-in-part of application Ser. No. 613,991, filed Sept. 17, 1975 now abandoned.
BACKGROUND AND SUMMARY OF THE INVENTION
The present invention is directed to compounds potentially useful in controlling insects. More particularly, the present invention is directed to active chromene compounds which are effective in inhibiting the effects of juvenile hormone in insects.
Of the various chemical compounds which have been employed in the prior art as insecticides for controlling insects, many of such prior art compounds have also been found to be harmful to humans and other animal life. In addition, many species of insect pests have developed a resistance and even immunity to available insecticides.
Alternative prior art methods for controlling insects have included the use of hormones, which interfere with the development of insects. Although such hormones have the advantage of apparently being harmless to other animals, their use is generally limited to application relatively late in the insect life cycle, after the insect has already produced its undesirable pest effect.
The endocrine systems of insects secrete a certain hormone known as juvenile hormone which functions to control the biological activities of metamorphosis, reproduction, diapause and sex attractant production. In particular, juvenile hormone functions initially to maintain the young developing insect in an immature condition until it has developed to the point where it is ready to molt to the adult form. When maturation of the insect begins, the body ceases to secrete juvenile hormone until after the insect has passed into the adult form, at which time secretion of juvenile hormone recommences in order to promote the development of the sex organs.
The forms in which juvenile hormone are known to occur in nature are discussed in the following publications: Trautmann et al., Z. Naturforsch, 29C 161-168 (1974); Judy et al., Proc. Nat. Acad. Sci. USA, 70, 1509-1513 (1973); Roller et al., Angew. Chem. Int. Ed. Eng., 6, 179-180 (1967); Meyer et al., Proc. Nat. Acad. Sci. USA, 60, 853-860 (1968); Judy et al., Life Sci., 13, 1511-1516 (1973); Jennings et al., Life Sci., 16, 1033-1040 (1975); and Judy et al., Life Sci., 16, 1059-1066 (1975).
In accordance with the present invention, it has been discovered that the lipid extract of the common bedding plant, Ageratum, contains two active compounds: (1) 6,7-dimethoxy-2-,2-dimethyl-3-chromene; and (2) 7-methoxy-2,2-dimethyl-3-chromene; each of which is effective to inhibit the effects of juvenile hormone in insects. Both compounds have been described in the literature: A. R. Alertsen "Ageratochromene, a Heterocyclic Compound from the Essential Oils of some Agertaum Species", Acta Chem. Scand. 9 (1955) No. 10, pp. 1725-1726; R. Huls "Syntheses De Chromenes Substitutes", Bull. Soc. Chim. Belg., 67 (1958), pp. 22-32; R. Livingston et al., J. Chem. Soc., p. 1509 et seq. (1957); and T. R. Kasturi et al., Tetrahedron Lett., 27 (1967), p. 2573 et seq.
These and related chromene compounds inhibit the effects of juvenile hormone, during early development of the insect and after reaching adulthood when the sex organs are undergoing development. By so inhibiting the effects of juvenile hormone, the maturing insect which has been treated with the present compounds is caused to die within a short time of such treatment. In addition, the ability of a treated insect to reproduce is prevented. The compounds of the present invention are also believed capable of interrupting embryogenesis in insect eggs, inducing diapause in insects and preventing sex pheromone secretion in insects. The present compounds may be applied by suitable means including topically, orally or in a vapor state as a fumigant.
As set forth in application Ser. No. 739,886, filed Nov. 8, 1976, based upon the activity of the extracts of Agertaum, compounds potentially suitable for use as antijuvenile hormones are selected from those with the following general structure of Formula I ##STR1## wherein:
R and R 1 are H, lower alkyl, straight or branched chain, of about 1 to 4 carbon atoms, lower alkoxy, straight or branched chain, of about 1 to 3 carbon atoms, Cl, Br or F;
R 2 , R 3 , R 4 and R 5 are H, lower alkyl, straight or branched chain, of 1 to 6 carbon atoms, lower alkoxy, straight or branched chain, of 1 to 6 carbon atoms, OH, --OCH 2 OCH 3 , --OC 2 H 4 OC 2 H 5 , --CO--OCH 3 , --CO--OCH 2 CH 3 , ##STR2## Cl, Br, F, --SCH 3 , --SCH 2 CH 3 , --SCH 2 CH 2 CH 3 , --NO 2 , or the structure wherein R 2 and R 3 , or R 3 and R 4 , or R 4 and R 5 are joined with a --OCH 2 O-- (methylenedioxy) group; or --OCH 2 CH 2 -- (ethylenedioxy) group and
Y is O, S or NH.
DESCRIPTION OF THE INVENTION
It has been further found that a particular group of compounds potentially suitable for use as anti-juvenile hormones comprises compounds corresponding to the formulae: ##STR3## wherein:
R 6 and R 7 are each hydrogen, or straight or branch chain lower alkyl containing 1-4 carbon atoms, preferably R 6 and R 7 both being methyl;
R 8 , R 9 , R 10 and R 11 are each hydrogen, straight or branch chain lower alkyl, alkenyl, alkoxy, or alkenoxy or alkynoxy containing 1-4 carbon atoms;
provided that at least one of R 9 and R 10 , preferably R 10 , is lower alkoxy or alkenoxy containing 1-4 carbon atoms;
and further provided that at least one of R 8 and R 11 is hydrogen, straight or branch chain lower alkyl, alkenyl, alkoxy, alkynoxy, or alkenoxy containing 1-4 carbon atoms;
or provided that R 10 is lower alkoxy or alkenoxy containing 1-4 carbon atoms and at least one of R 8 , R 9 and R 11 is phenyl;
or provided that R 10 is lower alkoxy or alkenoxy containing 1-4 carbon atoms and R 9 is lower alkyl containing 1-4 carbon atoms, preferably ethyl;
or ##STR4## where R 6 and R 7 are hydrogen or straight or branch chain lower alkyl containing 1-4 carbon atoms, preferably both R 6 and R 7 being methyl; X is O, S or N and R 12 is alkyl or alkenyl containing 1-4 carbon atoms or ##STR5## where R 13 and R 14 are methyl or ethyl.
Examples of such compounds include:
5-methyl-7-ethoxy-2,2-dimethyl-3-chromene
5-methyl-7-methoxy-2,2-dimethyl-3-chromene
7-ethoxy-6-methoxy-5-methyl-2,2-dimethyl-3-chromene
6,7-dimethoxy-5-methyl-2,2-dimethyl-3-chromene
7-ethoxy-8-methyl-2,2-dimethyl-3-chromene
7-methoxy-8-methyl-2,2-dimethyl-3-chromene
6,7-dimethoxy-8-methyl-2,2-dimethyl-3-chromene
7-ethoxy-6-ethyl-2,2-dimethyl-3-chromene
7-methoxy-6-ethyl-2,2-dimethyl-3-chromene
7-ethoxy-6-methyl-2,2-dimethyl-3-chromene
The present invention also relates to a process for the manufacture of compounds of the above formula, which process comprises reacting a compound of the general Formula III: ##STR6## wherein:
R 8 , R 9 , R 10 , and R 11 are substituents given in Formula II, with a compound of the general Formula IV: ##STR7## wherein, in Formula IV:
X is H, OH, Cl, Br or I; and
R 6 and R 7 are as given in connection with Formula II; in the presence of a Friedel-Crafts catalyst such as formic acid, methansulfonic acid, AlCl 3 , ZnCl 2 , polyphosphoric acid, SnCl 4 or other similar catalyst well known in the art. A suitable solvent which is compatible with the Friedel-Crafts catalyst may be employed as necessary. Such a solvent may be, for example, ether, nitrobenzene or carbon disulfide. The reaction produces a chromanone of the general Formula V: ##STR8## wherein the substituents are those given with regard to Formula II. The addition of heat, by means such as conducting the reaction on a steam bath for one to several hours, may be employed although such heating is not always necessary for obtaining the chromanone product.
The compounds of Formula V are reduced with a reducing agent which may be any of those well known to one skilled in the art, such as lithium aluminum hydride or sodium borohydride, in a suitable solvent such as tetrahydrofuran or ether, to give a chromanol of the general Formula VI: ##STR9## wherein the substituents are those given in connection with Formula II. If, following reduction, the reduction mixture containing the compounds of Formula VI are treated with a dilute acid such as hydrochloric, toluenesulfonic or other similar acid well known to those skilled in the art, dehydration of the hydroxyl group occurs given the chromenes directly corresponding to the compounds given in connection with Formula II. When the chromanols are isolated directly, subsequent treatment with catalytic amount of acid such as toluenesulfonic in refluxing benzene causes dehydration to the chromene.
In the case of the reaction of the compounds of general Formula III with unsaturated aldehydes of Formula IV in the presence of Friedel-Crafts catalysts, the desired chromenes are produced directly.
In alternative procedures, a compound having the structure of Formula III is reacted with one of the following: ##STR10## where R 6 and R 7 have the meaning specified above and X' is a halogen or hydroxyl group. The chromane resulting from this reaction is then dehydrogenated by conventional techniques to give the corresponding chromene.
The following specific examples further illustrate the preparation and utility of compounds within the scope of the general structure II above, and are to be considered illustrative and not limiting. All parts and percentages are by weight unless otherwise specified. All temperatures are degrees Centigrade unless otherwise specified.
EXAMPLE 1
Synthesis of 5-methyl-7-ethoxy-2,2-dimethyl-3-chromene
3 grams of 1,5-dihydroxy-3-methylbenzene are admixed with 3 grams of dimethylacrylic acid. There was then added 20 ml. of methanesulfonic acid and the mixture stirred for 1 hour at 70° C. The mixture was cooled and extracted with ether. The ether solution was washed twice with a saturated aqueous sodium bicarbonate solution and once with a saturated sodium chloride solution. The ether layer was dried over sodium sulfate and then evaporated to yield the corresponding 7-hydroxy-5-methylchromanone (4.5 g).
The above reaction product was dissolved in 40 ml. of dimethylformamide and there was then added 1.3 grams of powdered potassium hydroxide and the mixture stirred for 30 minutes. There was then added 17 grams of ethyl iodide and the mixture stirred overnight. The reaction mixture was then extracted with hexane and the hexane was then washed twice with 10% potassium hydroxide and once with a saturated salt solution. The hexane solution was then dried over sodium sulfate and evaporated to yield the corresponding 7-ethoxy-5-methyl-chromanone (5 g.).
The above reaction product was dissolved in 50 ml. of dry ether and there was then added 0.9 grams of lithium aluminum hydride and the mixture refluxed for 2 hours. The reaction mixture was cooled and excess hydride destroyed by addition of water. 50 ml. of 4NHCl was added and the mixture stirred for 5 minutes. The reaction mixture was washed once with water and once with a saturated salt solution and then dried over sodium sulfate. Upon evaporation 4.3 grams of a product comprising 5-methyl-7-ethoxy-2,2-dimethylchromene was recovered.
Induction of Precocious Development
In accordance with the present invention, active appropriately substituted chromene compounds were found to cause precocious maturation when applied to an immature insect. The juvenile hormone (JH) is a natural insect hormone which acts to keep the developing insect immature until it is ready to molt to the adult form. When maturation of the insect begins, the insect ceases to produce JH and the insect matures to the adult form. The compounds of the present invention have been found to stop the action of JH and cause the immature insect to undergo precocious maturation. For some insects the induced lack of JH causes such rapid maturation that the immature insect dies shortly prior to, or during the molting process. In other insects the lack of JH causes them to molt into miniature adults which completely avoids the tremendous feeding potential of the immature stages and results in tiny adults which are sterile, very fragile and which die soon after molting. The anti-juvenile hormone action can be overcome by the application of exogenous juvenile hormone, which indicates that the anti-juvenile hormone compounds act by interfering with the production of juvenile hormones.
Table I illustrates the induction of precocious maturation by contacting the milkweed bug with a chromene in accordance with the present invention. Other Hemiptera are also quite sensitive, and precocious metamorphosis has been induced in Lygaeus kalmii Stal and in Dysdercus cingulatus. Satisfactory results have not been obtained in inducing precocious metamorphosis in Holometabola.
Sterilization
In the normal adult insect, JH (or gonadotropic hormone) is produced again after molting to the adult form and is then necessary for the development of the insect ovaries. Treatment of adult insects with the compounds as described below in Table I was found to prevent or stop the action of JH and the insect ovaries failed to develop. If the insect ovaries were developed at the time of treatment, they rapidly regressed to the undeveloped state. In either event, reproduction was prevented. This technique has been successful with insects in the orders Hemiptera, Homoptera, and Orthoptera.
TABLE 1__________________________________________________________________________ Induction of Precocious Metamorphosis in Immature Milkweed Sterilization of Adult Bugs Oncopeltus fasciatus.sup.(1) Milkweed Bugs.sup.(2) Dose (μg/cm.sup.2) % Precocious Adults Dose (μg/cm.sup.2) % Sterile__________________________________________________________________________ ##STR11## 1.5 0.75 90 50 7.5 100 ##STR12## 3.9 75 15.0 50 ##STR13## 1.5 100 7.5 100__________________________________________________________________________ .sup.(1) Second instar nymphs were confined to a 9 cm. petri dish containing a residue of the test compound. .sup.(2) Newly emerged adult female milkweed bugs were confined to a 9 cm petri dish containing a residue of the test compound for 24 hours and the transferred to an untreated dish and held for 5 days at which time they were autopsied and the status of various development determined.
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Potential insect control compounds which are chromenes, as well as their method of preparation and use, are disclosed. Compounds have been found which are effective in the control of insects by inhibiting the actions of juvenile hormone. An example of a useful compound is 5-methyl-7-ethoxy-2,2-dimethyl-3-chromene. Such compounds act to induce precocious maturation of immature insects, resulting in death either during or within a short time before or after the molting to an incompetant precocious adult. Additional effects which have been obtained include sterilization of mature insects.
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BACKGROUND OF THE INVENTION
The present invention relates to a sheet feed apparatus for a lithographic printing machine or the like. More specifically, the present invention relates to an apparatus comprising a drum formed with vacuum openings for suckingly holding a sheet thereto for printing or the like.
In this type of apparatus, a drum is formed with openings such as slots and a sheet is fed thereto and suckingly held to the drum by vacuum applied to the openings. With the sheet held thusly tight to the drum, an image is printed on the sheet by a lithographic or other printing process, after which the sheet is fed away from the drum.
A problem which has remained unsolved in this type of apparatus is that sheet feed failures occasionally occur which must be detected and cleared before further printing operations can be performed. Conventional means for sensing for sheet feed failures utilize microswitches, photosensors and the like to detect the feeding of a sheet to a particular position. Failure of the sheet to be sensed means that a sheet feed failure has occurred. Such sensors are costly and involve complicated and expensive auxiliary circuitry.
Another problem is that the level of vacuum must be adjusted to correspond to the thickness of the sheet being fed. The obvious solution is to provide a regulator valve which is set by the operator after selecting the thickness of the sheets. Such a regulator valve is highly subject to missetting or being ignored.
Yet another problem is that different levels of vacuum must be provided for feeding the sheet to the drum and feeding the sheet away from the drum. If the vacuum is set to the proper value for feeding the sheet to the drum and unchanged while feeding the sheet away from the drum, the level of vacuum will be too low and the sheet will not be fed away from the drum. Conversely, if the vacuum is set to a high value for feeding sheets away from the drum and employed for feeding sheets to the drum, there is a good possibility that two sheets will be fed to the drum.
Such changeover of levels of vacuum may be accomplished by means of two or more vacuum sources and selector valve means. However, the cost of such an arrangement is unreasonably high and changeover generally requires more than 12 seconds before stable vacuum is achieved.
SUMMARY OF THE INVENTION
A sheet feed apparatus embodying the present invention includes a drum formed with openings, a vacuum source communicating with the openings so that a sheet is suckingly adhered to the drum by vacuum at the openings, means for feeding the sheet to the drum and means for feeding the sheet away from the drum, and is characterized by comprising sensor means for sensing when a level of vacuum at the source drops below a predetermined value and producing an output signal in response thereto.
In accordance with the present invention, a drum is provided with vacuum openings for suckingly holding a sheet thereto for printing or the like. A sheet feed failure is detected by sensing for a drop in the level of vacuum at a vacuum source below a predetermined value. Several regulators are provided for regulation to selected levels of vacuum.
It is an object of the present invention to provide an improved sheet feed apparatus comprising means for sensing a sheet feed failure and regulating a level of vacuum to a desired level.
It is another object of the present invention to provide a generally improved sheet feed apparatus.
Other objects, together with the foregoing, are attained in the embodiments described in the following description and illustrated in the accompanying drawing.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a diagram illustrating a first embodiment of the present invention;
FIGS. 2 and 3 are flowcharts illustrating the operation of the embodiment; and
FIGS. 4 to 7 are diagrams illustrating modified embodiments of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
While the sheet feed apparatus of the present invention is susceptible of numerous physical embodiments, depending upon the environment and requirements of use, substantial numbers of the herein shown and described embodiments have been made, tested and used, and all have performed in an eminently satisfactory manner.
Referring now to FIG. 1 of the drawing, a sheet feed apparatus embodying the present invention is generally designated by the reference numeral 11 and comprises a vacuum source or pump 12. A rotary drum 13 is provided with longitudinal slots 14 and 16 which communicate with the pump or source 12 through conduits 17 and 18 respectively. A sheet 19 is conveyed or fed to the drum 13 by movable suckers 21 which also communicate with the source 12 in the direction of an arrow 22. Due to vacuum at the slot 14, the leading edge of the sheet 19 is suckingly adhered to the drum 13 and the sheet 19 is wound around the drum 13 due to rotation thereof. The trailing edge of the sheet 19 is adhered to the drum 13 due to vacuum at the slot 16. With the leading and trailing edges of the sheet 19 thus held, the sheet 19 is tightly retained by the drum 13.
After the operation of feeding the sheet 19 to the drum 13 and adhering the sheet 19 thereto is completed, an image is printed on the sheet 19 by a lithographic printer or the like which is not part of the present invention and is not shown. Then, the sheet 19 is fed away from the drum 13 by the suckers 21.
The present invention is based on the fact that if the sheet 19 is not correctly fed to and wrapped around the drum 13, one or both of the slots 14 and 16 will not be covered by the sheet 19 and the level of vacuum produced by the pump 12 will drop. Such a drop in the level of vacuum below a predetermined value is detected by a sensor switch 23 which is turned on or closed in response thereto. When closed, the sensor switch 23 produces an output signal which is applied to an alarm control circuit 24 which energizes an alarm constituting a part thereof and causes further action.
FIG. 2 illustrates the operation of the circuit 24 in a mode of operation in which the sheet 19 is fed to the drum 13 and printed in the manner described above. If the switch 23 is on, indicating a sheet feed failure, the apparatus 11 is turned off except for the alarm which is turned on.
FIG. 3 illustrates another mode of operation in which one sheet is being fed to the drum 13 while another sheet is being discharged therefrom. If the switch 23 is on, valves 101 and 102 disposed in the conduits 17 and 18 are closed and the operation branches back to the first step.
FIG. 4 illustrates another embodiment of the present invention comprising improved means for regulating the level of vacuum applied to the suckers 21 and slots 14 and 16 to a selected predetermined value which corresponds to the thickness of the sheet 19. In this embodiment, solenoid valves 31 to 34 are connected in parallel with each other and in series with vacuum regulators 36 to 39 between the pump 12 and the suckers 21. Although not illustrated, the outputs of the regulators 36 to 39 also communicate with the slots 14 and 16. The regulators 36 to 39 regulate the output vacuum thereof by controlling the sectional area through which the vacuum acts. Switches 41 to 44 are connected to the valves 31 to 34 and open the respective valves 31 to 34 when turned on or closed. One of the switches 41 to 44 is closed automatically or by the operator to select the level of vacuum corresponding to the thickness of the sheet 19.
The regulator 36, for example, may be constructed to provide an output vacuum of 30 cmHg for feeding sheets of standard weight 110 kg. The regulator 37 may produce an output vacuum of 8 cmHg for feeding standard sheets of 70 kg. The regulator 38 may produce an output vacuum of 5 cmHg for 55 kg sheets. The regulator 39 may be adjustable by the operator for the feeding of sheets of non-standard weight or thickness or standard sheets having weights other than 110, 70 and 55 kg.
Whereas the regulators 36 to 39 regulate the vacuum by controlling the sectional area through which the vacuum acts, in FIG. 5 regulators 46 to 49 are connected in parallel with each other between the vacuum pump 12 and the atmosphere. The valves 46 to 49 provide the same function as the valves 36 to 39 respectively but are constructed to regulate the level of vacuum by controlling the sectional area of communication of the pump 12 with the atmosphere.
As discussed hereinabove, it is desirable to provide different levels of vacuum for feeding sheets to the drum 13 and feeding sheets away from the drum 13. It is also desirable to provide different levels of vacuum for a mode in which a sheet is discharged from the drum 13 before feeding another sheet thereto and a mode in which a sheet is discharged from the drum 13 while another sheet is being fed thereto. The embodiments of FIGS. 6 and 7 may be utilized in either of these two cases.
In FIG. 6, solenoid valves 51 and 52 are provided for selectively connecting regulators 53 and 54 to the pump 12. The regulators 53 and 54 are of the type used in FIG. 5 and communicate with the atmosphere. When a logically high LOAD signal is applied to a switching transistor 56 from a microcomputer 100 which controls the operation of the apparatus or a manual switch (not shown), the transistor 56 is turned on and grounds the valve 51 which opens and connects the pump 12 to the regulator 53. The LOAD signal is produced while the sheet 13 is being fed to the drum 13. A DISCHARGE signal is applied to a transistor 57 to open the valve 52 and connect the regulator 54 to the pump 12 while the sheet 13 is being fed away from the drum 13. Typically, the regulator 54 will regulate the vacuum to a level which is 2 cmHg higher than the level of the regulator 53.
FIG. 7 illustrates another sheet feed apparatus which is similar to the apparatus of FIG. 6 except that the regulators 53 and 54 are replaced by regulators 58 and 59 which are of the type used in FIG. 4.
In summary, it will be seen that the present invention overcomes the drawbacks of the prior art and provides a substantially improved sheet feed apparatus. Various modifications will become possible for those skilled in the art after receiving the teachings of the present disclosure without departing from the scope thereof.
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A drum (13) is provided with vacuum openings (14), (16), for suckingly holding a sheet (19) thereto for printing or the like. A sheet feed failure is detected by sensing for a drop in the level of vacuum at a vacuum source (12) below a predetermined value. Several regulators (36), (37), (38), (39) are provided for regulation to selected levels of vacuum.
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CROSS-REFERENCE TO RELATED APPLICATIONS
The present application is a continuation of U.S. patent application Ser. No. 12/970,171, filed Dec. 16, 2010, herein incorporated by reference in its entirety for all purposes.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
N/A
THE NAMES OF THE PARTIES TO A JOINT RESEARCH AGREEMENT
N/A
INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISC
N/A
BACKGROUND OF THE INVENTION
1. Field of the Invention
The subject matter of this disclosure relates to the electrical heating of metal cylinders to form a seam bond and applying a means of cooling to the metal cylinders corresponding at least in part to U.S. Classification 261/61.7 and IPC8 B23K9/02.
2. Description of Related Art
Industrial pipe systems involve multiple pipe configurations, different diameters and pipe wall thicknesses often joined to one of numerous connection elements such as flanges, elbows, T junctions. Engineers draft spool drawings as representations of a pipe section that needs to be created. These drawings detail the angles, fitting sizes, and other specifications needed to create the desired pipe structures (fabricated pieces). The pipe assembly process generally begins with preparing the segments. Bevels are created on the pipe ends to lay down the multiple weld passes, and other pipe end or surface preparations are performed. Next the spool components are generally tack welded together to align the pipe sections for multi-pass welding.
Multi-pass welding is traditionally performed manually by specialized and highly skilled welders. However, various forms of automation exist. A common automation is flat-position groove welding. In flat-position groove welding, two or more pipe sections are set horizontally on a support structure. The support structure rotates the pipes for welding. A fixed welding torch is aligned with the pipe junction and the pipes sections are welded together while the pipes are rotating. Automated welding can include a fixed or stationary pipe, with the automated welding torch rotating around the pipe as it welds. Other forms of semi-automation include manual weld first passes with orbital GTAW or orbital FCAW for subsequent weld passes. Finally, multi-pass welding may be performed by robotic arms programmed to apply welds according to the specifications of the spools.
It is common that welding codes and or procedures limit the process to a maximum interpass temperature during the entire multi pass weld. The process of multi-pass arc welding generally involves the steps of a) creating a first weld seal (root pass) of two sections of pipe, b) allowing the weld to cool, c) performing a subsequent weld over the previous weld, and d) repeating steps b) and c) until the piping sections are fully welded together across the thickness of the pipe wall, including weld reinforcement. Many codes or weld procedures require the weld area on the inside of the pipe to be free from atmospheric contaminants such as oxygen and sometimes nitrogen. In order to accomplish this, dams are inserted into the two sections of pipe while performing welding. These dams form a contained interior volume of piping with the weld seam generally in the center. In many circumstances, both water and oxygen should be minimized or eliminated while the weld is being made and during the post welding cool down period. Consequently, during arc welding of thick walled pipe sections together, an inert gas is continually flushed through the contained interior volume to prevent oxidation of the weld site and to evaporate and remove moisture from the weld site.
A major materials issue with multi-pass welding of pipes is the structural integrality of the resulting weld. It is critical in e.g. nuclear reactors, that pipes handling reactor coolant not fail due to rupture. A stress fracture of key pipes in a refinery could result in catastrophic failure causing great damage and endangering many lives. It is thus essential that these welded structures adequately withstand the extreme conditions to which they are exposed.
A variety of standards exist which quantify various material requirements for multi-pass welded pipes. See, e.g., Process Piping: The Complete Guide to ASME B31.3. Third Edition. Charles Becht IV. ASME Press, Three Park Avenue, New York, N.Y. 10016-5990. 2009; ISBN-13: 978-0-7918-0286-1. A key control parameter in producing multi-pass welded pipes is the “interpass temperature” parameter. There are empirically defined minimum and maximum interpass temperatures depending on such factors as the type of metal alloy making up the pipe sections. These temperatures define welding process conditions that produce pipe welds with acceptable material properties. In particular, before a subsequent welding pass, the weld site temperature should be at or below the maximum interpass temperature. In practice this requires waiting for the prior weld's temperature to drop to at least the interpass maximum temperature. The interval time between weld passes in the current practice will vary according to wall thickness and maximum interpass temperature but can range from a few minutes to an hour or more. This slows down the welding process and causes undesirable idle time for highly skilled specialty welders. There is also an ongoing risk of overheating the weld zone thereby causing structural flaws in the piping produced. A severe example of such structural flaws from overheating of a metal during welding is warping and distortion of the physical shape of the material.
It is therefore desirable to effect control over the temperature of weld sites in multi-pass welding to reduce or eliminate the down time between welding passes. The art has not effectively addressed this problem. Solutions to interpass temperature control generally relate to accelerated cooling between passes. These prior art operate by application of air and/or water for convective heat transfer from the weld. Use of air exposes the weld to oxygen and is thus contraindicated for the pipe welding of this disclosure. Water cooling potentially may be used, but this requires specially adapted equipment. Exposing water to the weld site during weld processing is also undesirable because the water has to be removed after welding, the water can pose safety hazards including electrical and slip and fall, this can also lead to oxidation on the inside of the pipe.
U.S. Pat. No. 4,152,568 describes a process of coolant circulation within a pipe to accelerate the cooling rate of welds. The coolant is water, liquid nitrogen or dry ice. Liquid nitrogen is preferred for cooling from the maximum interpass temperature to 800 degrees C. U.S. Pat. No. 4,152,568 does not address multi-pass welding where three or more welds are applied in series. U.S. Pat. No. 4,152,568 does not describe the control of the maximum temperature reached by the weld site. Finally, U.S. Pat. No. 4,152,568 still requires specially adapted equipment to carry out the described accelerated interpass cooling method. This method does not address the potential for metallurgical changes in the base material as a result of deep cryogenic treatment of the weld zone and other areas where the liquid nitrogen comes in contact with the pipe. This cryogenic treatment can be advantageous by increasing wear resistance in some materials but may also be disadvantageous to some materials by possibly decreasing tensile strength and or other mechanical properties. The limitations and effects are currently being researched.
BRIEF SUMMARY OF THE INVENTION
1. A process for welding pipe sections ( 19 ) together, the process comprising the steps of:
a) creating a first weld between the pipe sections ( 19 ) at a weld zone ( 70 ) while using an inert purge gas comprising nitrogen, argon, and/or helium at ambient temperatures, b) establishing an flow of an inert cooled gas through an interior ( 50 ) of the pipe sections ( 19 ) and in thermal communication with the first weld, the inert cooled gas comprising nitrogen, argon, and/or helium, c) monitoring a temperature of the weld zone ( 70 ), d) creating an additional weld between the pipe sections ( 19 ) at the weld zone ( 70 ), e) in response to the temperature of the weld zone ( 70 ) during step d), adjusting the temperature ( 12 , 40 ) and/or a flow rate ( 8 , 15 ) of the flow of the inert gas to maintain the weld junction temperature at or below a maximum interpass temperature during step d).
2. A process for welding pipe sections together, the process comprising the steps of:
a) establishing an initial flow of an ambient temperature inert gas through an interior ( 50 ) of the pipe sections ( 19 ) and in thermal communication with the weld zone ( 70 ), b) creating a first weld at a weld zone ( 70 ) between the pipe sections ( 20 ), c) switching from ambient temperature inert gas to cooled gas ( 8 , 15 ) for remaining weld passes, d) creating an additional weld between the pipe sections at the weld zone ( 70 ), e) adjusting the temperature ( 12 , 40 ) and/or a flow rate of the flow of the inert gas ( 8 , 15 ) to reduce the maximum temperature reached during step c) at the weld zone ( 70 ).
3. The process of sentence 1 or 2, further comprising the step of adjusting the temperature ( 12 , 40 ) and/or the flow rate ( 8 , 15 ) of the inert gas flow to a degree sufficient to accelerate the cooling rate of the weld after the additional weld is completed, measured relative to the rate of cooling using an inert gas flow at ambient temperature at an initial flow rate.
4. The process of sentence 1, wherein the maximum interpass temperature is from 100 degrees C. to 175 degrees C. for Austenitic stainless steels and from 250 degrees C. to 315 degrees C. for various grades of carbon steels.
5. The process of sentence 1, 2, 3 or 4, wherein the temperature of the flow of inert gas is from −75 degrees C. to −226 degrees C.
6. The process of sentence 1, 2, 3, 4 or 5, wherein a flow rate of the flow of inert gas is from 10 scfh to 100 scfh.
7. The process of any one of sentences 1-6, further comprising the step of establishing a flow of an inert cooled gas onto an exterior side ( 20 , 21 , 80 ) of the weld zone ( 70 ) of the pipe sections ( 19 ) and in thermal communication with the weld zone ( 70 ), the inert cooled gas comprising nitrogen, argon, and/or helium.
8. The process of any one of sentences 1-7, wherein the step of establishing an flow of an inert cooled gas through an interior comprised a sub-steps of:
i) blending cooled and ambient temperature inert gas ( 8 , 15 ), and ii) measuring the temperature of the blended inert gas ( 12 ).
9. The process of any one of sentences 1-8 wherein the pipe sections are located on a ground outside, on a floor of a building, or are in place at the location where the finished pipe is intended to be used.
10. An apparatus specifically adapted and configured to carry out the process of any one of sentences 1-9.
11. A pipe produced by the process of any one of sentences 1-9.
12. An apparatus for controlling interpass weld temperatures during a multi-pass welding operation, the apparatus comprising,
a) a containment barrier ( 18 ) adapted to at least partially isolate an interior volume ( 50 ) of the two or more pipe sections ( 19 ), wherein the interior volume ( 50 ) includes a part of a weld zone ( 70 ), b) an inert gas delivery sub-apparatus comprising,
i) an inlet ( 90 ) fluidly connected to the volume ( 50 ) and fluidly connected to an inert gas delivery line ( 2 , 22 ), ii) the inert gas delivery line ( 2 , 22 ) further fluidly connected to a source of inert gas ( 30 ), iii) an inert gas flow control device ( 8 , 15 ) configured to control the flow of inert gas from the inert gas source ( 30 ) into the interior volume ( 50 ),
c) a temperature control device ( 12 , 40 ) configured to be capable of adjusting the temperature of an inert gas at one or more places in the inert gas delivery sub-apparatus.
13. The apparatus of sentence 12, wherein a) the source of inert gas ( 30 ) comprises a pressurized tank comprising a liquefied inert gas stock ( 23 ) and b) the temperature control device comprises a liquefied gas vaporizer ( 12 ), the vaporizer being
a) in fluid communication with the inert gas source ( 30 ) and the inert gas delivery line ( 2 , 22 ), b) configured to receive the liquefied inert gas stock ( 23 ), and c) configured to vaporize the liquefied inert gas into a gaseous state.
14. The apparatus of sentence 12, wherein a) the source of inert gas ( 30 ) comprises a pressurized tank comprising a gaseous inert gas stock and b) the temperature control device comprises a cooling coil ( 40 ) at least partially submerged, including completely submerged, in a volume of a liquid cryogen ( 23 ).
15. The apparatus of sentences 12, 13 or 14, further comprising a temperature probe ( 60 ) configured to be capable of measuring the temperature of a weld junction a) between welding passes, b) during welding, or c) both.
16. The apparatus of sentence 12, 13, 14 or 15 further comprising a computer in operable communication with one or more component of the apparatus, the computer specifically programmed to operate the component in response to one or more of:
a) an instruction from an operator, b) a value derived from a temperature probe ( 60 ) and/or an inline temperature sensor.
17. The apparatus of sentence 12, 13, 14, 15 or 16 further comprising a support scaffold adapted to position two or more pipe sections ( 19 ) in an alignment suitable for welding the pipe sections ( 19 ) together.
18. An apparatus for controlling interpass weld temperatures during a multi-pass welding operation, the apparatus comprising,
a) a means for positioning two or more pipe sections in an alignment suitable for welding the pipe sections together ( 19 ), b) a means for at least partially isolating an interior volume of the two or more pipe sections ( 50 ), wherein the interior volume includes a weld zone ( 70 ), c) a means for providing a flow of inert gas through the interior volume ( 2 , 8 , 18 , 22 ), and d) a means for adjusting the temperature of the flow of the inert gas ( 12 , 40 ).
19. The apparatus of sentence 18 further comprising means for measuring the temperature ( 60 ) of a weld zone ( 70 ) a) between welding passes, b) during welding, or c) both.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING(S)
FIG. 1 shows an exemplary apparatus and method of implementing the invention using the same.
DETAILED DESCRIPTION OF THE INVENTION
Regardless of the general process of multi-pass welding, interpass temperature values should be constrained to produce welds with the required physical properties, and in some cases, the weld area must be free from oxygen and sometimes nitrogen as well. The devices and methods described herein provide a readily adopted way of controlling interpass temperatures in a multi-weld process while at the same time, providing an inert atmosphere in the weld area. The inert atmosphere will be free from oxygen and/or nitrogen depending on the cooling medium chosen. While some codes or weld procedure specifications will allow the use of nitrogen as the inerting gas, some companies or quality administrators simply prefer the use of a completely inert gas such as argon as it can provide a cleaner, more aesthetically pleasing surface on the weld root pass and heat affected zone.
An exemplary apparatus for controlling interpass weld temperatures during a multi-pass welding operation includes a) a support scaffold b) a containment barrier, c) an inert gas delivery sub-apparatus and d) a temperature control device.
Support Scaffold
The support scaffold, vice, jack stand or other similar device holds the pipe sections in alignment with each other and/or the welding torch. For example, flat-position groove welding generally uses rollers to both support and rotate the pipe sections. Other fabrication pieces have to be welded in place and can not be rotated. On site assembly of fabrication pieces in particular is often done manually on stationary fabrication pieces to form the pipe structure where the pipe will be used. The support scaffold in this context may be the same structures that will hold the final pipe in place in the final structure. Alternatively, the pipe sections may be placed on the floor or the ground outside and manually welded.
Containment Barrier
There are various types and designs of “purge dams” or containment barriers readily available in the market to date, or often the purge dams are made on site by the welders or fitters using one or more of the following or a combination of the following; tape or purge tape, cardboard, paper, wood, purge paper etc. The containments barrier forms an isolated interior pipe volume. This interior pipe volume is then flushed with an inert gas during welding. One form of containment barrier uses compression fittings to seal a hose to the end of a pipe section being welded. The hose transmits an inert purge gas from an inert gas source to the interior space of the pipes sections including the weld area. When welding larger diameter tubes, it is common to seal the hose to the tube using tape. A number of other means for forming a containments barrier are known in the art such as those disclosed in U.S. Pat. No. 4,723,064, which is incorporated herein by reference.
Inert Gas Delivery Sub-System
The Inert Gas Delivery Sub-system generally has at least three distinct elements, a source of inert gas, an inert gas delivery line (e.g. a purge hose) and an inert gas outlet.
Inert Gas Source
The source of inert gas may be any device, container or generation source of an inert gas. Examples include air separation units and industrial gas production facilities. The source of inert gas is preferably a pressurized tank holding liquefied inert gas stock such as liquid nitrogen, liquid argon, or liquid helium. The cylinder can be a standard liquid cylinder, or a liquid cylinder modified with sub-cooling coils installed. In many welding processes, the welding torch is supplied with an inert gas from an inert welding gas source. This same inert welding gas source may be used for the temperature control process described herein. In relation to industrial pipe welding for example, a common welding process used is GTAW (Tig). The GTAW process requires a supply of gaseous argon to the actual welding torch. The same argon source could be simultaneously used as a coolant gas for the process described herein.
Inert Gas Delivery Line
Each liquid cylinder generally has a gas use outlet or connection, a liquid use outlet or connection, a gas vent valve, and pressure relief devices. The liquid use line connects to the inlet side of the temperature control device, and then one end of a hose is connected to the outlet side of the temperature control device while the other end of the hose is connected to the inlet purge dam. This supplies gaseous nitrogen, argon, or helium that can range in temperature from ambient (e.g. 25 degrees C.) to −75 degrees C. to −156 degrees C. to −179 degrees C. (and any temperature sub-range or specific temperature within the forgoing range) when using either nitrogen or argon, and as cold as −212 to −226 degrees C. when using liquid helium. The inert gas delivery line structure depends in part on the inert gas source and the specific context of the welding work site. The structure may include fixed inert gas delivery pipes from industrial gas production facilities and/or standard liquefied gas dispensing hoses.
Temperature Control Device
The temperature control device may be any device capable of modifying the temperature of the inert liquid forming the inert gas flow through the contained interior volume of pipe sections. One preferred component of the temperature control device when the inert gas is derived from a liquefied gas stock is a electric heater or vaporizer attached to the liquid supply connection of a cylinder of liquid nitrogen, argon, or helium. These devices are available on the market. The vaporizer may be in fluid communication with the inert gas source and the inert gas delivery line such that the vaporizer receives the liquefied inert gas stock and vaporizes the liquefied inert gas into a gaseous state.
Another component of the temperature control device in embodiments using a liquefied inert gas stock may be a cooling coil completely or at least partially submerged in a liquefied inert gas stock. A stream of gaseous nitrogen, argon, or helium is circulated through the submersed coil to produce a sub cooled gas, and then flows through the vaporizer or heater to control the temperature to the desired range, and then is supplied to the inside of the piping fabrication piece via the purge dams.
An apparatus suitable for practicing the invention herein may include a number of other components including a temperature probe to provide a continuous monitoring of the temperature of the base material at the weld zone. A temperature probe may also be inserted into the inside of the pipe to monitor the inside temperature.
Temperature Probe
Temperature probes are typically electric and are readily available in the market. Suitable infrared thermometers are also commercially available.
Automated Temperature Control
The temperature probe and temperature control device for the inert gas may be linked by a computer specifically programmed to respond to the temperature from the probe to adjust the temperature and/or flow rate of the gas to control the temperature of the weld zone.
EXAMPLE
Standard gas cylinder 30 supplies the initial ambient temperature inert gas for creating a first pass weld between the pipe sections 19 via gas delivery lines 2 and 22 . This same gas cylinder is then switched by valve connections 15 and 8 to temperature control device 40 . In either case (ambient or cooled), the inert gas flows through gas delivery lines 2 and 22 through containment dams 18 and into the internal space 50 of pipe sections 19 . Temperature probe 60 is a laser, non-contact infrared thermometer. The temperature probe 60 is used to monitor the temperature of the weld zone 70 .
After the initial weld using ambient temperature inert gas, the switch valve connections 15 and 8 are actuated manually to deliver inert gas via the temperature control device 40 . The switch valve 15 may have intermediate settings whereby ambient temperature gas flows through both bypass gas delivery line 17 and temperature control device 40 . The flows of ambient and cooled gas may optionally be blended by a mechanical mixer inline with gas delivery line 50 . A separate temperature sensor may optionally be in communication with the gas in line 2 to measure the temperature of the inert gas being sent to the pipe sections 19 . The inert cooled gas may optionally also be delivered to the exterior 80 of the pipe sections 19 at the weld zone 70 via external line 21 . The external gas line may be connected to a collar 20 placed around the weld zone 70 for delivery to the weld zone 70 .
The temperature control device 40 is configured to receive the inert gas (including but not limited to nitrogen) from cylinder 30 and adapted to decrease or control the temperature of the inert gas for delivery via gas delivery line 2 to the weld zone 70 . In this example, the temperature control device comprises the following components:
1 . Outer vessel burst disc 2 . Ambient, Cooled, or Sub-Cooled gaseous Argon, Nitrogen, or Helium outlet to process 3 . Liquid fill/withdraw line 4 . Inner Vessel Rupture disc 5 . Pressure Gauge 6 . Relief valve 7 . Vent line 8 . Gaseous Nitrogen, Argon, or Helium inlet—to be cooled (Alternative Method-Optional) 9 . Outer vessel 10 . Inner vessel—containing liquid Nitrogen, Argon, Helium, or CO2 11 . Floating liquid level gauge 12 . In-line gas Heater/Vaporizer-temperature control device 13 . Relief valve 14 . Pressure Gauge 15 . Manual or Automated Valve or Solenoid 16 . By-pass to permit use of liquid argon, nitrogen, or helium contained in the cylinder, without using the sub-cooling coils 17 . By-pass to permit the use of ambient temperature Nitrogen, Argon, or Helium for making initial or root pass. 18 . Purge Dam 19 . Fabrication Piece Example 20 . External Application Device (Alternative Method-Optional) 21 . Supply Line for External Application (Optional) 22 . Supply Line for Internal Application 23 . Liquid Nitrogen, Argon, or Helium 24 . Pressure Regulator
The method of cooling the inert gas in this example is to flow the ambient temperature inert gas through a cooling coil 40 . The cooling coil 40 is submerged in a cryogenic liquid such as liquid nitrogen. In this example, final cooled inert gas temperature may be adjusted to anywhere between ambient temperature and the temperature and −212 degrees Celsius by blending cooled inert gas with ambient temperature inert gas (optionally through a static mixer with temperature determined by an inline temperature sensor).
An alternative embodiment used liquid cryogen and a heated vaporizer to deliver an inert gas at a specified temperature. In other alternative embodiments, the delivery pressure of the inert gas may be regulated by one of more inline pumps to control the flow rate of the inert gas in addition to the flow valves (e.g. valve 15 ) and the pressure derived from the inert gas source (e.g. standard cylinder 30 ).
One or more of the temperature probe 60 , inline temperature sensor, flow valves 15 , optional inert gas pressurizing pump may be operated by the welder via a computer operably connected with devices for operating these components. For example, valves 15 and 8 may have a motor configured to switch the valves to different positions. The computer may be specifically programmed to automate one or more steps of the process. For example, the ratio of ambient and cooled inert gas may be adjusted in response to temperature probe 60 to decrease the temperature of the inert gas if the weld zone 70 reaches a predetermined threshold temperature. The computer may further operate the vaporizer 12 to adjust the temperature of the inert gas flowing to delivery line 2 .
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This disclosure describes a method and apparatus for controlling the temperature of a welding zone for welding together pipe sections. The temperature is controlled by a flow of inert gas through the pipes. The inert gas flow is cooled and acts as a heat sink to remove heat from the weld zone thereby controlling the weld zone temperature.
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BACKGROUND OF THE INVENTION
This invention relates generally to a speed governor and in particular, to a braking device for a rotary shaft.
While the present invention is suitable for general application as described above, it is particularly well-suited for use with passenger loading bridges for aircraft. These bridges utilize an electrical motor and gear box chain drive to a ball screw to provide vertical movement to the bridge. The present systems do not have a safety provision to stop the bridge from going completely down to the bottom limit of the vertical drive column in case of failure of the brake of the electrical motor, chain, or gear box. The abrupt dropping of the bridge can cause injury to passengers as well as damage to the aircraft.
Other centrifugal force speed governors have previously been disclosed. These are exemplified by U.S. Pat. Nos. 3,715,016 to Frieder, 2,388,046 to Beall, and 3,415,343 to Svensson.
However, the prior art braking devices have been quite large, complicated, slow to respond, and require disassembly of the system for resetting once the problem has been corrected.
SUMMARY OF THE INVENTION
It is, therefore, an object of the present invention to provide a relatively simple, inexpensive centrifugal braking device for a rotary shaft.
It is another object of the present invention to provide a highly compact centrifugal braking device for a rotary shaft.
It is yet another object of the present invention to provide a centrifugal braking devise having a cam surface to aid the displacement of a centrifugal stop member from the stop or braking position to a rest position where the shaft can be rotated in the desired direction.
It is still another object of the present invention to provide a centrifugal braking device having a short response time for braking action.
It is still another object of the present invention to provide a centrifugal braking device responsible to both angular velocity and angular acceleration of a rotary shaft.
Briefly, in accordance with the invention, there is provided a centrifugal braking device for a rotary shaft comprising a sprocket, at least one centrifugal body, and a substantially stationary annular member. The centrifugal body is pivotally connected to the hub of the sprocket and is shiftable from a rest position to an outward stop position in response to centrifugal force. The annular member is substantially stationary and is disposed concentrically around the hub of the sprocket and has a bore aligned with the centrifugal body, said bore defining a stop thereon such that with sufficient centrifugal force the centrifugal body will move outwardly and engage the stop of the substantially annular member to brake the rotary shaft.
In the preferred embodiment, the braking device is also responsive to angular acceleration of the rotary shaft and the periphery of the bore of the annular member defines a cam surface that aids displacement of the cetrifugal body from the stop position to the rest position when the rotary shaft is rotated in a specified direction.
Other objects and advantages of the invention will become apparent on reading the following detailed description and upon reference to the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic elevational view of the centrifugal braking device as used in a screw lifting assembly;
FIG. 2 is an exploded perspective view of the present centrifugal braking device with certain symmetrical members omitted;
FIG. 3 is a plan view with portions broken away of the braking device illustrating the rest position for the centrifugal bodies;
FIG. 4 is a plan view of the braking device illustrating the stop position of the centrifugal bodies and the damping action of springs attached to the substantially stationary annular member;
FIG. 5 is a sectional elevational view of the centrifugal braking device of FIG. 3 taken in the direction of arrows 5--5 of FIG. 3;
FIG. 6 is a detail sectional view of the connection of a centrifugal body to the sprocket taken in the direction of arrows 6--6 of FIG. 3;
FIG. 7 is a detail sectional view of the attachment of a restraining spring to a keeper-block attached to the sprocket hub taken in the direction of arrows 7--7 of FIG. 3.
While the invention will be described in connection with the preferred embodiment, it will be understood that it is not intended to limit the invention to those embodiments. On the contrary, it is intended to cover all alternatives, modifications, and equivalents that may be included within the spirit and scope of the invention as defined by the appended claims.
DETAILED DESCRIPTION OF THE INVENTION
Turning first to FIG. 1, the centrifugal brake mechanism is shown functionally attached to a screw elevating assembly generally indicated at 10. The brake mechanism generally indicated at 12 is drivingly connected to a motor 14 through a chain 16. A ball screw 17 (Fig. 5) which can be located within a telescopic cover 18 raises and lowers by its rotation a support block 20. Thus, a support block 20 is shown in its lower position in solid lines and in elevated position shown in broken lines when raised in the direction of arrow 22. Stationary rails 26 and 27 (FIG. 3) act as side frames for the screw device 10 and also as stationary members for the brake device 12 to bear against to prevent rotation of the ball screw 17. Thus, when the angular speed (and acceleration if device 12 is so provided) of the ball screw rotation in the direction for moving support block 20 downward exceeds a predetermined level such that support block 20 would move downward at a dangerous speed, such as by the breaking of chain 16, the centrifugal brake device through a mechanism to be described hereinafter stops rotation of the ball screw 17 and thereby the descent of support block 20.
Referring now to FIG. 2, sprocket 30 is provided in engaging relationship with chain 16 (FIG. 1) to drive the ball screw 17 (FIG. 5). Sprocket 30 is drivingly connected to ball screw 17 by means of a key 140 on ball screw 17 and slot 32 within a central bore 34 in sprocket 30. Sprocket 30 has a hub generally indicated at 36 preferably integrally attached thereto. Hub 36 is made up of a lower ring 38 and upper ring 40 connected by axial wall 42. Lower ring 38 extends radially outward a greater distance relative to upper ring 40. A washer 50 is positioned concentric with and adjacent to lower ring 38 of hub 36. Washer 50 is preferably of a material, such as nylatron, that will present a relatively friction-free surface. A circular strip 52, also preferably of nylatron, is positioned over and perpendicular to washer 50 and also concentric with and adjacent to the outer periphery of ring 38.
An annular cam housing 60 is positioned over sprocket 30 concentric with hub 36 of sprocket 30 with the lower surface of cam housing 60 resting on washer 50 and the inner periphery of bore 62 of housing 60 contacting strip 52. Cam housing 60 is substantially stationary as opposed to sprocket 30 which rotates relative to cam housing 60, such rotation being relatively friction-free by virtue of nylatron washer 50 and strip 52. Cam housing 60 has an outer bore 64 also defined therein, said outer bore 64 having a relatively larger diameter than inner bore 62. In essence, cam housing 60 comprises a pair of rings 66 and 68 preferably integrally connected. Optimally, the combined thickness of ring 66 and washer 50 is equivalent to the thickness of ring 38 so that the upper surface of ring 66 is in alignment with the upper surface of ring 38.
At least one centrifugal body 70 (another could be symmetrically provided as shown in FIG. 3) is pivotally connected to the upper surface of ring 38 of hub 36. For this purpose, member 70 and ring 38 have aligned apertures 72 and 74 respectively, drilled therein in which a pin 76 is positioned. A washer 78 is preferably provided between apertures 72 and 74 to slightly elevate member 70 above the upper surface of ring 38 and ring 66 in order to lessen friction and allow for the free rotational movement of member 70. Centrifugal member 70 is resiliently biased inwardly by a spring 80 that is attached to an aperture 82 in member 70 and a nail head extension 86 of a bolt 84. The positioning of spring 80 is such that it provides decreasing resistance as member 70 pivots outwardly due to the decreasing size of the lever arm between pin 76 and bolt 84, thereby causing a snap-out effect. The spring 80 is located above member 70 and additionally functions to elevate member 70 above ring 38 and ring 66. Bolt 84 is positioned within aperture 90 of keeper-block 92, aligned aperture 94 of washer 96, and aligned aperture 98 in ring 38 of hub 36. Keeper-block 92 is additionally fastened to ring 38 by means of a cap screw 100 which fits in aperture 102 of keeper-block 92, aligned aperture 104 of washer 96, and aperture 106 of ring 38.
Referring now to FIGS. 2, 3, and 4, it is seen that the centrifugal member 70 has arcurately shaped sides 110 and 112. The inner side 110 preferably has a radius of curvature substantially the same as that of the outer periphery of axial wall 42 of hub 36. Thus, in the rest position as illustrated in FIG. 3, centrifugal bodies 70 (in this case two centrifugal bodies 70 are used, as are two keeper blocks 92 and the attachments thereto) are positioned with their side 110 adjacent axial wall 42 of hub 36. In this position, bodies 70 simply rotate with sprocket 30 without interfering with such rotation by contact with outer bore 64 of cam housing 60.
Outer bore 64 of cam housing 60 is defined by two semi-circles 114 and 116 having the same radius, but offset centers of curvature 118 and 119 respectively. By virtue of this offset, two rib-like areas or stops 120 are defined at the junctures of semi-circles 114 and 116. When the angular velocity of sprocket 30 increases above a predetermined level, the centrifugal force upon members 70 will be sufficient to overcome the restraining bias of springs 80 forcing outward rotary movement (by virtue of pivotal connections at 76) of members 70. When the direction of rotation is counter-clockwise as shown by arrows 130 which corresponds to a downward movement of support block 20 (FIG. 1), members 70, when sufficiently outwardly rotated, will contact stop members 120 at their contact surfaces 122, which are preferably flat.
By virtue of this contact with stops 120 of cam housing 60 which is stationary or substantially stationary, rotation of members 70 in the direction of arrows 130 is prevented, accordingly preventing such rotation of sprocket 30 by virtue of the pinned connection to members 70 and also thereby rotation of ball screw 17 by virtue of its keyed connection to sprocket 30 at 140. Thus, downward movement of support block 20 is halted when the centrifugal members 70 are in the stop position (FIG. 4).
Cam housing 60 can be made stationary in any suitable manner or, preferably, made substantially stationary. As an example of this latter design approach, cam housing 60 has integral flanges 140 positioned on the outer periphery 69 of ring 68. Each flange 140 has a pin 142 connected perpendicular thereto. Stationary supports made up of end rails 26 and 27 and center rails 29 which join parallel rails 26 and 27 are positioned adjacent flanges 140. A spring 144 is positioned around each pin 142 and bears against one edge of flange 140 and an inner edge of end rails 26. In the rest position of members 70, the free end 143 of pins 142 is spaced from respective rails 26, and the spring 144 biases the opposite end of flanges 140 against the inner edge of the rail members 27 (See FIG. 3). When, however, centrifugal bodies 70 contact stops 120 of cam housing 60, the cam housing is rotated due to the force of contact in a counter-clockwise direction overcoming the force of springs 144 until ends 143 of pins 142 contact rail members 26. In this manner the rotation of ball screw 17 and the downward movement of support block 20 is slowed resiliently by springs 144 prior to being stopped when pins 142 contact rail members 26, thereby cushioning the shock of an abrupt stop.
Centrifugal bodies 70 can also be designed to be responsive to angular acceleration of ball screw 17 (and sprocket 30), i.e., bodies 70 pivot outwardly in response to angular acceleration above a predetermined valve. This is accomplished in the present invention by having the centrifugal bodies 70 designed such that the center of gravity 150 of each body 70 is located so that the force responsive to the angular acceleration on bodies 70 which is directed along a line 151 perpendicular to the line 153 between the axis of rotation 155 and center of gravity 150 acts outwardly of the center of pin 76 a distance 157 (directed parallel to line 153). The magnitude of distance 157 should not be too great or else the members 70 would become overly responsive to acceleration causing unnecessary actuation of the braking mechanism. Conversely, if distance 157 is too small, the acceleration responsiveness is minimized. Should the center of gravity 150 be such that line 151 falls inward of pivot 76, increasing angular acceleration will act to restrain members 70 from outward movement.
When ball screw 17 and sprocket 30 are rotating in the clockwise direction corresponding to an upward movement of support block 20, the brake mechanism 12 of the present system will be substantially inoperable. During such upward movement, the brake need not operate as dangerous failures in the system would only cause or result in a counter-clockwise movement 130, thereby activating the brake. In any case, should the clockwise rotation of sprocket 30 and ball screw 17 exceed a predetermined value, centrifugal bodies 70 will rotate outwardly contacting outer bore 64 of cam housing 60 due to the centrifugal force on members 70 overcoming the spring force of springs 80 thereby resulting in some braking due to the frictional contact between sides 112 of members 70 and outer bore 64 of cam housing 60. There will, of course, not be a complete stop caused by brake mechanism 12 because stops 120 and contact surfaces 122 are directed for counter-clockwise rotation and will not register in clockwise rotation.
It should be noted that when the brake mechanism 12 is in the stop position shown in FIG. 4 with centrifugal members 70 engaging stops 120, clockwise rotation of ball screw 17 and sprocket 30 corresponding to upward movement of support block 20 (which indicates that the failure of the system has been corrected) will separate contact surface 122 of members 70 from stops 120 thereby allowing springs 80 to exert an effective return force upon members 70 to the rest position of FIG. 3. In addition to such spring force, outer bore 64 of cam housing 60 is designed to cam members 70 inwardly when sprocket 30 is rotating clockwise by virtue of the offset of semi-circles 114 and 116.
Referring now to FIG. 5, the fitted relationship of the parts illustrated in FIG. 2 is shown along with the compact nature of brake mechanism 12. In essence, brake mechanism 12 is seen to be a sprocket 30 with attachments thereto. As is also more clearly illustrated in this figure, inner ring 66 of cam housing 60 has an outer periphery 67 radially inward of the outer periphery 69 of outer ring 68. Also shown is the cavity 160 (See also FIG. 6 and FIG. 7) defined by an outer axially extending cylindrical wall 162 connected to sprocket wheel 31 and concentric with an axially extending cylindrical wall 164 which is an extension of hub 36. In this cavity 160 is positioned bearing 166 and bearing housing 168. Bearing housing 168 is fixedly attached to support plate 170.
FIGS. 6 and 7 illustrate in detail the connection of centrifugal bodies 70 (FIG. 6) and the spring connection to keeper-block 92 (FIG. 7).
Thus, it is apparent that there has been provided, in accordance with the invention, a centrifugal braking device that fully satisfies the objects, aims, and advantages set forth above. While the invention has been described in conjunction with specific embodiments thereof, it is evident that many alternatives, modifications, and variations will be apparent to those skilled in the art. Accordingly, it is intended to embrace all such alternatives, modifications, and variations as fall within the spirit and scope of the appended claims.
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A centrifugal braking device of compact design uses at least one centrifugal body pivotally connected to a sprocket to shift from a rest position to a stop position to brake movement of a rotary shaft under certain conditions. Thus, depending upon the rotary speed and/or acceleration of the rotary shaft, the centrifugal body will pivotally shift from a rest position to a stop position to prevent rotation of the shaft. A substantially stationary annular member disposed concentrically around the hub of the sprocket has an inner bore which defines a stop for the centrifugal body when said body is shifted outwardly. Said outer bore also defines a cam surface to aid displacement of the centrifugal body from the stop position to the rest position when the shaft is rotated in a specified direction.
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BACKGROUND OF THE INVENTION
This invention concerns a method for weaving cloths with a weaving pattern, and weaving machines designed to use this method. More specifically, by weaving pattern is meant all weaving patterns which can be carried out in a cloth, such as the weft pattern, the binding pattern and the cloth take-up pattern or a combination of these patterns, which as is known can be created respectively by working with different weft threads, by using different bindings and by using different cloth take-up speeds.
Weaving patterns in which different pattern areas are formed successively are well known. The fact that different pattern areas are formed successively has the disadvantage that, at least with the ordinary working methods, the appearance of the cloth is not optimum for all pattern areas. Especially in the transitions between the various pattern areas, i.e. whenever there is a change in the cloth take-up pattern and/or the weft pattern and/or the binding pattern, faults can appear in the cloth, such as marks in the cloth.
SUMMARY OF THE INVENTION
The present invention has as its aim a method for weaving cloths with any of the above-mentioned weaving patterns which offers a solution to the above-mentioned disadvantages, so that a cloth of that sort can be woven flawlessly, and as a result with a cloth appearance of extremely good quality.
For this purpose, the present invention concerns a method for weaving cloths with a weaving pattern, according to which warp threads are supplied and weft threads are bound into them, so that according to the preset weaving pattern, different pattern areas can be formed successively, characterized in that the warp tension is regulated during weaving according to a reference value and that this reference value is controlled in such a manner during weaving that its variation is a function of the different pattern areas to be formed according to the weaving pattern. In other words, this means that the variations in the warp tension pattern are carried out simultaneously or practically simultaneously with the transitions in the cloth or with the variations in the weaving pattern. It is obvious that according to this method the most suitable warp tension for the pattern area being woven can always be selected. The desired optimum warp tension as a function of the weaving pattern to be woven can be determined in advance by experience or on the basis of tables, etc.
The present invention also concerns a weaving machine which uses the above-mentioned method. In this weaving machine, the selected, and thus known weaving pattern is used to set the reference values for the warp tension, whereby regulating the actual warp tension is preferably done by controlling the warp let-off motor of the warp let-off. In order to achieve this, the actual warp tension is measured and the warp let-off motor is controlled in such a way, by means of a feed-back mechanism, that the difference between the measured value and the reference value is regulated to nil.
In order to better explain the characteristics of the invention, the following embodiments are described by way of example, without being limitative in any way, with reference to the drawings, where:
FIG. 1 shows a section of a cloth in which a number of variations which may appear in a weaving pattern are represented;
FIG. 2 shows a schematic illustration of a weaving machine according to the invention;
FIG. 3 shows an example of a setting of the warp tension according to the invention, in particular for the cloth in FIG. 1;
FIG. 4 shows the trigger signal of the weaving machine;
FIG. 5 shows a view of a warp tension gauge, more specifically in the direction of the arrow F5 in FIG. 2;
FIG. 6 shows a variant of the warp tension gauge according to FIG. 5.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a cloth 1 with a weaving pattern. As is known, such a weaving pattern extends over a certain cloth length W and is made up of different pattern areas A, B, C, D and E, whereby the cloth 1 is uniform within this pattern area. The transitions between the successive pattern areas are indicated by references P0 to P5.
At point P1, there is a change in the cloth take-up pattern, more specifically due to an increased speed of the cloth take-up, as a result of which the weft threads 2 are farther away from each other.
At point P2, there is a change in the weft pattern, which in the given example has been caused by a switch to a different sort of weft threads 2A which are thinner.
At point P3, there is a change in the binding pattern, i.e. the weft threads 2A are e.g. woven into the warp threads 3 in a different way in pattern area D than in pattern area C.
At point P4, there is a change in both the weft and the binding.
Finally, at point P5 there is again a change in the weaving pattern because of a change in the cloth take-up pattern, due to for example a lowering of the speed of the cloth take-up. At that point, P5, a new similar cloth length W begins.
In order to obtain an optimum cloth appearance and to prevent the formation of cloth marks near the points P1 to P5, the warp tension is regulated in accordance with a reference value R according to the invention, which is described hereafter and which, in its turn, is controlled during weaving as a function of the character of the pattern areas A to E to be woven and the character of the transitions P0 to P5 between the successive pattern areas. It is clear that all sorts of changes in the weaving pattern can be taken into account, i.e. changes which result either from the binding or shedding pattern, the weft pattern, the cloth take-up pattern or a combination of two or more of said types of patterns.
FIG. 2 shows a schematic illustration of a weaving machine which is specially designed for weaving according to the method of the present invention. The conventional parts of a weaving machine are, as is known: the warp beam 4; the warp let-off motor 5; the warp 6; the backrest roller 7, provided with a spring-damping device 8; the harnesses 9; the harness motion, which consists for example of a dobby 10 which moves the harnesses 9 up and down according to the preset binding pattern; the sley 11 with the reed 12; the main drive motor 13; the insertion means 14 which make it possible to insert the weft threads 2-2A into the shed 15 according to the selected preset weft pattern; the breast beam 16; the cloth take-up motion 17 consisting of the sand beam 18, the counter roller 19 and the controllable motor 20 for the sand beam, which can make the speed of the cloth take-up vary according to the selected preset cloth take-up pattern; the cloth beam 21 and the motor 22 to drive the cloth beam 21. The general control unit 23 which controls said parts of the weaving machine is also indicated, as well as the conventional pulse generator 24 which emits a certain number of pulses, ten for example, per rotation of the main drive shaft, i.e. per weft insertion.
It is clear that in the case of an airjet weaving machine, by said insertion means 14 are meant the color selector and the main nozzles. In the case of a rapier weaving machine, by insertion means 14 are meant the thread presentation mechanism and the rapiers which introduce weft threads 2-2A into the shed 15.
The weaving pattern to be woven can be entered by means of an input device 25, for example on a data storage medium or by reading it into a memory. According to the data read in, the control unit 23 controls the parts of the weaving machine which determine the weaving pattern, i.e. in the example given above the dobby 10, the insertion means 14 and the motor 20 in the desired order, by means of control signals 26, 27 and 28 respectively. According to the present invention, a control unit 23 is used which also emits a signal 29 according to the weaving pattern read in, representing a reference value R which gives the optimum desired warp tension for that current weaving pattern. This signal 29 is transmitted to a control element 30, which also receives a signal 31 from a warp tension gauge 32, representing the current warp tension. The control element 30 emits a control signal 33 and controls the motor 5 of the warp let-off such that the tension in the warp 6 takes the value demanded by the signal 29. In order to achieve this the warp tension is continually measured by means of said warp tension gauge 32, such that the measured tension, according to signal 31, tends towards the current reference value R. This also means that the control signal 33 is always in accordance with, and preferably in proportion to, the difference between the signal 29 and the signal 31. The motor 5 of the warp let-off is controlled in a way that its speed is in proportion to said difference.
FIG. 3 shows the possible variation of said reference value R for the cloth in FIG. 1 according to the number of crank angle degrees X of the main shaft of the weaving machine. It is clear that for each change at point P1 to P5 in the weaving pattern, another reference value R for the warp tension will normally have to be set in order to obtain an optimum cloth appearance.
The curve R1 in FIG. 3 shows a rather theoretical variation of the selected reference value. The reference value R1 is varied at the moments corresponding to P1 to P5. Because of the inertia of the regulation system, which consists of a control element 30 which, as mentioned before, emits a control signal 33 according to the difference between the signal 29 and the signal 31, it is advisable, however, for the reference value R, i.e. the signal 29, to be controlled in advance, as shown by the curve R2; this has the advantage that the changes in the actual warp tension virtually occur at the right moment, i.e. when the transitions P1 to P5 occur in the cloth. In order to counter the inertia of said system, it is also possible to build in a brief amplitude overshoot in the variation of the reference value, as shown in curve R3. In this way, the warp tension actually obtained will respond very quickly to the signal 29.
The variations of the curves R1, R2 or R3 as mentioned above can be stored in the memory of the control unit 23. In order to make the variation of the reference value R which is produced by signal 29, and which represents the desired warp tension, synchronous with the control of the weaving machine parts which determine the weaving pattern, use is made of the trigger signal Tr, produced by the pulse generator 24 mounted on the main shaft of the weaving machine. This signal Tr is represented schematically in FIG. 4 as a function of the number of crank angle degrees X of the main shaft. In order to effect the changes in the reference values according to the curves R1, R2 or R3, the number of pulses per cloth length W can be counted, whereby a certain pulse can be used to supply the exact reference value R to the control element 30 at the right moment. If the trigger signal emits ten pulses per rotation of the main shaft, as in FIG. 4, the signal 29 can be corrected every tenth of the weft insertion cycle, according to the selected variation of the reference value R.
In the example shown in FIGS. 3 and 4, in the case where the curve R1 is used, the thirty-first pulse N31 is the signal for changing the reference value R at the transition P1. In the case where the curve R2 is used, the reference value R is changed at the transition P1 at the twenty-third pulse N23. In the case where the curve R3 is used, the reference value R is changed at the transition P1 according to the given function variation at each pulse from the sixteenth pulse N16 up to the thirty-sixth pulse N36. A similar reasoning applies to the transitions P2 to P5.
It is obvious that according to the present invention it is not necessary to enter the variation of the reference value R in the control unit 23, but the data for controlling the weaving machine parts 10, 14 and 20 which determine the weaving pattern should however be entered. For this purpose, the control unit 23 can be equipped with interpretation means, for example an appropriate program, which make it possible to automatically determine the most favourable variation of the reference value R on the basis of the data entered for controlling said weaving machine parts.
It is also obvious that the variation of the reference value R (R1, R2, R3) between the successive transitions P0 to P5 does not necessarily have to be horizontal.
An important characteristic of the present invention is that to measure the actual warp tension, a very sensitive measuring device is used in order to limit time delays. Therefore, warp tension gauge 32 should preferably be of the type represented in FIG. 5. This warp tension gauge 32 includes three thread guides 36, 37 and 38, mounted on a support 35 attached to the frame 34 of the weaving machine, and which operate on only a part 39 of the warp 6. The warp threads of this part 39 pass under the thread guides 36 and 37 and over the thread guide 38, such that the pressure exerted on the thread guide 38 represents the tension in the warp 6. According to FIG. 5, this pressure is measured by means of a pressure-sensitive element 40, for example a piezoelectric crystal which supports the thread guide 38 and emits a signal 31 which is a function of said pressure.
FIG. 6 shows a variant of the warp tension gauge 32. Three thread guides 41, 42 and 43 are also used here. The warp threads of the part 39 pass over the outer thread guides 41 and 42, and under the thread guide 43 positioned between the two latter, such that an upward force is exerted on them. The middle thread guide 43 is mounted on an elastic lever 44 whose inflection is measured by means of a strain gauge 45 which provides a signal 31 proportional to the tension in the warp 6 by means of a measuring device 46.
It is obvious that said signal 31 can represent either the instantaneous warp tension or the average warp tension over a certain period of time.
The present invention is not restricted to the embodiments described by way of example and shown in the accompanying drawings; on the contrary, such a method for weaving cloths with one of said weaving patterns and the weaving machines which use these methods can be made in several sorts of variants while still remaining within the scope of the invention.
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A method of weaving cloth having a weaving pattern which varies according to which warp threads are supplied and according to which weft threads are bound into the warp threads, includes the steps of forming successive different pattern areas and regulating the warp tension according to a reference value during weaving such that its variation is a function of the different pattern areas to be formed. Control of the reference value is accomplished by determining a reference value for the warp tension as a function of the weaving pattern, and regulating the warp tension by measuring the actual warp tension, comparing the measured warp tension with the reference value, and controlling the motor of the let-off such that the difference between the reference value and the measured warp tension is regulated to zero. A weaving machine is arranged to carry out each of the above method steps.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims priority of Chinese Patent Application No. 200520054965.5 filed on Feb. 19, 2005, entitled “Portable Clothes Washer” which is incorporated herein by reference for all purposes.
TECHNICAL FIELD
[0002] The present invention relates to a clothes-washing apparatus, and more particularly, to a portable clothes washer.
BACKGROUND OF THE INVENTION
[0003] Generally, clothes-washing apparatus in the present market include domestic or commercial clothes-washing machines, which are bulky and not portable. A portable clothes-washing apparatus is present in the market for people who travel for business or pleasure, e.g. a portable impeller-type clothes-washing machine including a wash tub assembly and a bottom assembly, wherein said wash tub assembly includes a handle, a top cover, a tub body and an impeller; said bottom assembly includes a base, a motor, a retarder and a controller. As compared to traditional clothes-washing machines, said portable impeller-type clothes-washing machine has following advantages: 1. The wash tub assembly is much smaller in size; 2. When not in use, the bottom assembly can be put into the tub body so as to save the occupied space. With this type of clothes-washing machine, to wash clothes of 0.5 Kg, a 300 mm high tub body with 200-300 mm diameter is needed; such a large tub body is still too big and not convenient to be carried for outgoing. Meanwhile, said clothes-washing machine implements clothes washing only by the rotation of the impeller, which is unitary in washing modes.
[0004] It is undue wasteful to use the present domestic or commercial clothes-washing machines in some cases, e.g., for people putting up in a hotel who have little clothes to be washed, or for people staying at home who need to specifically wash a few clothes (e.g. socks). Therefore, in the present hotels, a washstand or a bathtub is usually provided, but a clothes-washing machine is not provided in each room, and it is not convenient to wash clothes for the guests.
SUMMARY OF THE INVENTION
[0005] The object of the present invention is to provide a compact and less costly portable clothes washer by integrating a wash component with a control component while eliminating the tub body, so as to overcome the above-mentioned shortcomings of the prior clothes-washing machines.
[0006] A portable clothes washer according to the present invention, comprises a control component, a wash component, a shell for carrying said control component and said wash component; wherein said control component is electrically connected with said wash component, so that said wash component can be operated by controlling said control component; and wherein said wash component can produce mechanical rotations or physical vibrations, by which said wash component impacts on a wash medium outside said shell so as to implement a function of washing clothes.
[0007] Wherein said wash medium may be a liquid.
[0008] Wherein said wash component is an ultrasonic generator or a mechanical agitator or the combination of both.
[0009] Wherein said ultrasonic generator includes a vibration plate and an ultrasonic transducer.
[0010] Wherein said mechanical agitator includes a driving device and an impeller, said driving device is disposed inside said shell, said impeller is disposed outside said shell.
[0011] Wherein said portable clothes washer further comprises a clamp for clamping onto external upholders.
[0012] Wherein said shell is designed into an elongated stick, with the wash component disposed at one end of the shell, and the opposite end of the shell is designed into a shape convenient for hand-holding or is equipped with a handle.
[0013] Wherein said wash component and said control component may be disposed inside different shells respectively, so as to form a wash part and a control part which are detachably connected, and when they are mechanically connected, said wash part and said control part are also electrically connected.
[0014] Wherein said portable clothes washer may include one control part and more than one wash parts, and each of said wash parts may be detachably connected with said control part, and they are also electrically connected when they are mechanically connected.
[0015] In use of the present invention, clothes to be washed are put into a cleaning solvent, such as water or other solutions, in an external washstand or bathtub, when necessary a strong sterilization detergent may be further added to said cleaning solvent, and the wash component disposed at the end of the shell is immerged into the cleaning solvent, so as to wash clothes. Moreover, a clamp may be installed on the shell when necessary, so that the whole clothes washer may be clamped onto external washing receptacles or other upholders, e.g. a tap.
[0016] Since the bulky tub body of the prior clothes-washing machine is eliminated, the portable clothes washer of the present invention is less costly, and is compact and convenient for users to put into a traveling bag. Moreover, since a washing receptacle, like a washstand or a bathtub, is provided in service sites like hotels, the portable clothes washer of the present invention can be widely used.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] FIG. 1 is a schematic view of the portable clothes washer according to embodiment 1 of the present invention;
[0018] FIG. 2 is a schematic view of the portable clothes washer according to embodiment 2 of the present invention;
[0019] FIG. 3 is a schematic view of the portable clothes washer according to embodiment 3 of the present invention;
[0020] FIG. 4-1 is a schematic view of the control part of the portable clothes washer according to embodiment 4 of the present invention;
[0021] FIG. 4-2 is a schematic view of a wash part of the portable clothes washer according to embodiment 4 of the present invention;
[0022] FIG. 4-3 is a schematic view of another wash part of the portable clothes washer according to embodiment 4 of the present invention;
[0023] FIG. 4-4 is a schematic view of another wash part of the portable clothes washer according to embodiment 4 of the present invention;
[0024] FIG. 5 is a schematic view of the portable clothes washer according to embodiment 5 of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Embodiment 1
[0025] In this embodiment, a portable clothes washer adopts ultrasonic technology and makes use of cavitation effect of high frequency mechanical oscillations so as to implement the function of washing clothes. Wherein the wash component is constructed by a vibration plate 101 and an ultrasonic transducer 102 .
[0026] As shown in FIG. 1 , the clothes washer is in the shape of a stick, comprising a vibration plate 101 , an ultrasonic transducer 102 , a shell 103 , a controller 104 , a switch 105 of the controller 104 , and a clamp 106 . Wherein the vibration plate 101 is installed at one end of the shell 103 , the ultrasonic transducer 102 is fixed with the vibration plate 101 , the ultrasonic transducer 102 is electrically connected with the controller 104 , the controller 104 is disposed inside the shell 103 , and the switch 105 is installed on the outer wall of the shell 103 . The other end of the shell 103 , which is opposite to the end where the vibration plate 101 is located, is designed with a neck for hand-holding. The clamp 106 may be clamped onto the shell 103 when necessary. The numerals 107 and 108 in FIG. 1 refer to the locations for hand-holding and clamping respectively.
[0027] Furthermore, the portable clothes washer may be provided with accessories such as a strong sterilization detergent.
[0028] The working principle of this embodiment is as follows:
[0029] The portable clothes washer removes the dirt by “cavitation effect” of ultrasonic wave. The so-called “cavitation effect” is formed as follows: high frequency oscillation signals emitted from an ultrasonic generator are converted into high frequency mechanical oscillations by a transducer and propagate to the wash medium, namely the cleaning solvent; the ultrasonic wave radiates forwards sparsely and densely alternately in the liquid, and makes the liquid to flow so as to form thousands of tiny bubbles, which are formed and grow up in the region of negative pressure, and collapse rapidly in the region of positive pressure.
[0030] In this embodiment, the controller 104 is started by turning on the switch 105 , high frequency oscillation signals are produced by the controller 104 , then the signals are converted into high frequency mechanical oscillations by the transducer 102 , and the vibration plate 101 vibrates as well because the transducer 102 and the vibration plate 101 are fixed together. When the vibration plate 101 moves forward, the cleaning solvent, e.g. water, is pushed forward; on the other hand, when the vibration plate 101 moves backward, the water cannot catch up with the moving velocity of the vibration plate, and a gap is formed between the water and the vibration plate, so that many bubbles will be produced during vibration. These cavitation formed bubbles propagate in the water along the vibration direction, and an instant high pressure of over 1000 atmospheric pressure will be formed when the bubbles collapse; the process of continuously producing instant high pressure is like that a series of “explosions” impact on the clothes uninterruptedly, which makes the dirt striped from the surface and cracks of the clothes so as to implement the function of washing clothes. Meanwhile, the cleaning solvent itself impacts on the dirt as well because the cleaning solvent also vibrates ultrasonically.
[0031] Since it will be tiring for holding the stick-shaped clothes washer for a long time, the clamp 106 may be put on in case of long-time washing, then the clothes washer may be directly clamped to an external washing receptacle or a rigid object nearby, e.g. a tap, and the user only needs to operate the switch of the clothes washer without holding the clothes washer.
[0032] If the strong sterilization detergent is added into the cleaning solvent additionally, the ultrasonic wave will facilitate the chemical dissolution of the dirt by the sterilization detergent, by way of combining the physical effect of the ultrasonic oscillation with the chemical effect of sterilization detergent, the washing process will be sped up greatly.
Embodiment 2
[0033] A portable clothes washer of this embodiment is shown in FIG. 2 . As compared to embodiment 1, the difference is that, in this embodiment, the wash component adopts an impeller driven by a motor. The details are as follows:
[0034] The portable clothes washer of this embodiment comprises an impeller 201 , a retarder 202 , a motor 203 , a shell 204 , a controller 205 , a switch 206 of the controller 205 , and a clamp 207 . Wherein the switch 206 is installed on the outer wall of the shell 204 , the rotation direction and intermittent of the motor 203 is controlled by the controller 205 , the output speed from the motor 203 is reduced by the retarder 202 , and the rotation speed of the impeller 201 is lower. The impeller 201 is installed at one end of and outside the shell 204 , and in turn in the shell 204 are disposed the retarder 202 , the motor 203 and the controller 205 . Similarly to that in embodiment 1, the other end of the shell 204 , opposite to the location where the impeller 201 is located, is designed with a neck for hand-holding. The clamp 207 may be clamped onto the shell 203 when necessary. The numerals 208 and 209 in FIG. 2 refer to the locations for hand-holding and clamping respectively.
[0035] Said impeller 201 is situated outside the shell 204 , and comprises a cover and a rotary wheel, wherein said rotary wheel having one or more vanes. Said rotary wheel and vanes are in direct contact with cleaning solvent for washing clothes.
[0036] The working principle of this embodiment is as follows:
[0037] The impeller 201 is driven to rotate by the motor 203 , so that the cleaning detergent can be dissolved adequately to effect the function of washing, the details are as follows:
[0038] The controller 205 is switched on by the switch 206 . When the controller 205 works, the motor 203 is driven to rotate at a high speed, including a positive rotating, a reversal rotating and intermitting. The output speed from the motor 203 is reduced by the retarder 202 , and the impeller 201 is driven to rotate at a lower speed, implementing a repeated motion cycle including positive rotation, intermittent, reversal rotation, intermittent. The cleaning process is as follows: the impeller 201 drives the clothes to rotate, and the dirt is wiped off the clothes by the centrifugal force produced; meanwhile the rotation of the clothes makes the dirt and the cleaning detergent to contact more quickly and thoroughly so that the chemical effect of the cleaning detergent is enforced and the dirt will be better dissolved.
[0039] The operation method of the clamp 207 is the same as that in embodiment 1.
Embodiment 3
[0040] A portable clothes washer of this embodiment is shown in FIG. 3 . As compared to embodiment 1 and embodiment 2, the difference is that, in this embodiment, the wash component is a combination of the ultrasonic washing means and the impeller washing means, which are integrated into the same shell; so that, different washing modes can be chosen according to specific conditions, which is more convenient for users. The details are as followings:
[0041] The portable clothes washer of this embodiment comprises a shell 301 ; an impeller washing means including a motor switch 302 , a motor controller 303 , a motor 304 , a retarder 305 , an impeller 306 ; and an ultrasonic washing means including a transducer switch 307 , a transducer controller 308 , an ultrasonic transducer 309 , a vibration plate 310 ; and a clamp 311 . Wherein the structure and working principle of the ultrasonic washing means and the impeller washing means are the same as those in embodiment 1 and in embodiment 2 respectively. The difference is that, in this embodiment, the two different washing means are integrated into a same shell 301 , and the vibration plate 310 and impeller 306 are placed at the same end of the shell 301 .
[0042] Similarly, the other end of the shell 301 , opposite to the location where the vibration plate 310 and the impeller 306 are located, is designed with a neck for hand-holding. The clamp 311 may be clamped onto the shell 301 when necessary. The numerals 312 and 313 in FIG. 3 refer to the locations for hand-holding and clamping respectively.
[0043] The working principle of this embodiment is as follows:
[0044] With two separate switches, the clothes can be washed either using one of these two different washing means or both of them. The washing process is the same as that in embodiment 1 or embodiment 2 if only one of these washing means is used. If the two washing means are used simultaneously, the rotation of the impeller 306 will reinforce the washing effect of the ultrasonic wave, in addition to the specific washing effect of each of the two washing means. Since there is an optimum range for the effect of caviation bubbles formed by high frequency mechanical oscillations produced by an ultrasonic wave, if these bubbles are too far from the vibration plate 310 , the effect of “bombing” formed by bubbles collapsing will damp; while the impeller 306 will bring different clothes within the optimum range of the vibration plate 310 when it rotates, and different parts of clothes can be impacted by the ultrasonic vibration, so that the dirt drops easily to attain a better washing effect. Double washing mode is more suitable and has better effect in case there are more clothes and there is a bigger washing receptacle.
[0045] The operation method of the clamp 311 is the same as that in embodiment 1.
Embodiment 4
[0046] A portable clothes washer of this embodiment is shown in FIGS. 4-1 , 4 - 2 , 4 - 3 , 4 - 4 . As compared to embodiment 1, embodiment 2 and embodiment 3, the difference is that, in this embodiment, the control component and wash component are disposed in two separate shells respectively, and the two parts are detachably connected and can be replaced easily. The details are as follows:
[0047] The portable clothes washer of this embodiment comprises a control part and three interchangeable wash parts.
[0048] As shown in FIG. 4-1 , the control part comprises a shell, a clamp 405 , a mode selection switch 406 , an electric socket 416 , a controller 407 for an ultrasonic wave washing component and a controller 408 for an impeller type washing component, wherein the two controllers 407 and 408 can be selected to be switched on by the mode selection switch 406 , including only ultrasonic wave mode, only impeller mode, and ultrasonic wave plus impeller mode. The electric socket 416 is disposed at one end of the shell, and the opposite end of the shell is designed with a neck for hand-holding. The clamp 405 may be clamped onto the shell when necessary. The numerals 414 and 415 in FIG. 4-1 refer to the locations for hand-holding and clamping respectively.
[0049] As shown in FIG. 4-2 , a wash part includes a shell, an electric connector 4216 , an ultrasonic transducer 4209 and a vibration plate 4210 . As shown in FIG. 4-3 , another wash part includes a shell, an electric connector 4316 , a motor 4311 , a retarder 4312 and an impeller 4313 . As shown in FIG. 4-4 , another wash part includes a shell, an electric connector 4416 , an ultrasonic transducer 4409 and a vibration plate 4410 , a motor 4411 , a retarder 4412 and an impeller 4413 .
[0050] Each of the electric connectors of different wash parts is engageable with the electric socket 416 of the control part, so that the control part can be engaged with one of the wash parts in use, and the different wash parts are interchangeable and can be replaced according to desire.
[0051] The working principle is as follows:
[0052] In use, choose a suitable wash part, and connect it with the control part. When the wash part of FIG. 4-2 is assembled with the control part, a portable clothes washer as that in embodiment 1 is formed. When the wash part of FIG. 4-3 is assembled with the control part, a portable clothes washer as that in embodiment 2 is formed. When the wash part of FIG. 4-4 is assembled with the control part, a portable clothes washer as that in embodiment 3 is formed. Choose an appropriate mode by the mode selection switch 406 , then the portable clothes washer will work as in embodiments 1, 2 and 3 respectively.
[0053] According to demands of different users and taking into consideration of the cost, the portable clothes washer may include only one or more than one wash parts as shown in FIGS. 4-2 , FIG. 4-3 , FIG. 4-4 .
[0054] Since this embodiment adopts a detachable structure, the portable clothes washer is further shortened and more convenient for carrying.
Embodiment 5
[0055] A portable clothes washer of this embodiment is shown in FIG. 5 . As compared to embodiment 1, the difference is that, in this embodiment, a sucking disc 506 is adopted instead of the clamp.
[0056] In use, the portable clothes washer can be fixed to a washstand or a bathtub by the sucking disc 506 .
[0057] The above description is for the purpose of illustration and is not intended to limit the invention specifically to those embodiments. Rather, the invention is intended to cover all that is included within the spirit and scope of the invention, including variations, modifications, additions, alternatives and the like made by one having ordinary skill in the art.
|
The present invention discloses a portable clothes washer by integrating a wash component with a control component while eliminating the tub body. The present invention is less costly, and is compact, convenient for users to put into a traveling bag, and can be widely used in service sites like hotels.
| 3
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RELATED APPLICATIONS
[0001] Pursuant to 35 U.S.C. §119(e), this application claims the benefit of the filing date of Provisional U.S. Patent Application Ser. No. 61/207,670 filed on Feb. 13, 2009. This application is a continuation application of PCT/JP2007/073935 filed on Dec. 12, 2007. The entire contents of these applications are hereby incorporated by reference.
TECHNICAL FIELD
[0002] The present invention relates to a semiconductor device, and more specifically to a semiconductor device having a surrounding gate transistor (SGT) which is a three-dimensional semiconductor.
BACKGROUND ART
[0003] Through miniaturization of semiconductor devices using a planar transistor, the planar transistor is used in a wide range of fields, such as computers, communication devices, measurement devices, automatic control devices and domestic devices, as a low-power consumption, low-cost, high-throughput microprocessor, an ASIC, a microcomputer, and a low-cost, large-capacity memory. However, the planar transistor is two-dimensionally formed on a plane of a semiconductor substrate. Specifically, the planar transistor has a structure where a source, a gate and a drain thereof are arranged along a surface of a silicon substrate in a horizontal direction. In contrast, the SGT has a structure where a source, a gate and a drain thereof are arranged in a direction perpendicular to a surface of a silicon substrate while allowing the gate to surround a convex-shaped semiconductor layer (see, for example, FIG. 20 in the following Non-Patent Document 1). Therefore, the SGT can largely reduce an occupancy area as compared with the planar transistor. However, in the SGT, along with miniaturization of ultra-large-scale integrated circuits (ULSI), a gate length becomes shorter to provide a lower channel resistance, whereas, as a silicon pillar becomes miniaturized, a diffusion-layer resistance and a contact resistance, i.e., a parasitic resistance, become larger to cause a reduction in drive current. Thus, in a miniaturized SGT device, it is essential to further reduce a parasitic resistance.
[0004] There has been known a technique of reducing a contact resistance as a parasitic resistance of source and drain regions to achieve a higher-speed operation of the device, as disclosed, for example, in the following Patent Document 1. FIG. 21 shows an SGT structure disclosed in the Patent Document 1, which is intended to reduce the contact resistance. In an SGT, along with scaling down of a silicon pillar, a contact area between the silicon pillar and a contact to be connected to a top of the silicon pillar becomes smaller to cause an increase in contact resistance. Consequently, a drive current of the SGT is reduced. As measures against this problem, the Patent Document 1 discloses a structure for increasing the contact area between the silicon pillar and the contact so as to reduce the contact resistance. Specifically, the structure is configured to allow the contact to come into contact with not only a top surface of the silicon pillar but also a part of a side surface of the silicon pillar, so that the contact area between the silicon pillar and the contact is increased to reduce the contact resistance.
[0005] Non-Patent Document 1H. Takato et al., IEEE transaction on electron device, Vol. 38, No. 3, March 1991, pp 573-578
[0006] Patent Document 1 JP 2007-123415A
[0007] As an SGT structure for reducing the contact resistance, the Patent Document 1 proposes a structure where the contact area between the silicon pillar and the contact is set to become greater than an area of the top surface of the silicon pillar, to reduce the contact resistance. However, in order to actually achieve a higher-speed operation of an SGT constituting a ULSI, it is desirable that the contact resistance is less than a reference resistance of the SGT.
[0008] In view of the above circumstances, it is an object of the present invention to provide a semiconductor device capable of reducing a contact resistance as a parasitic resistance to solve the problem of lowering in operation speed of an SGT.
SUMMARY OF THE INVENTION
[0009] In order to achieve the above object, according to a first aspect of the present invention, there is provided a semiconductor device which comprises: a first silicon pillar formed on a semiconductor substrate; a second silicon pillar formed on the first silicon pillar; a first insulator surrounding a part of a surface of the second silicon pillar; a gate surrounding the first insulator; a third silicon pillar formed on the second silicon pillar; a first silicide surrounding a part of a surface of the first silicon pillar; and a second silicide surrounding a part of a surface of the third silicon pillar, wherein each of a contact resistance formed by the first silicide and the first silicon pillar, and a contact resistance formed by the second silicide and the third silicon pillar, is less than a reference resistance of the semiconductor device.
[0010] According to a second aspect of the present invention, there is provided a semiconductor device which comprises: a second silicon pillar formed on a semiconductor substrate; a first insulator surrounding a part of a surface of the second silicon pillar; a gate surrounding the first insulator; a third silicon pillar formed on the second silicon pillar; and a second silicide surrounding a part of a surface of the third silicon pillar, wherein a contact resistance formed by the second silicide and the third silicon pillar is less than a reference resistance of the semiconductor device.
[0011] According to a third aspect of the present invention, there is provided a semiconductor device which comprises: a first silicon pillar formed on a semiconductor substrate; a second silicon pillar formed on the first silicon pillar; a first insulator surrounding a part of a surface of the second silicon pillar; a gate surrounding the first insulator; and a first silicide surrounding a part of a surface of the first silicon pillar, wherein a contact resistance formed by the first silicide and the first silicon pillar is less than a reference resistance of the semiconductor device.
[0012] As above, the present invention makes it possible to reduce a parasitic resistance of a semiconductor device element to provide a semiconductor device having a high-speed, low-power consumption ULSI.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a bird's-eye view showing a semiconductor device according to a first embodiment of the present invention.
[0014] FIG. 2 is a sectional view of the semiconductor device, taken along the line A-A′ in FIG. 1 .
[0015] FIG. 3 is a top view of the semiconductor device in FIG. 1 .
[0016] FIG. 4 is a sectional view of the semiconductor device, taken along the line B-B′ in FIG. 2 .
[0017] FIG. 5 is a sectional view of the semiconductor device, taken along the line C-C′ in FIG. 2 .
[0018] FIG. 6 is a sectional view of the semiconductor device, taken along the line D-D′ in FIG. 2 .
[0019] FIG. 7 is a graph showing a relationship between a diameter W 1 and a length L 1 of a first silicon pillar 830 for satisfying a condition that a contact resistance formed by a silicide and the first silicon pillar 830 is less than a reference resistance in the semiconductor device in FIG. 1 .
[0020] FIG. 8 is a graph showing a relationship between a diameter W 2 and a length L 2 of a third silicon pillar 820 for satisfying a condition that a contact resistance formed by a silicide and the third silicon pillar 820 is less than a reference resistance in the semiconductor device in FIG. 1 .
[0021] FIG. 9 is a bird's-eye view showing a semiconductor device according to a second embodiment of the present invention.
[0022] FIG. 10 is a sectional view of the semiconductor device, taken along the line A-A′ in FIG. 9 .
[0023] FIG. 11 is a top view of the semiconductor device in FIG. 9 .
[0024] FIG. 12 is a sectional view of the semiconductor device, taken along the line B-B′ in FIG. 10 .
[0025] FIG. 13 is a sectional view of the semiconductor device, taken along the line C-C′ in FIG. 10 .
[0026] FIG. 14 is a graph showing a relationship between a diameter W 2 and a length L 2 of a third silicon pillar 820 for satisfying a condition that a contact resistance formed by a silicide and the third silicon pillar 820 is less than a reference resistance in the semiconductor device in FIG. 9 .
[0027] FIG. 15 is a bird's-eye view showing a semiconductor device according to a third embodiment of the present invention.
[0028] FIG. 16 is a sectional view of the semiconductor device, taken along the line A-A′ in FIG. 15 .
[0029] FIG. 17 is a top view of the semiconductor device in FIG. 15 .
[0030] FIG. 18 is a sectional view of the semiconductor device, taken along the line B-B′ in FIG. 16 .
[0031] FIG. 19 is a sectional view of the semiconductor device, taken along the line C-C′ in FIG. 16 .
[0032] FIG. 20 is a graph showing a relationship between a diameter W 1 and a length L 1 of a first silicon pillar 830 for satisfying a condition that a contact resistance formed by a silicide and the first silicon pillar 830 is less than a reference resistance in the semiconductor device in FIG. 1 .
[0033] FIG. 21 is a bird's-eye view showing one example of a conventional SGT.
[0034] FIG. 22 is a top view of the conventional SGT.
[0035] FIG. 23 is a sectional view of the conventional SGT, taken along the line I-I′ in FIG. 22 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0036] With reference to the drawings, a semiconductor device of the present invention will now be specifically described.
First Embodiment
Semiconductor Device
[0037] FIG. 1 is a schematic bird's-eye view showing a transistor of a semiconductor device according to a first embodiment of the present invention. FIG. 2 is a schematic sectional view taken along the line A-A′ in FIG. 1 , and FIG. 3 is a top view of the transistor in FIG. 1 . FIG. 4 , FIG. 5 and FIG. 6 are a schematic sectional view taken along the line B-B′ in FIG. 2 , a schematic sectional view taken along the line C-C′ in FIG. 2 , and a schematic sectional view taken along the line D-D′ in FIG. 2 , respectively. The semiconductor device according to the first embodiment comprises: a first silicon pillar 830 formed on a first conductive-type semiconductor substrate 100 to have a cross-sectionally circular shape; a second silicon pillar 810 formed on the first silicon pillar 830 to have a cross-sectionally circular shape; a first insulator 310 surrounding a part of a surface of the second silicon pillar 810 ; a gate 210 surrounding the first insulator 310 ; and a third silicon pillar 820 formed on the second silicon pillar 810 to have a cross-sectionally circular shape.
[0038] The second silicon pillar 810 includes a second conductive-type high-concentration impurity region 520 formed as a part of the second silicon pillar 810 , and a second conductive-type high-concentration impurity region 530 formed as a part of the second silicon pillar 810 .
[0039] The semiconductor substrate 100 includes a second conductive-type high-concentration impurity region 510 formed as a part of the semiconductor substrate 100 , and a silicide region (first silicide) 720 formed as a part of the high-concentration impurity region 510 . The semiconductor substrate 100 also has an element isolation region 910 formed therein.
[0040] The third silicon pillar 820 includes a second conductive-type high-concentration impurity region 540 formed as a part of the third silicon pillar 820 , and a silicide region (second silicide) 710 is formed in the high-concentration impurity region 540 .
[0041] The first silicon pillar 830 includes a second conductive-type high-concentration impurity region 550 formed as a part of the first silicon pillar 830 .
[0042] The semiconductor device according to the first embodiment further comprises a contact 430 formed on the silicide region 720 , a contact 420 formed on the silicide region 710 , and a contact 410 formed on the gate 210 .
[0043] Each of a contact resistance R 1 formed by the first silicon pillar 830 including the high-concentration impurity region 510 and the silicide region 720 formed in the first silicon pillar 830 , and a contact resistance R 2 formed by the third silicon pillar 820 including the high-concentration impurity region 540 and the silicide region 710 formed in the third silicon pillar 830 , is a parasitic resistance. In order to reduce the parasitic resistance, it is preferable that the contact resistances R 1 , R 2 satisfy the following relational formulas (1-1), (1-2) with respect to a reference resistance Rs:
[0000] R1<Rs (1-1)
[0000] R2<Rs (1-2)
[0044] The reference resistance Rs is calculated according to the following formula (1-3) based on a current I (A) which flows between the contact 410 and the contact 430 in the above semiconductor device when 0 (V) is applied to one of the contacts 410 , 430 and V (V) is applied to a remaining one of the contacts 410 , 430 , while applying V (V) to the contact 420 , under a condition that the contact resistance R 1 =0 and the contact resistance R 2 =0:
[0000] Rs=V/I (1-3)
[0045] Specifically, when a length of the gate 210 , a film thickness of the gate oxide layer, and a diameter of the second silicon pillar 810 , are, respectively, 20 nm, 1 nm, and 10 nm, the parasitic resistance R 1 of the first silicon pillar 830 , a contact resistivity ρ C , a sheet resistance ρ D of a first conductive-type impurity region, a circumferential length K 1 of a cross-section of the first silicon pillar 830 , and a height dimension L 1 of the first silicon pillar 830 , satisfy the following formula (1-4), wherein α is expressed as the formula (1-5). Further, given that the circumferential length K 1 (cm) of the cross-section of the first silicon pillar 830 satisfies the following relational formula (1-6) with respect to a diameter W 1 (cm) of the first silicon pillar 830 .
[0000]
R
1
=
ρ
C
α
K
1
coth
(
L
1
α
)
(
1
-
4
)
α
=
(
ρ
C
ρ
D
)
1
2
(
1
-
5
)
K
1
=
π
W
1
(
1
-
6
)
[0046] The parasitic resistance R 2 of the third silicon pillar 820 , a contact resistivity ρ C , a sheet resistance ρ D of a first conductive-type impurity region, a circumferential length K 2 of a cross-section of the third silicon pillar 820 , and a height dimension L 2 of the third silicon pillar 820 , satisfy the following formula (1-7). Further, given that the circumferential length K 2 (cm) of the cross-section of the third silicon pillar 820 satisfies the following relational formula (1-8) with respect to a diameter W 2 (cm) of the third silicon pillar 820 .
[0000]
R
2
=
ρ
C
α
K
2
coth
(
L
2
α
)
(
1
-
7
)
K
2
=
π
W
2
(
1
-
8
)
[0047] The formula (1-4) is assigned to the formula (1-1), and the formula (1-7) is assigned to the formula (1-2), to obtain the following conditional formulas (1-9), (1-10):
[0000]
ρ
C
α
K
1
coth
(
L
1
α
)
<
R
s
(
1
-
9
)
ρ
C
α
K
2
coth
(
L
2
α
)
<
R
s
(
1
-
10
)
[0048] As one example, given that the contact resistivity ρ C and the sheet resistance ρ D , are, respectively, 6.2e-8 (Ω-cm 2 ) and 6.4e-3/W 1 (Ω/sq.), and the current I (A) flowing between the contact 410 and the contact 430 in the above semiconductor device is 44 (μA) when 0 (V) is applied to one of the contacts 410 , 430 and 1 (V) is applied to a remaining one of the contacts 410 , 430 , while applying 1 (V) to the contact 420 , the reference resistance Rs is calculated as 2.3e-8 (Ω) according to the formula (1-3). These values are assigned to the formulas (1-9), (1-10) to obtain the following relational formula (1-11) between the height dimension L 1 of the first silicon pillar 830 and the circumferential length K 1 of the cross-section of the first silicon pillar 830 , and the following relational formula (1-12) between the height dimension L 2 (cm) of the third silicon pillar 820 and the circumferential length K 2 (cm) of the cross-section of the third silicon pillar 820 :
[0000]
1
W
1
3
/
2
coth
(
L
1
W
1
1
/
2
·
3.1
e
-
3
)
<
3.6
e
9
(
1
-
11
)
1
W
2
3
/
2
coth
(
L
2
W
2
1
/
2
·
3.1
e
-
3
)
<
3.6
e
9
(
1
-
12
)
[0049] If these conditional formulas (1-11), (1-12) are satisfied, the formulas (1-1) are satisfied. Thus, the following formulas (1-13), (1-14) are obtained (see FIGS. 7 and 8 ):
[0000]
1
W
1
3
/
2
coth
(
L
1
W
1
1
/
2
·
3.1
e
-
3
)
<
3.6
e
9
⇒
R
1
<
Rs
(
1
-
13
)
1
W
2
3
/
2
coth
(
L
2
W
2
1
/
2
·
3.1
e
-
3
)
<
3.6
e
9
⇒
R
2
<
Rs
(
1
-
14
)
[0050] As another example, given that a circumferential length of the second silicon pillar 810 , each of the circumferential lengths of the third and first silicon pillars 820 , 830 and the gate length are set, respectively, in the range of 8 nm to 100 μm, in the range of 8 nm to 100 μm and in the range of 6 nm to 10 μm. Further, given that the diameter of the second silicon pillar 810 , the contact resistivity ρ C and the sheet resistance ρ D are, respectively, 2.6 nm, 7e-9 (Ω-cm 2 ) and 6.4e-3/W 1 (Ω/sq.), and the current I (A) flowing between the contact 410 and the contact 430 in the above semiconductor device is 11.4 (μA) when 0 (V) is applied to one of the contacts 410 , 430 and 1 (V) is applied to a remaining one of the contacts 410 , 430 , while applying 1 (V) to the contact 420 , the reference resistance Rs is calculated as 9.0e-8 (Ω) according to the formula (1-3). These values are assigned to the formulas (1-8), (1-9) to obtain the following formulas (1-15), (1-16):
[0000]
1
W
1
3
/
2
coth
(
L
1
W
1
1
/
2
·
1.1
e
-
3
)
<
4.3
e
10
(
1
-
15
)
1
W
2
3
/
2
coth
(
L
2
W
2
1
/
2
·
1.1
e
-
3
)
<
4.3
e
10
(
1
-
16
)
[0051] If these conditional formulas (1-15), (1-16) are satisfied, the formulas (1-1), (1-2) are satisfied. Thus, the following formulas (1-17), (1-18) are obtained:
[0000]
1
W
1
3
/
2
coth
(
L
1
W
1
1
/
2
·
1.1
e
-
3
)
<
4.3
e
10
⇒
R
1
<
Rs
(
1
-
17
)
1
W
2
3
/
2
coth
(
L
2
W
2
1
/
2
·
1.1
e
-
3
)
<
4.3
e
10
⇒
R
2
<
Rs
(
1
-
18
)
Second Embodiment
Semiconductor Device
[0052] FIG. 9 is a schematic bird's-eye view showing a transistor of a semiconductor device according to a second embodiment of the present invention. FIG. 10 is a schematic sectional view taken along the line A-A′ in FIG. 9 , and FIG. 11 is a top view of the transistor in FIG. 9 . FIG. 12 is a schematic sectional view taken along the line B-B′ in FIG. 10 , and FIG. 13 is a schematic sectional view taken along the line C-C′ in FIG. 10 . The semiconductor device according to the second embodiment comprises a second silicon pillar 810 formed on a first conductive-type semiconductor substrate 100 to have a cross-sectionally circular shape, and a third silicon pillar 820 formed on the second silicon pillar 810 to have a cross-sectionally circular shape.
[0053] A part of a surface of the second silicon pillar 810 is surrounded by a first insulator 310 , and the first insulator 310 is surrounded by a gate 210 . The second silicon pillar 810 includes a second conductive-type high-concentration impurity region 520 formed as a part of the second silicon pillar 810 , and a second conductive-type high-concentration impurity region 530 formed as a part of the second silicon pillar 810 .
[0054] The semiconductor substrate 100 includes a second conductive-type high-concentration impurity region 510 formed as a part of the semiconductor substrate 100 , and a silicide region (first silicide) 720 formed as a part of the high-concentration impurity region 510 . The semiconductor substrate 100 also has an element isolation region 910 formed therein.
[0055] The third silicon pillar 820 includes a second conductive-type high-concentration impurity region 540 formed as a part of the third silicon pillar 820 , and a silicide region (second silicide) 710 is formed in the high-concentration impurity region 540 .
[0056] The semiconductor device according to the second embodiment further comprises a contact 430 formed on the silicide region 720 , a contact 420 formed on the silicide region 710 , and a contact 410 formed on the gate 210 .
[0057] Differently from the first embodiment, on an assumption that a contact resistance R 1 formed by the semiconductor substrate 100 including the high-concentration impurity region 510 and the silicide region 720 formed in the semiconductor substrate 100 is ignorable, the structure in the second embodiment is designed to satisfy the following formula (2-1):
[0000] R1<<Rs, R 1 <<R2 (2-1)
[0058] In this case, in order to reduce a contact resistance or parasitic resistance R 2 formed by the third silicon pillar 820 including the high-concentration impurity region 540 and the silicide region 710 formed in the third silicon pillar 830 , it is preferable that the contact resistance R 2 and a reference resistance Rs satisfy the following formula (2-2):
[0000] R2<Rs (2-2)
[0059] The reference resistance Rs is calculated according to the following formula (2-3) based on a current I (A) which flows between the contact 410 and the contact 430 in the above semiconductor device when 0 (V) is applied to one of the contacts 410 , 430 and V (V) is applied to a remaining one of the contacts 410 , 430 , while applying V (V) to the contact 420 , under a condition that the contact resistance R 1 =0 and the contact resistance R 2 =0:
[0000] Rs=V/I (2-3)
[0060] Specifically, when a length of the gate 210 , a film thickness of the gate oxide layer, and a diameter of the second silicon pillar 810 , are, respectively, 20 nm, 1 nm, and 10 nm, the contact resistance R of the third silicon pillar 820 , a contact resistivity ρ C , a sheet resistance ρ D of a first conductive-type impurity region, a circumferential length K 2 of a cross-section of the third silicon pillar 820 , and a height dimension L 2 of the third silicon pillar 820 , satisfy the following formula (2-4), wherein α is expressed as the formula (2-5). Further, given that the circumferential length K 2 (cm) of the cross-section of the third silicon pillar 820 satisfies the following relational formula (2-6) with respect to a diameter W 2 (cm) of the third silicon pillar 820 .
[0000]
R
2
=
ρ
C
α
K
2
coth
(
L
2
α
)
(
2
-
4
)
α
=
(
ρ
C
ρ
D
)
1
2
(
2
-
5
)
K
1
=
π
W
2
(
2
-
6
)
[0061] The formula (2-4) is assigned to the formula (2-1) to obtain the following conditional formulas (2-7):
[0000]
ρ
C
α
K
2
coth
(
L
2
α
)
<
R
s
(
2
-
7
)
[0062] As one example, given that the contact resistivity ρ C and the sheet resistance ρ D are, respectively, 6.2e-8 (Ω-cm 2 ) and 6.4e-3/W 1 (Ω/sq.), and the current I (A) flowing between the contact 410 and the contact 430 in the above semiconductor device is 44 (μA) when 0 (V) is applied to one of the contacts 410 , 430 and 1 (V) is applied to a remaining one of the contacts 410 , 430 , while applying 1 (V) to the contact 420 , the reference resistance Rs is calculated as 2.3e-8 (Ω) according to the formula (2-3). These values are assigned to the formula (2-7) to obtain the following relational formula (2-8) between the height dimension L 2 (cm) of the third silicon pillar 820 and the circumferential length K 2 (cm) of the cross-section of the third silicon pillar 820 :
[0000]
1
W
2
3
/
2
coth
(
L
2
W
2
1
/
2
·
3.1
e
-
3
)
<
3.6
e
9
(
2
-
8
)
[0063] If the conditional formula (2-8) is satisfied, the formula (2-1) is satisfied. Thus, the following formula (2-9) is obtained (see FIG. 14 ):
[0000]
1
W
2
3
/
2
coth
(
L
2
W
2
1
/
2
·
3.1
e
-
3
)
<
3.6
e
9
⇒
R
2
<
Rs
(
2
-
9
)
[0064] As another example, given that a circumferential length of each of the second and first silicon pillars 810 , 830 , the circumferential length of the third silicon pillar 820 and the gate length are set, respectively, in the range of 8 nm to 100 μm, in the range of 8 nm to 100 μm and in the range of 6 nm to 10 μm. Further, given that the diameter of the second silicon pillar 810 , the contact resistivity ρ C and the sheet resistance ρ D are, respectively, 2.6 nm, 7e-9 (Ω-cm 2 ) and 6.4e-3/W 1 (Ω/sq.), and the current I (A) flowing between the contact 410 and the contact 430 in the above semiconductor device is 11.4 (μA) when 0 (V) is applied to one of the contacts 410 , 430 and 1 (V) is applied to a remaining one of the contacts 410 , 430 , while applying 1 (V) to the contact 420 , the reference resistance Rs is calculated as 9.0e-8 (Ω) according to the formula (2-3). Thus, the formula (2-7) is expressed as the following formula (2-10):
[0000]
ρ
C
α
K
2
coth
(
L
2
α
)
<
R
s
(
2
-
10
)
[0065] The above values are assigned to the formula (2-10) to obtain the following formula (2-11):
[0000]
1
W
2
3
/
2
coth
(
L
2
W
2
1
/
2
·
1.1
e
-
3
)
<
4.3
e
10
(
2
-
11
)
[0066] If the conditional formula (2-11) is satisfied, the formula (2-1) is satisfied. Thus, the following formula (2-12) is obtained:
[0000]
1
W
2
3
/
2
coth
(
L
2
W
2
1
/
2
·
1.1
e
-
3
)
<
4.3
e
10
⇒
R
2
<
Rs
(
2
-
12
)
Third Embodiment
Semiconductor Device
[0067] FIG. 15 is a schematic bird's-eye view showing a transistor of a semiconductor device according to a third embodiment of the present invention. FIG. 16 is a schematic sectional view taken along the line A-A′ in FIG. 15 , and FIG. 17 is a top view of the transistor in FIG. 14 FIG. 18 is a schematic sectional view taken along the line B-B′ in FIG. 15 and FIG. 19 is a schematic sectional view taken along the line C-C′ in FIG. 15 . The semiconductor device according to the third embodiment comprises: a first silicon pillar 830 formed on a first conductive-type semiconductor substrate 100 to have a cross-sectionally circular shape; a second silicon pillar 810 formed on the first silicon pillar 830 to have a cross-sectionally circular shape; a first insulator 310 surrounding a part of a surface of the second silicon pillar 810 ; a gate 210 surrounding the first insulator 310 ; and a third silicon pillar 820 formed on the second silicon pillar 810 to have a cross-sectionally circular shape.
[0068] The second silicon pillar 810 includes a second conductive-type high-concentration impurity region 520 formed as a part of the second silicon pillar 810 , and a second conductive-type high-concentration impurity region 530 formed as a part of the second silicon pillar 810 .
[0069] The semiconductor substrate 100 includes a second conductive-type high-concentration impurity region 510 formed as a part of the semiconductor substrate 100 , and a silicide region (first silicide) 720 formed as a part of the high-concentration impurity region 510 . The semiconductor substrate 100 also has an element isolation region 910 formed therein.
[0070] The third silicon pillar 820 includes a second conductive-type high-concentration impurity region 540 formed as a part of the third silicon pillar 820 , and a silicide region (second silicide) 710 is formed in the high-concentration impurity region 540 .
[0071] The first silicon pillar 830 includes a second conductive-type high-concentration impurity region 550 formed as a part of the first silicon pillar 830 .
[0072] The semiconductor device according to the third embodiment further comprises a contact 430 formed on the silicide region 720 , a contact 420 formed on the silicide region 710 , and a contact 410 formed on the gate 210 .
[0073] Differently from the first embodiment, on an assumption that a contact resistance R 2 formed by the third silicon pillar 820 including the high-concentration impurity region 540 and the silicide region 710 formed in the third silicon pillar 830 is ignorable, the structure in the third embodiment is designed to satisfy the following formula (3-1):
[0000] R2<<Rs, R2<<Rs (3-1)
[0074] In this case, in order to reduce a contact resistance or parasitic resistance R 1 formed by the first silicon pillar 830 including the high-concentration impurity region 510 and the silicide region 720 formed in the first silicon pillar 830 , it is preferable that the contact resistance R 1 and a reference resistance Rs satisfy the following formula (3-2):
[0000] R 1 <Rs (3-2)
[0075] The reference resistance Rs is calculated according to the following formula (3-3) based on a current I (A) which flows between the contact 410 and the contact 430 in the above semiconductor device when 0 (V) is applied to one of the contacts 410 , 430 and V (V) is applied to a remaining one of the contacts 410 , 430 , while applying V (V) to the contact 420 , under a condition that the contact resistance R 1 =0 and the contact resistance R 2 =0:
[0000] Rs=V/I (3-3)
[0076] Specifically, when a length of the gate 210 , a film thickness of the gate oxide layer, and a diameter of the second silicon pillar 810 , are, respectively, 20 nm, 1 nm, and 10 nm, the contact resistance R 1 of the first silicon pillar 830 , a contact resistivity ρ C , a sheet resistance ρ D of a first conductive-type impurity region, a circumferential length K 1 of a cross-section of the first silicon pillar 830 , and a height dimension L 1 of the first silicon pillar 830 , satisfy the following formula (3-4), wherein α is expressed as the formula (3-5). Further, given that the circumferential length K 1 (cm) of the cross-section of the first silicon pillar 830 satisfies the following relational formula (3-6) with respect to a diameter W 1 (cm) of the first silicon pillar 830 .
[0000]
R
1
=
ρ
C
α
K
2
coth
(
L
1
α
)
(
3
-
4
)
α
=
(
ρ
C
ρ
D
)
1
2
(
3
-
5
)
K
1
=
π
W
1
(
3
-
6
)
[0077] The formula (3-4) is assigned to the formula (3-1) to obtain the following conditional formula (3-7):
[0000]
ρ
C
α
K
1
coth
(
L
1
α
)
<
R
s
(
3
-
7
)
[0078] As one example, given that the contact resistivity ρ C and the sheet resistance ρ D are, respectively, 6.2e-8 (Ω-cm 2 ) and 1.6e-3×4/W 1 (Ω/sq.), and the current I (A) flowing between the contact 410 and the contact 430 in the above semiconductor device is 44 (μA) when 0 (V) is applied to one of the contacts 410 , 430 and 1 (V) is applied to a remaining one of the contacts 410 , 430 , while applying 1 (V) to the contact 420 , the reference resistance Rs is calculated as 2.3e-8 (Ω) according to the formula (3-3). These values are assigned to the formula (3-7) to obtain the following relational formula (3-8) between the height dimension L 1 of the first silicon pillar 830 and the circumferential length K 1 of the cross-section of the first silicon pillar 830 :
[0000]
1
W
1
3
/
2
coth
(
L
1
W
1
1
/
2
·
3.1
e
-
3
)
<
3.6
e
9
(
3
-
8
)
[0079] If the conditional formula (3-8) is satisfied, the formula (3-1) is satisfied. Thus, the following formula (3-9) is obtained (see FIG. 20 ):
[0000]
1
W
1
3
/
2
coth
(
L
1
W
1
1
/
2
·
3.1
e
-
3
)
<
3.6
e
9
⇒
R
1
<
Rs
(
1
-
13
)
[0080] As another example, given that a circumferential length of each of the second and third silicon pillars 810 , 820 , the circumferential length of the first silicon pillar 830 and the gate length are set, respectively, in the range of 8 nm to 100 μm, in the range of 8 nm to 100 μm and in the range of 6 nm to 10 μm. Further, given that the diameter of the second silicon pillar 810 , the contact resistivity ρ C and the sheet resistance ρ D are, respectively, 2.6 nm, 7e-9 (Ω-cm 2 ) and 1.6e-3×4/W 1 (Ω/sq.), and the current I (A) flowing between the contact 410 and the contact 430 in the above semiconductor device is 11.4 (μA) when 0 (V) is applied to one of the contacts 410 , 430 and 1 (V) is applied to a remaining one of the contacts 410 , 430 , while applying 1 (V) to the contact 420 , the reference resistance Rs is calculated as 9e-8 (Ω) according to the formula (3-3). Further, given that L 1 =L 2 and K 1 =K 2 , the following formula (3-10) is obtained:
[0000]
ρ
C
α
K
1
coth
(
L
1
α
)
<
R
s
(
3
-
10
)
[0081] The above values are assigned to the formula (3-10) to obtain the following formula (3-11):
[0000]
1
W
1
3
/
2
coth
(
L
1
W
1
1
/
2
·
1.1
e
-
3
)
<
4.3
e
10
(
3
-
11
)
[0082] If the conditional formula (3-11) is satisfied, the formula (3-1) is satisfied. Thus, the following formula (3-12) is obtained:
[0000]
1
W
1
3
/
2
coth
(
L
1
W
1
1
/
2
·
1.1
e
-
3
)
<
4.3
e
10
⇒
R
1
<
Rs
(
3
-
12
)
[0083] In the first to third embodiments, each of the first silicide region 710 and the second silicide region 720 may be made of one selected from the group consisting of nickel (Ni) silicide, platinum (Pt) silicide, erbium (Er) silicide, ytterbium (Yb) silicide and a combination of two or more thereof.
[0084] As mentioned above, the present invention provides a semiconductor device which comprises: a first silicon pillar formed on a semiconductor substrate; a second silicon pillar formed on the first silicon pillar; a first insulator surrounding a part of a surface of the second silicon pillar; a gate surrounding the first insulator; a third silicon pillar formed on the second silicon pillar; a first silicide surrounding a part of a surface of the first silicon pillar; and a second silicide surrounding a part of a surface of the third silicon pillar, wherein each of a contact resistance formed by the first silicide and the first silicon pillar, and a contact resistance formed by the second silicide and the third silicon pillar, is less than a reference resistance of the semiconductor device.
[0085] The present invention can provide a semiconductor device capable of solving problems of increase in power consumption and lowering in operation speed due to an increase in parasitic resistance of an SGT, to achieve high-speed SGT operation and low power consumption.
|
A hermetic compressor includes a closed vessel for storing lubricating oil, an electric-driving element, and a compressing element driven by the electric-driving element. The compressing element includes a cylinder block forming a compression chamber, a piton that reciprocates inside the compression chamber, and an oiling device for supplying the lubricating oil to an outer circumference of the piston. A first oil groove is concavely formed on the outer circumference of the piston, and a second oil groove is concavely formed on a side opposite to the compression chamber relative to the first oil groove. The second oil groove has a spatial volume same or greater than that of the first oil groove. An expanded clearance portion is provided such that a clearance between the piston and the cylindrical hole portion broadens from a top dead point to a bottom dead point.
| 7
|
RELATED APPLICATION INFORMATION
This application is a continuation-in-part of application Ser. No. 60/051,848 filed Jul. 7, 1997, now expired, entitled “Computer Programmable Remote Control System,” which is incorporated herein by reference.
NOTICE OF COPYRIGHTS AND TRADE DRESS
A portion of the disclosure of this patent document contains material which is subject to copyright protection. This patent document may show and/or describe matter which is or may become trade dress of the owner. The copyright and trade dress owner has no objection to the facsimile reproduction by any one of the patent disclosure, as it appears in the Patent and Trademark Office patent files or records, but otherwise reserves all copyright and trade dress rights whatsoever.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to remote control devices for electronics products.
2. Description of Related Art
The modern home may have a wide array of consumer electronics devices. These may include nearly any type of audio or video entertainment product, such as televisions, video cassette recorders, audio cassette recorders, audio/video receivers and preamps, cable boxes, laser disc players and camcorders.
Consumer electronics devices typically utilize hand-held remote control units to permit a user to rapidly and efficiently control selected functions from a distance. Early mechanical/ultrasonic remote control units were fairly limited and generally permitted only one or two functions to be controlled. For example, television remote control units utilizing mechanical/ultrasonic technology generally permitted a user to turn the power on to the television and to cycle through each channel in a preselected rotation. For some time, remote control units have been available which transmit control signals by way of infrared or radio frequency transmitters. These wireless remote control units have freed the user to move about a room or even about their home and to control the device from wherever it is most convenient to the user.
Consumer electronics devices and systems have become very complex and loaded with functionality. Particularly, with the expanding use of microprocessor-based devices and the ability to interconnect audio systems, video systems, security system, home automation systems and personal computers, the possible ways to interconnect and operate device has grown significantly. Remote control units have correspondingly become highly complex. A number of manufacturers sell remote control units which include as many as one hundred small buttons or keys, resulting in a severe decrease in the usability of these devices. This is remarkable, considering the huge number of consumers who cannot set the time on their VCR. Furthermore, the number and complexity of remote control units typically found in a home have reached a level where the convenience provided by the remote control units is often overcome by the difficulty in locating and operating them.
Thus, several problems have arisen. First, there is the problem of how to allow the user to control a huge number of features from a remote control unit. Second, there is the problem of how to avoid overwhelming the user with controls on a remote control unit which the user will never use. Third, there is the problem of users having to deal with multiple remote control units with overlapping operability. Fourth, there is the problem of the considerable amount of space which an aggregation of remote control units often occupy.
One solution which has found some acceptance in the market is the universal remote control unit. A universal remote control unit consolidates multiple remote control units and, it is hoped, improves their usability. Typical universal remote control units can learn the commands of other Remote control units, either through pre-programmed lists of consumer electronics devices or by teaching the universal remote control unit each command which the user might wish to have available on the universal Remote control unit. One of the problems with universal remote control units has been that their generic keypads are often cumbersome and not particularly intuitive in layout or labeling. Furthermore, the designers of these devices must compromise between having separate buttons for each possible command and small button sizes.
With the advent of home theater systems, the complexity of controls has advanced to an even greater plateau. Now, the remote must not only control the TV, the VCR, the cable box and the stereo, it must be able to control the surround sound quality, turn on multiple devices at the same time, and issue a series of commands to multiple devices to accomplish a single task. Naturally, the consumer electronics industry has developed products to serve this new need in the marketplace. These more advanced universal remote control units are exemplified by the Home Producer 8 from Universal Electronics, Inc. (Tustin, Calif.), the RC 2000 from Marantz (Roselle, Ill.), the RR990 from Rotel (North Reading, Mass.), and the RC-R0905 from Kenwood.
There has also been an increasing desire to integrate consumer electronics with security systems and to provide some control from a remote control unit of the home environment. For example, it is desirable that, when a user wishes to watch a cable program, not only is the TV set powered on and set to receive the video input, the A/V receiver is powered on and set to play the cable program at a reasonable loudness, the cable decoder is powered on and set to a favorite channel, but also the room's lighting is dimmed, the air conditioner is set to a comfortable level and the home security system is armed against perimeter violations. Some products (not necessarily Remote control units) are available which can be programmed to do these kinds of things. These products include the HAS-1350 HomeVision Intelligent Home Controller available from Home Automation Systems, Inc. (Irvine, Calif.), the ISR TronArch Intelligent Home Automation System, the BrightTouch from Crestron, the TheaterLink from Vantage, and the Landmark System from PHAST, the IntelliControl from Niles, and the 700T from Lexicon.
One of the common problems with universal remote control units, and a problem which is especially severe with the most flexible and programmable remote control units, is programming. A universal remote control unit simply cannot be factory-programmed with every possible configuration. The user is left with poor choices—do without some functions, spend many hours programming and reprogramming their programmable remote control unit, suffer through a remote control unit which is not programmed in a memorable manner, or paying a professional to program the remote control unit. Despite the availability of programmable remote control units, the best remote control unit for a multimedia processing unit is usually the one which is provided with a multimedia processing unit. It is very difficult to overcome this one-to-one correspondence of remote control units and multimedia processing units. These problems have resulted in the marketplace largely rejecting the more advanced universal remote control units.
SUMMARY OF THE INVENTION
The previously described problems are solved in a remote control unit which has the ability to control nearly any device controllable from a remote, yet is easily programmed. These benefits are obtained from a remote control unit which is programmable from a PC using an advanced, object-oriented user interface. The remote control unit's programming is easily modified from the PC. The user may quickly and easily build a full range of capabilities into the remote control unit, including the issuance of multiple commands with a single key press. Furthermore, because the remote control unit has a large memory, the user may focus on functionality, rather than the efficiency or compactness of the programs.
The present invention, together with additional features and advantages thereof, may best be understood by reference to the following description taken in connection with the accompanying illustrative drawings.
DESCRIPTION OF THE DRAWINGS
Further objects of this invention, together with additional features contributing thereto and advantages accruing therefrom, will be apparent from the following description of a preferred embodiment of the present invention which is shown in the accompanying drawings with like reference numerals indicating corresponding parts throughout and which is to be read in conjunction with the following drawings, wherein:
FIG. 1 is a block diagram showing a PC, a programmable remote control in accordance with the invention and multimedia processing units.
FIG. 2A is a frontal plan view of a prior art programmed remote control unit.
FIG. 2B is a frontal plan view of a programmable remote control unit in accordance with the invention.
FIG. 3 is a screen shot of a selection screen of a remote control development program in accordance with the invention.
FIG. 4 is a screen shot of name entry screen of a remote control development program in accordance with the invention.
FIG. 5 is a screen shot of a command learning screen of a remote control development program in accordance with the invention.
FIG. 6 is a screen shot of another command learning screen of a remote control development program in accordance with the invention.
FIG. 7 is a screen shot of a screen object layout screen of a remote control development program in accordance with the invention.
FIG. 8 is a partial perspective view of a docked programmable remote control unit in accordance with the invention.
FIG. 9 is a screen shot of a screen object layout screen of a remote control development program having commands for multiple multimedia processing units in accordance with the invention.
FIG. 10 is a screen shot of a custom screen object creation screen of a remote control development program in accordance with the invention.
FIG. 11 is a screen shot of another custom screen object creation screen of a remote control development program in accordance with the invention.
FIG. 12 is a flowchart of a method of programming a programmable remote control unit in accordance with the invention.
These and additional embodiments of the invention may now be better understood by turning to the following detailed description wherein an illustrated embodiment is described.
DETAILED DESCRIPTION OF THE INVENTION
Throughout this description, the preferred embodiment and examples shown should be considered as exemplars, rather than limitations on the apparatus and methods of the present invention.
The Components of the System
Referring now to FIG. 1, there is shown a block diagram of a general purpose computer 100 , a programmable remote control unit 200 , a docking station 130 and a multimedia processing unit 300 . By “multimedia processing unit” it is meant a device which provides some functionality which an end user can recognize and appreciate. Most TVs, VCRs, stereo receivers, CD players, laser disk players and cable decoders are self-contained multimedia processing units. Many security systems and home automation systems are dispersed multimedia processing units. By “remote control unit” it is meant a hand-held, portable device which can be used by a user to issue commands to a multimedia processing unit which the multimedia processing unit will recognize and result in a predetermined change of performance by the multimedia processing unit. By “programmed remote control unit” it is meant a remote control unit which has a fixed set of commands which it can issue and which commands are permanently assigned to specific keys on the remote control unit. Most multimedia processing units are provided with a programmed remote control unit which is programmed with all of the commands the multimedia processing unit's engineers believed desirable. By “programmable remote control unit” it is meant a remote control unit which can be programmed with the commands needed to control an multimedia processing unit. By “command” it is meant a message which can be recognized by a multimedia processing unit as an instruction to change a particular setting of the multimedia processing unit.
The multimedia processing unit 300 includes a receiver 310 through which the multimedia processing unit may receive commands.
The general purpose computer 100 includes a processor 155 which preferably from Intel Corporation (San Jose, Calif.) and runs a Microsoft Corporation (Redmond, Wash.) Windows operating system. In conjunction with the processor 155 , the general purpose computer 100 has a short term memory 150 (preferably RAM) and a long term memory 180 (preferably a hard disk) as known in the art. The general purpose computer 100 further includes a graphics display 105 , a user input device preferably comprising a keyboard 120 a and mouse 120 b, an IO interface 115 , a power supply 125 and a bus 110 as known in the art. From the user's perspective, the docking station 130 once connected to the general purpose computer 100 is a component of the general purpose computer 100 .
The programmable remote control unit 200 includes a processor 260 and preferably runs Microsoft Corporation's (Redmond, Wash.) Windows CE operating system. In conjunction with the processor 260 , the programmable remote control unit 200 has a short term memory 270 and a long term memory 250 as known in the art. The processor 260 is preferably a microprocessor, but may be an ASIC, logic processor or other type of processor which can operate in accordance with a program. The long term memory 250 is preferably comprised of EEPROM, but may also be a magnetic disk drive, an optical disk drive, and MO disk drive, NVRAM, SRAM, chemical storage device or other type of rewritable, non-volatile memory. The short term memory 270 is preferably a RAM. The programmable remote control unit 200 further includes a bus 210 , an I/O processor 230 , a power management unit 280 and a battery 285 , all as known in the art.
For interfacing with a user, the programmable remote control unit 200 further includes a panel 220 . The panel 220 comprises various user input devices 222 , 223 , 224 and a graphic display 221 . The graphic display 221 may be an LCD panel, an LED panel, a holographic projection, a cathode ray tube or other compact display device which can display graphics. The user input devices preferably include fixed keys 224 , programmable keys 223 and a touch screen overlay 222 .
The programmable keys 223 and fixed keys 224 may be comprised of buttons—mechanical, electromechanical or solid state. As shown in FIG. 2B, there are preferably four programmable keys 223 a, 223 b, 223 c, 223 d disposed in a cross-like shape. Though programmable, the programmable keys 223 preferably are programmed with consistent functions, namely, that key 223 a is for increasing speaker volume, key 223 b is for changing channels in an upward direction, key 223 c is for decreasing speaker volume, and key 223 d is for changing channels in a downward direction. As explained further below, programs for controlling multimedia processing units preferably include these assignments.
The fixed keys 224 have functions which cannot be changed. The fixed keys 224 preferably include a key 224 a for toggling a back light on the display 221 , keys 224 b, 224 c for scrolling to the next and previous screen, and a power key 224 d.
The touch screen overlay 222 , in conjunction with the graphic display 221 , allows the programmable remote control unit 200 to be programmed with soft keys.
For interfacing with the multimedia processing unit 300 and the general purpose computer 100 , the programmable remote control unit 200 includes a communications transceiver 235 . The communications transceiver 235 may be electro mechanical, but is preferably wireless and conforms to the IrDA specification and consumer IR standards, and also includes an infrared transceiver and an RF transceiver which permit the programmable remote control unit 200 to control a wide range of multimedia processing units. Alternatively, the functions of communicating with the general purpose computer 100 and the multimedia precessing unit may be embodied as separate units.
The docking station 130 preferably comprises a cup-like unit into which the programmable remote control unit 200 may be inserted and which has a shape adapted to receive and firmly hold the programmable remote control unit 200 . FIG. 8 shows the programmable remote control unit 200 inserted into the docking station 130 . When the programmable remote control unit 200 is inserted into the docking station 130 , the programmable remote control unit's communications transceiver 235 is in registration with a corresponding communications transceiver 135 in the docking station 130 . The docking station 130 is coupleable to the I/O interface 115 of the general purpose computer 100 , preferably in conformance with an interface standard which is common, bidirectional and inexpensive, such as serial or USB.
As an alternative to the docking station 350 , the communications transceiver 235 of the programmable remote control unit 200 may include a USB port or similar means which can be connected directly to a USB port in the general purpose computer 100 .
The communications transceiver 135 of the docking station preferably includes an infrared receiver and an RF receiver which permit the docking station 130 to recognize the commands which are recognized by a wide range of multimedia processing units.
The Method of the Invention
Methods of the invention includes a learning phase, a development phase, a transfer phase and a use phase. The description of these phases is accompanied by an example of how the commands issued from a prior art programmed remote control unit 200 A shown in FIG. 2A maybe programmed and used by the programmable remote control unit 200 of FIG. 2 B.
The exemplary programmed remote control unit 200 A is of a common variety for controlling a television, which is the multimedia processing unit of the example. Similar programmed remote control units are provided with other multimedia processing units, such as cable boxes. The programmed remote control unit 200 A includes a number of keys, each resulting in a designated command as shown in Table I below. Typical TVs generate an appropriate display when a key is pressed and the TV recognizes the command. Other multimedia processing units also have similar capabilities, though this is not described further herein.
TABLE I
Label
Reference
Command
mute
220A
toggle the TV's speaker on and off
power
230A
toggle power to the TV on and off
enter
275A
after one or more numbers keys has been
pressed, cause the TV to recognize the
corresponding entered number
1
201A
enter the number 1
2
202A
enter the number 2
3
203A
enter the number 3
4
204A
enter the number 4
5
205A
enter the number 5
6
206A
enter the number 6
7
207A
enter the number 7
8
208A
enter the number 8
9
209A
enter the number 9
0
210A
enter the number 0
ch−
260A
change the displayed TV station to the
station next lower in a predefined order
ch+
265A
change the displayed TV station to the
station next higher in the predefined
order
display
250A
toggle an information display of such
things as currently tuned station, volume,
and the time
vol−
270A
decrease the speaker volume by a
predetermined amount
vol+
275A
increase the speaker volume by a
predetermined amount
In setting up the system of the invention, the user first connects the docking station 130 to the general purpose computer 100 . Preferably, the docking station 130 includes a serial communications cable which may be connected to an open serial port of the I/O interface 115 , or a USB cable which may be connected to an open USB port. The user then installs remote control development software on the hard drive 180 . The remote control development software preferably detects the docking station 130 and determines if the docking station 130 is working correctly. Next, a configuration wizard prompts the user to insert the programmable remote control unit 200 into the docking station 130 and begin the learning phase.
Learning Phase
Referring now to FIG. 12, a method of programming the programmable remote control unit 200 is described and is accompanied with a description of an exemplary embodiment. The remote control development software preferably uses Active X objects technology.
The remote control development software provides the user with the ability to create, edit, delete and download to the programmable remote control unit 200 one or more “screen objects.” A screen object comprises a screen layout definition, soft key objects and programmable key objects, altogether which provide for a single screen which occupies the display 222 and the commands associated therewith. A “soft key object” comprises a graphic or pointer to a graphic representing a soft key which will be displayed on the display 221 , a text label for the graphic, a location on the display 221 for the graphic, and a tagname for command which the programmable remote control unit 200 will issue when the soft key is pressed by the user. A “programmable key object” preferably comprises an identifier of one of the programmable keys 223 and a tagname for a command which the programmable remote control unit 200 will issue when the identified programmable key 223 is pressed by the user.
The remote control development software preferably stores screen objects in a database. The remote control development software preferably is provided with a number of preconfigured screen objects, and during installation of the remote control development software, a database of the preconfigured screen objects is preferably created. Preconfigured screen objects provide a short cut to programming the programmable remote control unit 200 , and may be used as templates in the development phase, discussed below. The preconfigured screen objects can come from an image table or dynamically created by software based upon functionality of the remote and its purpose. The database preferably can differentiate preconfigured screen objects from custom screen objects, and deter the user from editing them.
The publisher of the remote control development software preferably makes available new preconfigured screen objects as new multimedia processing units are put on the market to further increase the ease-of-programming of the programmable remote control unit of the invention. The preconfigured screen objects may also be obtained in the aftermarket from third parties, such as the vendors of multimedia processing units.
In the learning phase, the commands for the multimedia processing unit 300 are obtained by the remote control development software and used to prepare a screen object corresponding to the programmed remote control unit 200 A of the multimedia processing unit 300 . It should be appreciated, however, that the remote control development software can be used to learn commands from multipurpose, universal and programmable remote control units as well as single-purpose programmed remote control units as shown in the example.
In step 1210 , the user starts the remote control development software and activates the wizard for learning the commands for a multimedia processing unit. A screen 300 such as that shown in FIG. 3 is preferably displayed on the display 105 of the general purpose computer 100 . This screen 300 displays the beginning point of the learning wizard. The screen 300 , as well as the other screens described herein, conform to the Windows95 (or later) user interface which is well known in the art. A menu bar 310 shows several commands which a user may select.
The screen 300 includes a prominent dialog 320 . The dialog 320 includes descriptive text and a list of multimedia processing unit types 325 . The dialog 320 also includes a Cancel button 322 and a Help 323 which will be self-evident to those of skill in the art, as well as a Look Up button 324 and a Learn button 325 . A row of radio buttons 321 is provided to permit the user to select the multimedia processing unit type, and there is preferably a free-form field 326 as well. In step 1230 , the user selects one of the displayed multimedia processing unit types or enters a free-form name. As shown further below, the multimedia processing unit type selected here, or the name entered in field 326 , will be used by the remote control development software as a prefix name for the screen object and for the tagnames for the commands in the screen object.
After the user has selected the multimedia processing unit type, the commands of the multimedia processing unit 300 are learned. If the user clicks on the Look Up button 324 (step 1290 ), the remote control development software allows the user to select the multimedia programming unit from the database of screen objects (step 1295 ). Accordingly, the remote control development software displays a list of preconfigured screen objects, sorted or limited according to characteristics such as multimedia processing unit type, manufacturer, and date of manufacture. The user may then select one of the preconfigured screen objects, and learning of the commands of the multimedia processing unit 300 is complete (step 1280 ).
If the user clicks on the Learn button, the individual keys of the programmed remote control 200 A will be learned (steps 1240 - 1265 ). In this regard for example, the remote control development software displays a dialog 420 as shown in FIG. 4 . The dialog 420 includes the buttons 322 , 323 as well as a Back button 424 and a Next button 425 .
The user now enters the name of the multimedia processing unit 300 whose commands are to be learned (step 1240 ). Dialog 420 includes a prompt 425 and a data entry field 435 where the user enters the name of the multimedia processing unit 300 . The remote control development software preferably provides a default name for the multimedia processing unit 300 in the field 435 . This default name preferably comprises the type of multimedia processing unit selected in step 1210 , plus a sequential number for each multimedia processing unit of the type learned. The remote control development software also preferably utilizes the multimedia processing unit type in the prompt 425 .
Preferably, remote control development software is intelligent enough to save the user from teaching every key of the programmed remote control unit 200 A. In this regard, after the user teaches the remote control development software each new key, the remote control development software attempts to correlate the learned key commands against those in the database, and to select the multimedia processing unit which appears to be that being taught.
In another convenient aspect, the remote control development software preferably includes, for each multimedia processing unit type, a list of command types which that type of multimedia processing unit normally will recognize. For example, all typical TVs recognize commands for power control, volume control, and number keys, and all typical VCRs recognize commands for play, stop, pause, rewind and fast forward. When learning keys of the programmed remote control 200 A, the remote control development software preferably asks the user to teach commands of expect command types first, and then, if no match in the database has been found, then non-standard commands.
After the user clicks on the Next button 425 , a dialog 520 as shown in FIG. 5 is displayed. From this screen, the remote control development software learns a number of expected command types of the multimedia processing unit. Accordingly, the remote control development software displays a prompt 525 in the dialog 520 for the user to aim the programmed remote control unit 200 A that came with the multimedia processing unit 300 at the communications transceiver 135 of the docking station 130 , and to press the expected keys on the programmed remote control unit 200 A. After the remote control development software recognizes each key press and records the command from the programmed remote control unit 200 A (step 1250 ), the remote control development software displays a next expected key, until all of the expected keys have been learned (step 1255 ). Preferably, after the remote control development software learns each new expected command, it test the learned commands against those of the screen objects in the database. If a match is found, then the user is given the opportunity to accept the match found by the remote control development software or to continue teaching.
After the user clicks on the Next button 425 , a dialog 620 as shown in FIG. 6 is displayed. In this step 1260 , the remote control development software learns a non-standard commands of the multimedia processing unit 300 . Accordingly, the remote control development software displays a prompt 625 in the dialog 620 for the user to enter the name of the non-standard key in an entry field 626 and to aim the programmed remote control unit 200 A at the transceiver 135 of the docking station 130 , and to press the named key on the programmed remote control unit 200 A. After the remote control development software recognizes each key press and records the command from the programmed remote control unit 200 A, the remote control development software displays the same dialog 620 until all of the non-standard keys have been learned (step 1265 ).
If the remote control development software has identified the user's multimedia processing unit and selected the corresponding preconfigured screen object, the remote control development software preferably shows a representation of the screen object as exemplified by the screen shot of FIG. 7 . FIG. 7 shows the menu bar 310 mentioned above, plus a left pane 710 and a right pane 720 .
The right pane 720 shows a representation 726 of the programmable remote control unit 200 , with a representation 721 of the appearance of the screen object in the programmable remote control unit's display 221 , the programmable keys 723 and the fixed keys 724 . The representation 721 includes the multimedia processing unit's name 766 as entered by the user in step 1240 . The representation 721 also includes soft keys 722 corresponding to the keys 201 A- 275 A of the multimedia processing unit's programmed remote 200 A (FIG. 2 A). The representation 721 preferably precisely mimics the key sizes and locations of the multimedia processing unit's programmed remote control unit 200 A.
The left pane 710 is a display of screen object information. The left pane 710 shows the screen object's name 711 , plus a list 712 of tagnames of the commands in the screen object. Those of skill in the art will appreciate the correspondence between the tagnames 712 of commands, the soft keys 722 and commands. For preconfigured screen objects, programmable key objects for controlling speaker volume and channel rotation are preferably also mapped to the programmable keys 723 / 223 as discussed above. Soft key objects may include these mappings.
The left pane 710 preferably is for displaying information about all available screen objects. This display is preferably hierarchical, and a user may toggle the display of the component objects of a screen object by clicking on a ‘+’ (to display) or ‘−’ (to hide) to the tagnames 712 . A scroll bar 715 allows the user to scroll through the list of screen objects and their respective components (if displayed).
The right pane 720 preferably is for displaying all available screen object representations. A scroll bar 725 allows the user to scroll through the screen object representations.
In the case where the user is teaching the remote control development software the commands of a multimedia processing unit for which the remote control development software lacks a preconfigured screen object, the user will need to create the screen object's layout manually. This is performed in the Development Phase. The user may also modify edit screen objects and even create new screen objects by copying layout information, soft key objects and programmable key objects from existing screen objects.
Development Phase
In the development phase, a user may add, edit, delete or reorder screen objects. Each of these functions preferably may be activated by the user from a Tools menu 920 as shown in FIG. 9 . There are preferably also short-cut keys or tool bar buttons for accessing this feature in the manner known in the art.
As shown in FIG. 9, the remote control development software is displaying in the left pane 710 not only the screen object information of the TV multimedia processing unit described above, but also screen object information of a cable box multimedia processing unit. Although not shown in FIG. 9, a representation of the cable box's screen object is also available in the right pane 720 and can be displayed using the scroll bar 725 .
If a new screen object is to be created, the user selects an Add Screen command 941 from the Tools menu 940 . As shown in FIG. 10, the remote control development software then creates a new screen object with the title Custom 1066 , and a representation 1026 of the programmable remote control unit 200 in the right pane 720 with only a title 1066 .
The remote control development software preferably provides drag and drop tools for the user to create and edit the screen object, and displays a tool box 1050 having a number of object creating and editing tools for the user to use. For example, the user could create a new soft key object by dragging a button tool 1052 to the display area 721 of the representation 726 of the programmable remote control unit 200 . A mouse cursor 1260 is shown in FIG. 12 dragging a graphic of a button 1265 for the soft key object. The remote control development software preferably provides other object-oriented editing controls as known in the art. These controls permit the user to modify the shape and location of soft keys, edit the commands associated with soft keys and programmable keys, change text labels, and otherwise edit the appearance of the screen object.
The soft key objects and programmable key objects preferably may include more than one command. Tagnames may be dragged from the left pane 710 and dropped onto representations of the desired object in the right pane 720 . Preferably, if the user moves the mouse cursor 1060 over the representation of an object in the right pane 720 , the remote control development software displays the commands associated with that representation. By double-clicking on the representation of the object, an edit window is preferably displayed so that the order of tagnames may be rearranged and sequence controls, such as if-else and for-next structures, may be inserted. Preferably, a user may assign commands to a screen object directly, so that when the screen object is selected from the programmable remote control unit 200 , the commands assigned to the screen object directly are automatically issued by the programmable remote control unit 200 .
Referring now to FIG. 11, there is shown a screen shot wherein of an exemplary custom screen object. This screen object is entitled “Dad” 1166 and was created for the father of a household. The title 1166 is shown both in the left pane 710 and in the right pane 720 as 1111 . The Dad screen object has two soft key objects and corresponding soft keys 1161 , 1162 . The Dad screen object also has four programmable key objects in the manner previously described whose tagnames 1114 are shown in the left pane 710 . Below the title 1166 , there are no tagnames. This is because all of the commands of the Dad screen object are drawn from other screen objects.
This screen object demonstrates one of the significant benefits of the system and method of the invention. The soft key object 1161 has been programmed with a series of commands for turning on the TV and cable box, then tuning the TV to receive from the cable box, then tuning the cable box to Dad's favorite cable channel, ESPN. The soft key object 1162 has been programmed with a series of commands for turning on the stereo receiver, then tuning the stereo receiver to Dad's favorite radio station, KTWV.
Transfer Phase
After the user is satisfied with his screen objects, he then downloads them from the general purpose computer 100 to the programmable remote control unit 200 . The first step in this process is for the user to insert the programmable remote control unit 200 into the docking station 130 , as shown in FIG. 8 . Once docked, software in the programmable remote control unit 200 and general purpose computer 100 logically connect the devices and test the connection.
Next, the user uses the general purpose computer 100 to select the screen objects stored in the database to be downloaded, and the user activates a download command from the general purpose computer 100 . As shown by example in FIG. 7, the user selects a Download command 741 from a Connect menu 740 on the menu bar 310 . The Connect menu 740 preferably also includes commands for testing the connection between the general purpose computer 100 and the programmable remote control unit 200 , and for checking on the status of the connection. There are preferably also short-cut keys or tool bar buttons for accessing these features in the manner known in the art. Screen objects preferably may be downloaded individually or in groups.
Once the programmable remote control unit 200 is loaded with screen objects, the programmable remote control unit 200 may be removed from the docking station 130 and is ready for use to control the multimedia processing unit 300 .
It should be appreciated that the general purpose computer 100 may be used to create and edit screen objects apart from any remote control units and without having the programmable remote control unit 200 in the docking station 130 .
Use Phase
Once loaded with screen objects, the programmable remote control unit 200 is ready for use. When powered on, the programmable remote control 200 unit preferably automatically loads one of the stored screen objects. The user may scroll through loaded screen objects using the fixed keys 224 b, 224 c. The programmable remote control unit 200 generates displays of soft keys and other features of the screen object on the display 221 , and generates the commands of the soft key objects and programmable key objects when the corresponding soft keys or programmable keys are pressed.
Although exemplary embodiments of the present invention have been shown and described, it will be apparent to those having ordinary skill in the art that a number of changes, modifications, or alterations to the invention as described herein may be made, none of which depart from the spirit of the present invention. All such changes, modifications and alterations should therefore be seen as within the scope of the present invention.
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A portable hand-held remote control unit device is disclosed which may be utilized for selecting designated functions in a plurality of remotely controllable multimedia processing units. Multiple user selectable screen objects may be created from a general purpose computer and transferred to the remote control unit. The screen objects include screen layout and descriptions of soft keys to be displayed on a graphic display of the remote control unit, as well as commands associated with the screen object, the soft keys and programmable keys on the remote control unit. The user may select any of the loaded screen objects for controlling various multimedia processing units, for performing complex functions of commands to various multimedia processing units.
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BACKGROUND OF THE INVENTION
[0001] This invention relates to a method of making a CBN compact.
[0002] Boron nitride exists typically in three crystalline forms, namely cubic boron nitride (CBN), hexagonal boron nitride (hBN) and wurtzitic cubic boron nitride (wBN). Cubic boron nitride is a hard zinc blend form of boron nitride that has a similar structure to that of diamond. In the CBN structure, the bonds that form between the atoms are strong, mainly covalent tetrahedral bonds. Methods for preparing CBN are well known in the art. One such method is subjecting hBN to very high pressures and temperatures, in the presence of a specific catalytic additive material, which may include the alkali metals, alkaline earth metals, lead, tin and nitrides of these metals. When the temperature and pressure are decreased, CBN may be recovered.
[0003] CBN has wide commercial application in machining tools and the like. It may be used as an abrasive particle in grinding wheels, cutting tools and the like or bonded to a tool body to form a tool insert using conventional electroplating techniques.
[0004] CBN may also be used in bonded form as a CBN compact, also known as PCBN. CBN compacts tend to have good abrasive wear, are thermally stable, have a high thermal conductivity, good impact resistance and have a low coefficient of friction when in contact with a ferrous workpiece.
[0005] Diamond is the only known material that is harder than CBN. However, as diamond tends to react with certain materials such as iron, it cannot be used when working with iron containing metals and therefore use of CBN in these instances is preferable.
[0006] CBN compacts comprise sintered polycrystalline masses of CBN particles. When the CBN content exceeds 80 percent by volume of the compact, there is a considerable amount of direct CBN-to-CBN contact and bonding. When the CBN content is lower, e.g. in the region of 40 to 60 percent by volume of the compact, then the extent of direct CBN-to-CBN contact and bonding is less.
[0007] CBN compacts will generally also contain a binder or second phase which may be a CBN catalyst or may contain such a catalyst. Examples of suitable binder/second phases are aluminium, alkali metals, cobalt, nickel, and tungsten.
[0008] When the CBN content of the compact is less than 75 percent by volume there is generally present another hard phase, a third phase, which may be ceramic in nature. Examples of suitable ceramic hard phases are nitrides, borides and carbonitrides of a Group IVA or VB transition metal, aluminium oxide, and carbides such as tungsten carbide and mixtures thereof.
[0009] CBN compacts may be bonded directly to a tool body in the formation of a tool insert or tool. However, for many applications it is preferable that the compact is bonded to a substrate, forming a supported compact structure, and then the supported compact structure is bonded to a tool body. The substrate is typically a cemented metal carbide that is bonded together with a binder such as cobalt, nickel, iron or a mixture or alloy thereof. The metal carbide particles may comprise tungsten, titanium or tantalum carbide particles or a mixture thereof. The substrate, when provided, will generally have a size and thickness considerably greater than that of the CBN compact.
[0010] A known method for manufacturing the polycrystalline CBN compacts and supported compact structures involves subjecting an unsintered mass of CBN particles to high temperature and high pressure conditions, i.e. conditions at which the CBN is crystallographically stable, for a suitable time period. A binder phase may be used to enhance the bonding of the particles. Typical conditions of high pressure and temperature (HPHT) which are used are pressures of the order of 2 GPa or higher and temperatures in the region of 1100° C. or higher. The time period for maintaining these conditions is typically about 3 to 120 minutes.
[0011] The sintered CBN compact, with or without substrate, is often cut into the desired size and/or shape of the particular cutting or drilling tool to be used and then mounted onto a tool body utilising brazing techniques.
SUMMARY OF THE INVENTION
[0012] According to the present invention, there is provided a method of making a CBN compact having a layer of a refractory material bonded to a surface thereof including the steps of producing a reaction mass by placing a mass of CBN particles in contact with a material capable of forming the layer of refractory material, and subjecting the reaction mass to elevated temperature and pressure conditions suitable to form a CBN compact.
[0013] Thus, the invention provides an in-situ method of producing a CBN compact having a layer of refractory material bonded to a surface thereof. There is no need for a post-sintering operation to apply the layer of refractory material to the CBN compact. Such post-sintering operation adds to the cost and can cause degradation or damage to the CBN compact. Adequate bonding of the refractory material to the CBN compact can also be difficult to achieve in a post-sintering operation.
[0014] The nature of the refractory material for the layer will vary according to the application to which the CBN compact is to be put. For example, if the layer is intended to reduce the crater damage to a working surface of the CBN compact in a cutting operation, then the refractory will be chosen to have a higher crater resistance than the CBN compact.
[0015] The refractory material will typically be a carbide, nitride, carbonitride, oxide, boride, or silicide, preferably of a Group 4, 5 or 6 metal or aluminium or silicon. The refractory material may be as a mixture or solid solution of such refractory materials.
[0016] The refractory material will typically have a binder present, generally in an amount of less than 20 volume percent of the refractory material. Examples of suitable binders are transition metals such as cobalt, iron, nickel, yttrium and titanium, and copper, aluminium and silicon and compounds and alloys containing such a metal.
[0017] In one form of the invention, the refractory-forming material in the reaction mass takes the form of a layer in contact with the mass of CBN particles. The layer preferably has a coherent green state form.
[0018] The layer of refractory-forming material in the reaction mass may be formed of two or more different layers with different compositions.
[0019] In another form of the invention the reaction mass is produced by placing the mass of CBN particles in a container of a refractory-forming material. The container may be made of a metal selected from titanium, niobium, tungsten, molybdenum, aluminium, hafnium, iron, cobalt, nickel, chromium, vanadium, zirconium and tantalum or alloy containing such a metal. During the application of the elevated temperature and pressure, the material of the container reacts with the CBN particles forming nitrides and/or borides and thus forms a layer of this refractory material bonded to a surface of the CBN compact. In the case where a metal alloy is employed as the canister material, then one of the alloying elements can be selected to facilitate the formation of an appropriate binder phase for the refractory material. Examples of suitable elements for this are nickel and cobalt. The element may persist in the metallic form within the final sintered product. The thickness of such layers is typically about 20 to 50 microns, the depth to which boron and nitrogen from the CBN particles diffuses into the container material. Some residual metal from the container may remain in the layer of refractory material and act as a binder phase.
[0020] The layer of refractory material bonded to a surface of the CBN compact will generally be thin and preferably no greater than 300 microns in thickness. Generally, the thickness of the layer will be at least 30 microns. For such layers, the thickness of the layer of refractory-forming material in the reaction mass will be chosen such as to produce a refractory layer of the desired thickness.
[0021] A layer of a metal such as copper, silver, zinc, cobalt and nickel may be provided between the refractory material and the mass of CBN particles in the reaction mass. The purpose of such a metal may, for example, be to improve the bonding between the layer of refractory material and the CBN compact.
[0022] Typical conditions of elevated (high) pressure and temperature (HPHT) which are used to produce a CBN compact are temperatures in the region of 1100° C. or higher and pressures of the order of 2 GPa or higher. The time period for maintaining these conditions is typically about 3 to 120 minutes.
[0023] The CBN compact may be a high content CBN compact, i.e. one having a CBN content of at least 70 percent by volume, and will generally contain a second phase. The CBN compact may also be a low CBN content compact which will contain a second phase and generally also a third phase. Both such CBN compacts are well known in the art.
[0024] Second and third phase materials, when provided, will generally be in particulate form and then mixed with the mass of CBN particles prior to the application of the elevated temperature and pressure conditions.
[0025] The mass of CBN particles, with or without particulate second and third phases, will preferably be formed into a coherent green state compact which is then subjected to the elevated temperature and pressure conditions.
[0026] The CBN compact may be bonded to a substrate such as a cemented carbide substrate. For such compacts, the cemented carbide substrate will be massive relative to the CBN compact and the layer of refractory material will generally be bonded to a surface of the compact opposite to that bonded to the substrate.
[0027] The CBN compact typically has a thickness range from about 300 μm to 2000 μm, preferably from about 500 μm to 1000 μm.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0028] The invention will now be illustrated by the following non-limiting examples.
Example 1
[0029] A sub-stochiometric titanium carbonitride powder, Ti(C 0.7 NO 0.3 ) 0.8 of average particle size of 1.4 micron was mixed with Al powder, average particle size of 5 micron, using a tubular mixer. The mass ratio between Ti(C 0.7 N 0.3 ) 0.8 and Al was 90:10. The powder mixture was pressed into a titanium cup to form a green compact and heated to 1025° C. under vacuum for 30 minutes and then crushed and pulverized. The powder mixture was then attrition milled for 4 hours and then 1.4 micron average particle size of CBN was added and attrition milled in hexane for an hour. The CBN was added in an amount such that the total volume percentage of calculated CBN in the mixture was about 60 percent. The slurry was dried under vacuum and formed into a green compact, which was supported by a tungsten carbide hard metal.
[0030] The green compact and support of tungsten carbide were placed in a titanium canister and sintered at 55 kbar (5.5 GPa) and at a temperature around 1300° C. The canister was recovered and unreacted titanium was removed by grinding. A thin layer of a refractory material containing titanium diboride and titanium nitride was left on at least one surface of the CBN compact. This layer of refractory was formed by interaction of the titanium with boron and nitrogen diffusing into the titanium cup from the CBN particles. The depth of the diffusion is typically 20 to 50 microns. Some residual titanium may be present in the refractory layer, acting as a binder.
Example 2
[0031] A sub-stochiometric titanium carbonitride powder, Ti(C 0.7 N 0.3 ) 0.8 of average particle size of 1.4 micron was mixed with Al powder, average particle size of 5 micron, using a tubular mixer. The mass ratio between Ti(C 0.7 N 0.3 ) 0.8 and Al was 90:10. The powder mixture was pressed into a titanium cup to form a green compact and heated to 1025° C. under vacuum for 30 minutes and then crushed and pulverized. The powder mixture was then attrition milled for 4 hours and then 1.4 micron average particle size of CBN was added and attrition milled in hexane for an hour. The CBN was added in an amount such that the total volume percentage of calculated CBN in the mixture was about 60 percent. The slurry was dried under vacuum and formed into a green compact.
[0032] A powder mixture containing about 89 vol % TiC 0.8 , and equal volume percentage of Al and Ni, was milled and mixed in an attritor mill and dried. A binder, PMMA (poly methyl methacylate), a plastisizer, DBP (dibutyl phthalate) of equal volume percentages were added into a container together with 50 vol % of total volume of the solvent material, containing 70 vol % methyl ethyl ketone and 30 vol % ethanol. The mixture was stirred at high speeds and then a powder mixture, containing TiC 0.8 , Al and Ni, was added gradually into the liquid mixture to achieve a consistent viscosity that is suitable for tape casting. The mixed slurry was poured into a Dr. Blade set up and a thin layer (about 100 micron in thickness) of ceramic tape was cast and dried. After drying, layers of ceramic (refractory) tape were placed on top of the already formed green compact. After encapsulation, the unit was sintered at 55 kbar (5.5 GPa) and at a temperature around 1300° C.
[0033] Recovered after sintering was a CBN compact having a layer of a refractory material containing titanium carbide, titanium diboride, aluminium nitride and nickel alloy, bonded to a surface thereof.
Example 3
[0034] A sub-stochiometric titanium carbonitride powder, Ti(C 0.7 N 0.3 ) 0.8 of average particle size of 1.4 micron was mixed with Al powder, average particle size of 5 micron, using a tubular mixer. The mass ratio between Ti(C 0.7 N 0.3 ) 0.8 and Al was 90:10. The powder mixture was pressed into a titanium cup to form a green compact and heated to 1025° C. under vacuum for 30 minutes and then crushed and pulverized. The powder mixture was then attrition milled for 4 hours and then 1.4 micron average particle size of CBN was added and attrition milled in hexane for an hour. The CBN was added in an amount such that the total volume percentage of calculated CBN in the mixture was about 60 percent. The slurry was dried under vacuum and formed into a green compact.
[0035] A powder mixture containing about 63.5 vol % TiC 0.8 , 30 vol % CBN, 2.6 vol % Al and 3.9 vol % of Ni was milled and mixed in an attritor mill and dried. A binder, PMMA (poly methyl methacylate), a plastisizer, DBP (dibutyl phthalate) of equal volume percentages were added into a container together with 50 vol % of total volume of the solvent material, containing 70 vol % methyl ethyl ketone and 30 vol % ethanol. The mixture was stirred at high speeds and then the powder mixture, containing TiC 0.8 , CBN, Al and Ni, was added gradually into the liquid mixture to achieve a consistent viscosity that is suitable for tape casting. The mixed slurry was poured into a Dr. Blade set up and a thin layer (about 100 micron in thickness) of ceramic tape was cast and dried. After drying, layers of ceramic tape were placed on top of the already formed green compact. After encapsulation, the unit was sintered at 55 kbar (5.5 GPa) and at a temperature around 1300° C.
[0036] Recovered was a CBN compact having a layer of a refractory containing titanium carbide, CBN, titanium diboride, aluminium nitride and nickel alloy bonded to a surface thereof.
Example 4
[0037] A sub-stochiometric titanium carbonitride powder, Ti(C 0.7 N 0.3 ) 0.8 of average particle size of 1.4 micron was mixed with Al powder, average particle size of 5 micron, using a tubular mixer. The mass ratio between Ti(C 0.7 N 0.3 ) 0.8 and Al was 90:10. The powder mixture was pressed into a titanium cup to form a green compact and heated to 1025° C. under vacuum for 30 minutes and then crushed and pulverized. The powder mixture was then attrition milled for 4 hours and then 1.4 micron average particle size of CBN was added and attrition milled in hexane for an hour. The CBN was added in an amount such that the total volume percentage of calculated CBN in the mixture was about 60 percent. The slurry was dried under vacuum and formed into a green compact.
[0038] A powder mixture containing about 46.9 vol % TiN 0.8 , 46 vol % CBN, 3.1 vol % Ni and 4 vol % Al was milled and mixed in an attritor mill and dried. A binder, PMMA (poly methyl methacylate), a plastisizer, DBP (dibutyl phthalate) of equal volume percentages were added into a container together with 50 vol % of total volume of the solvent material, containing 70 vol % methyl ethyl ketone and 30 vol % ethanol. The mixture was stirred at high speeds and then a powder mixture, containing TiN 0.8 , CBN, Al and Ni, was added gradually into the liquid mixture to achieve a consistent viscosity that is suitable for tape casting. The mixed slurry was poured into a Dr. Blade set up and a thin layer (about 100 micron in thickness) of ceramic tape was cast and dried. After drying, layers of ceramic tape were placed on top of the already formed green compact. After encapsulation, the unit was sintered at 55 kbar (5.5 GPa) and at a temperature around 1300° C.
[0039] Recovered was a CBN compact having a layer of a refractory material containing titanium nitride, CBN, titanium diboride, aluminium nitride and nickel alloy bonded to a surface thereof.
Example 5
[0040] A sub-stochiometric titanium carbonitride powder, Ti(C 0.7 N 0.3 ) 0.8 of average particle size of 1.4 micron was mixed with Al powder, average particle size of 5 micron, using a tubular mixer. The mass ratio between Ti(C 0.7 N 0.3 ) 0.8 and Al was 90:10. The powder mixture was pressed into a titanium cup to form a green compact and heated to 1025° C. under vacuum for 30 minutes and then crushed and pulverized. The powder mixture was then attrition milled for 4 hours and then 1.4 micron average particle size of CBN was added and attrition milled in hexane for an hour. The CBN was added in an amount such that the total volume percentage of calculated CBN in the mixture was about 60 percent. The slurry was dried under vacuum and formed into a green compact.
[0041] A powder mixture containing about 90.7 vol % Ti(C 0.5 N 0.5 ) 0.8 , 4.6 vol % Ni and 4.7 vol % Al was milled and mixed in an attritor mill and dried. A binder, PMMA (poly methyl methacylate), a plastisizer, DBP (dibutyl phthalate) of equal volume percentages were added into a container together with 50 vol % of total volume of the solvent material, containing 70 vol % methyl ethyl ketone and 30 vol % ethanol. The mixture was stirred at high speeds and then a powder mixture, containing Ti(C 0.5 N 0.5 ) 0.8 , Ni and Al was added gradually into the liquid mixture to achieve a consistent viscosity that is suitable for tape casting. The mixed slurry was poured into a Dr. Blade set up and a thin layer (about 100 micron in thickness) of ceramic tape was cast and dried. After drying, layers of ceramic tape were placed on top of the already formed green compact. After encapsulation, the unit was sintered at 55 kbar (5.5 GPa) and at a temperature around 1300° C.
[0042] Recovered was a CBN compact having a layer of a refractory material containing titanium carbonitride, titanium diboride, nickel alloy and aluminium nitride bonded to a surface thereof.
Example 6
[0043] A sub-stochiometric titanium carbonitride powder, Ti(C 0.7 N 0.3 ) 0.8 of average particle size of 1.4 micron was mixed with Al powder, average particle size of 5 micron, using a tubular mixer. The mass ratio between Ti(C 0.7 N 0.3 ) 0.8 and Al was 90:10. The powder mixture was pressed into a titanium cup to form a green compact and heated to 1025° C. under vacuum for 30 minutes and then crushed and pulverized. The powder mixture was then attrition milled for 4 hours and then 1.4 micron average particle size of CBN was added and attrition milled in hexane for an hour. The CBN was added in an amount such that the total volume percentage of calculated CBN in the mixture was about 60 percent. The slurry was dried under vacuum and formed into a green compact.
[0044] A powder mixture containing about 31.5 vol % TiN 0.8 , 61.7 vol % ZrO 2 , 1.4 vol % Al 2 O 3 and 5.5 vol % Y 2 O 3 was milled and mixed in an attritor mill and dried. A binder, PMMA (poly methyl methacylate), a plastisizer, DBP (dibutyl phthalate) of equal volume percentages were added into a container together with 50 vol % of total volume of the solvent material, containing 70 vol % methyl ethyl ketone and 30 vol % ethanol. The mixture was stirred at high speeds and then a powder mixture, containing TiN 0.8 , ZrO 2 , Al 2 O 3 and Y 2 O 3 , was added gradually into the liquid mixture to achieve a consistent viscosity that is suitable for tape casting. The mixed slurry was poured into a Dr. Blade set up and a thin layer (about 100 micron in thickness) of ceramic tape was cast and dried. After drying, layers of ceramic tape were placed on top of the already formed green compact. After encapsulation, the unit was sintered at 55 kbar (5.5 GPa) and at a temperature around 1300° C.
[0045] Recovered was a CBN compact having a layer of a refractory material containing titanium nitride, zirconium oxide, aluminium oxide and yttrium oxide bonded to a surface thereof.
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A layer of a refractory material produced and bonded in situ to a surface of a CBN compact during the high temperature/high pressure manufacture of the CBN compact.
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TECHNICAL FIELD
[0001] The invention relates to a multilevel optical signal system and in particular a multilevel optical signal system suitable for converting electrical signal to optical signal.
BACKGROUND ART
[0002] The need for fast transmission of signals in optical fibers is general increasing. Whereas today's optical interconnects are based on optical NRZ (non return to zero) modulation formats with two optical power levels, future interconnects might be based on other modulation schemes, multi-level optical links being one proposal, and several methods of converting electrical signals to multilevel signals have been suggested.
[0003] U.S. Pat. No. 8,380,085 (NEC LABORATORIES AMERICA INC) describes a method of processing data that includes receiving a plurality of binary electronic signals and generating an optical signal by a number of lasers that is equal to or greater than the number of binary electronic signals. The optical signal is generated at one of a plurality of intensity levels, and each intensity level represents a particular combination of bit values for the plurality of binary electronic signals. The optical signal is converted into an electronic signal having the plurality of intensity levels. An apparatus for processing data is provided that includes a plurality of lasers configured to emit light at a plurality of frequencies, and a plurality of modulators configured to receive a plurality of binary electronic signals and to modulate the light
DESCRIPTION OF THE INVENTION
[0004] Whereas the method disclosed in U.S. Pat. No. 8,380,085 may increase the transmission rate in optical fiber, there is still a need for an effective multilevel optical signal where the resulting optical signal can be decoded with a relatively low bit error rate.
[0005] In an embodiment of the invention it is an object to provide a fast multilevel optical signal system suitable for converting electrical signal to optical signal and where the multilevel optical signal can be converted to electrical signals with a low bit error rate.
[0006] These and other objects have been solved by the invention or embodiments thereof as defined in the claims and as described herein below.
[0007] It has been found that the invention or embodiments thereof have a number of additional advantages which will be clear to the skilled person from the following description.
[0008] The term “substantially” should herein be taken to mean that ordinary product variances and tolerances are comprised.
[0009] All features of the inventions and embodiments of the invention as described above including ranges and preferred ranges can be combined in various ways within the scope of the invention, unless there are specific reasons not to combine such features.
[0010] The inventors of the present invention has found that by providing the multilevel optical signal system such that the data signals are in phase and are synchronized in frequency to have fully timely overlying bit rate a very effective multilevel optical signal system is provided which can be reconverted to electrical signals in a relatively simple and effective way.
[0011] In an embodiment of the invention modulated light from a number of branches are combined in a passive, optical power-combiner into one optical signal. Each branch comprises a CW (continuous wave) light source, L j , an optical modulator and an electrical driver for the modulator. Each electrical driver takes the two-level data signal, D j , and all data signals are synchronous in phase and frequency with a bit rate of B. The combined output will have the same baud-rate as the data signals bit rate, B, now carrying all N signals, with 2 n different symbols and a total bit-rate of N*B.
[0012] In an embodiment the optical power level out of each branch is adjusted to different levels, or weights. A preferred design is binary stepped weights so that the output of branch n+1 is the double of branch n. For N=2 the suggested 4-level signal generated by branch 1 having a power of P 0 and branch 2 a power of 2P 0 .
[0013] In an embodiment the branches of the multilevel optical signal system are configured to generate the respective 2-level data signals such that the power from a laser source of a first branch is P0 and the power of from a laser source of an N'th branch is 2̂N times P0.
[0014] In the general case, the transmitted power is P out =ΣD j *P j =ΣD j *W j *P 0 ; j=1 . . . N.
[0015] In the binary weighted 4-level transmitter P out =P 0 ΣD j *2 j-1 =P 0 {D 1 2D 2 }, i.e., the levels are 0, P 0 , 2P 0 , 3P 0 . Or by different scaling, 0, ½P 0 , P 0 , 1½P 0 .
[0016] The light sources L 1 . . . L N in each branch will advantageously generate light having different wavelengths and may also be designed with deliberately different wavelengths. In an embodiment the integrating photo receiver on the receive side will not distinguish the wavelengths, only integrate the power of light. Applying different wavelengths may add to distinguish the signals e.g. for splitting the signals e.g. by optical filters at the receiver.
[0017] In an embodiment the light sources must not correlate in optical phase as interference may occur in the combiner and constructive or destructive interference is undesirable. The combiner advantageously add optical power and it is therefore desired that the coherence length between the sources to be relatively short. There is no reason to believe that separate lasers would not be uncorrelated and have very short and insignificant coherence length.
[0018] In an embodiment it is desired that the lasers are not narrow band, but relatively broad, so stochastically destructive interference will become a relatively small part of the combined power. In other words, the phases of the optical carriers must preferably be misaligned.
[0019] A “dithering” signal may be applied to the forward current to the lasers so that the phase changes over time and/or to some extend decreases the phase alignment between lasers. The frequencies of the dithering signals may be prime factors to avoid common frequencies.
[0020] In an embodiment Fabry-Perot lasers are used and in another narrow line width lasers are used. In both cases, difference in wavelength and the above described dithering signal may be applied. Other continuous wave light sources could also be applied.
[0021] Requirements on the linearity of the electrical drivers are avoided as each drivers will have only two levels. All drivers can be equal and operate equally. Also the light modulators need no strict linearity. This can be achieved with today's technology.
[0022] The weight of the light of each branch (same as the optical power level of each branch) can be maintained by monitoring the CW output of the laser before the modulator, or even after the modulator if a fixed modulation index is maintained, e.g., 50% modulation over a period of time.
[0023] On the receive side, a multi-level-capable receiver is needed to detect and decode the optical signal. The suggested transmitter does not impose special requirements to the receiver over other multi-level-capable receivers.
[0024] Compared to a 2-level transmitter that can provide optical power up to P 0 , a 4-level binary weighted transmitter of an embodiment of the invention requires 3 dB of the optical link budget, because the power levels of the two branches would have to be ½P 0 and P 0 with available technology. The loss in the optical power combiner is considered negligible. Other multi-level transmitters may impair the link budget even further by imposing complicated linearity requirements to the drivers and optical modulators which this proposal avoids. It means at an unchanged baud-rate, the link bit-rate can be doubled at a cost of 3 dB optical penalty. There may be other inevitable penalties but the solution provided by the present invention is close to ideal.
[0025] FIG. 1 shows a preferred embodiment of the multilevel optical signal system comprising an optical power combiner and a number of branches here represented by branches J and N, where each branch comprises a light source, a modulator and a driver for the modulator.
[0026] In use the electrical signals D j and D N are transmitted to the drivers or the respective branches where they are concerted to respective 2-level optical data signals by the light sources L J ,L N and the modulators of the respective branches. The 2-level optical data signals are transmitted to the optical power combiner where they are combined to a multilevel optical signal P out .
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The invention comprises a multilevel optical signal system comprising two or more light source branches and an optical power-combiner, wherein each branch comprising a light source, an optical modulator and an electrical driver for the modulator, wherein each electrical driver is configured for being driven by electrical signals to drive the modulator to modulate the light generated by the light source into a corresponding 2-level data signalsuch that the respective 2-level data signals differs in power level.
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BACKGROUND OF THE INVENTION
The present invention relates generally to dental orthopedic correction and, more particularly, to an adjustable, functional and removable orthopedic appliance for correcting dental Class II malocclusions.
DESCRIPTION OF THE RELATED ART
A Class II malocclusion is defined as the malposition of the maxillary and mandibular teeth so that the lower dental arch is posterior to the upper dental arch resulting in loss of efficiency during movements of the jaw that are essential for mastication. In a Class II, division 1 malocclusion, the upper incisors are protruding and the occlusion is usually evidenced by an excessive overbite of the lower incisors. In a Class II, division 2 malocclusion the upper incisors are tipped lingually and the laterals are flared labially.
Class II malocclusions may be corrected utilizing either fixed appliances or functional, removable appliances, or a combination of both. Fixed appliances such as braces, are typically worn an average of 24 to 30 months to correct a Class II malocclusion. Fixed appliances also require either extra-oral force, intramaxillary elastics, or a combination of both to effect a basal maxilla-mandibular change and to eliminate the excessive overbite, overjet or apical base discrepancy.
Removable functional appliances may often eliminate the need for extra-oral force or intramaxillary elastics required by fixed appliances. A removable and functional orthopedic appliance corrects a Class II malocclusion by causing the entire mandible, or lower jaw, to move forward, freeing the condyle in the temporal mandibular joint from any possible growth restrictions from the dominant retrusive muscular activity associated with the inherent Class II malocclusion. The forward movement of the mandible is caused by a stretch reflex initiated by introducing the orthopedic appliance into the patient's mouth, causing the muscles to pull the mandible in an anterior direction.
Present orthodontic practice utilizes a series of two or more removable functional orthopedic appliances to correct a Class II type of malocclusion. Examples of these devices are commonly known in the orthodontic profession as "Saggital," "Frankel," "Bionater," and "Ortho Redir Corrector" devices. Each successive appliance is elongated along an anterior-posterior medial line relative to the previously used appliance and as the treatment progresses and the mandible more closely aligns with the maxilla, the second or third appliances of the series is used by the patient. With each successive appliance the mandible is repositioned more closely to a correctly aligned state relative to the maxilla while concurrently restricting maxillary forward growth.
Adjustable, functional and removable devices have also been proposed which eliminate the need for using two or more of the above-described orthopedic appliances. For example, U.S. Pat. No. 4,433,956 discloses an adjustable, functional and removable orthopedic corrector having an anterior segment and a posterior segment interconnected by two expansion screw assemblies. As treatment of the Class II malocclusion progresses, each of the two expansion screw assemblies are turned, separating the anterior and posterior segments of the corrector with resultant forward movement of the mandible It is necessary, however, to carefully adjust each expansion screw assembly equally to result in the proper correction of the malocclusion.
U.S. Pat. Nos. 4,348,179; 3,977,082 and 4,468,196 disclose various other adjustable orthodontic appliances fitting into the palatal cavity of the mouth for treatment of various orthodontic dysfunctions. However, none of these patents proposes a device for the treatment and correction of Class II malocclusions.
There is a need for a single orthopedic appliance for correcting Class II malocclusions which eliminates the need for sequentially employing two or more devices. The appliance should be easy to fabricate, comfortable for the user to wear, easily adjustable and effective in the correction of the Class II malocclusions in as short as time possible. The present invention addresses these problems by providing a single, removable, functional, active appliance for use in the full course of treatment and correction of Class II malocclusions. In addition, the appliance of the present invention is relatively comfortable to wear, thereby eliciting a high degree of patient compliance. These and other advantages of the present invention will be apparent from the drawings, discussion, description and claims which follow.
SUMMARY OF THE INVENTION
The present invention provides an orthopedic appliance for correcting Class II malocclusions comprising a frontal portion configured to engage the mandibular and maxillary frontal arches of the mouth. The frontal portion includes a cavity corresponding to at least a portion of the inner and outer surfaces of the mandibular incisors and which engages the rear surface of the maxillary incisors. Engagement of the mandibular incisors into the cavity over an extended period of time corrects the Class II malocclusion. The frontal portion further includes a pair of ball clasps which engage the front surfaces of the maxillary incisors.
The appliance further includes first and second side portions, each configured to engage at least some of the maxillary molars. Each side member includes a retaining clasp for engaging the maxillary molars and securing the device into the palatal cavity of the mouth. The side portions may also include other orthodontic attachments such as distalizing springs and the like to perform other orthodontic corrections.
The orthopedic appliance of the present invention further includes adjustment means interconnecting the frontal portion to the first and second side portions. The adjustment means includes a first expansion screw interconnecting the side members and operative to adjust the lateral spacing therebetween and a second expansion screw associated with the frontal member to adjust the anteriorposterior spacing between the frontal portion and the two side portions. In this manner, the present invention provides a single appliance for correcting Class II malocclusions which is easily adjustable in two directions.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of an orthopedic appliance of the present invention;
FIG. 2 is a bottom plan view of the orthopedic appliance of FIG. 1 seated in the palatal cavity of a user; and
FIG. 3 is a perspective view of the orthopedic appliance of the present invention fitted into a plaster model of a mouth with closed jaws.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings, as is shown in FIG. 1, an orthopedic appliance 10 comprises a frontal portion 12, a first side portion 14 and a second side portion 16, molded to conform to the interior of the patient's mouth. Orthopedic appliance 10 is removably secured in the palatal cavity of a patient's mouth by retentive springs and clasps as will be explained below. The frontal portion 12 is configured to engage at least a portion of the mandibular and maxillary frontal arches when the mouth is closed, while the first and second side portions 14, 16 engage the interior sides of at least some of the maxillary molars.
Frontal portion 12, first side portion 14 and second side portion 16 are fabricated from a synthetic polymeric material, preferably a tissue compatible acrylic, using established techniques known in the dental art. In one such technique, a plaster cast from an alginate mold is made of the patient's mouth and dentition in the construction bite position. The construction bite is defined as the amount of forward movement of the mandible and opening of the mandible which the patient self-induces at the doctor's direction prior to treatment. Orthopedic appliance 10 is molded using the shape taken from the plaster cast. Retaining clasps 18, ball clasps 24 and various other orthopedic attachments, such as distalizing springs 22, are placed in the mold at the desired locations and are embedded into place in the acrylic during the molding process.
FIGS. 2 and 3 show the orthopedic appliance 10 in place in a plaster model of in the mouth of a 7-year old patient. This patient has not completely lost all of her deciduous or "baby" teeth as will be noted by those skilled in the art. This model is shown as an example only and in no way is meant as a limitation upon the present invention. Although the appliance 10 may be used to correct Class II malocclusions at any stage during a patient's life, the appliance 10 is most favorably used while the patient is actively growing, i.e., at or before puberty.
As is particularly illustrated in FIG. 3, the ball clasps 24 are embedded in the frontal portion 12 and act to engage the front surface of the maxillary arch between the central 21 and lateral 23 maxillary incisors. The top of the frontal portion 12 further includes indentations 28 (best seen in FIG. 1) for engaging the rear surfaces of the maxillary incisors 21,23. The bottom of frontal portion 12 includes a cavity 30, as shown in phantom in FIG. 1 and shown more clearly in FIGS. 2 and 3, for receiving at least a portion of the inner and outer surfaces of the central 27 and lateral 29 mandibular incisors as well as the mandibular cuspids 32 therein.
The first side portion 14 and the second side portion 16 are molded to conform to the roof of the patient's upper mouth. As shown more clearly in FIG. 2, the first and second side portions 14,16 respectively, include retaining clasps 18, (in this case known as Adams clasps), for engagement with molars 34,36. Retaining clasps 18 and ball clasps 24 cooperate to actively secure orthopedic appliance 10 firmly in the roof of the patient's mouth. This particular feature represents an improvement over prior art devices which utilize tongue position and intimate fit on the upper teeth to hold the appliance in position.
In the illustrated embodiment, the first side portion 14 and the second side portion 16 further include molar distalizing springs 22 which are integral in action with the lower jaw advancement bite. As shown in FIGS. 2 and 3, molar distalization springs 22 engage the first permanent (6 year) molars 38 along their exterior surfaces and between the first permanent molars and the adjacent (deciduous or permanent) second 39 molars. Distalizing springs 22 force the first permanent molars to move distally during the treatment of the Class II malocclusions. Various other orthodontic attachments and/or springs for causing buccal, labial, rotational and/or lingual movement of individual teeth may also be molded into appliance 10. Orthopedic appliance 10 further includes adjustment means such as universal screw assembly 20, for altering the spatial relationship between the front 12 and side 14,16 portions. The universal screw assembly 20 may preferably be fabricated from stainless steel, chromium-nickel alloys, non-ferrous metals, or combinations thereof. The universal screw assembly 20 includes a first expansion screw 40 which interconnects the first side portion 14 to the second side portion 16 and operates to adjust the lateral spacing therebetween. The first expansion screw 40 includes an adjuster member 44 containing a plurality of holes 46 for receiving the end of an adjustment tool, such as a small allen wrench key therein. Holes 46 are equidistantly, circumferentially spaced on adjuster member 44 and the pitch of the screw is such that a 90 degree rotation of adjuster member 44 translates into a lateral spacing increase of approximately one-quarter millimeter between the first side portion 14 and the second side portion 16. By utilizing a single adjustment mechanism or expansion screw 40 in this manner, expansion of the device can be easily and accurately adjusted without the need for adjusting two separate screw assemblies as is required in prior art devices.
Adjusting the first expansion screw 40 to cause the lateral spacing between the first and second side portions to increase and to increase maxillary arch width. This is a necessary step because, as the upper molars move distally as a result of a molar distalizing springs 22, the maxillary arch width must increase as growth occurs in order to reduce cross bite occurrence.
The universal screw assembly 20 includes a second expansion screw 42 which is similar to the first expansion screw 40 in that it also includes an adjuster member 48 having a plurality of adjustment holes 50. As described above with reference to the first expansion screw 40, holes 50 are equally spaced around adjuster member 48 so that the second expansion screw 42 can be adjusted by inserting the tool into the hole and moving it relative to a threaded shaft assembly. As before, a 90 degree rotation of adjuster 48 causes the frontal portion 12 to moVe either posteriorly or anteriorly to the first 14 and second side portions 16, a distance of about one-quarter millimeter.
As the second expansion screw 42 is turned in the direction of the arrow, the anterior and posterior segments of the appliance are separated, resulting in forward movement of the mandible. Also, an increase in distance between the frontal portion 12 and the posterior portion 14,16 causes an increase in the upper anterior tooth protrusive guidance as well as movement of the maxillary posterior teeth distally. This upper activation also causes an equal and opposite distalizing effect on the maxillary posterior teeth.
Appliance 10 differs from prior art orthopedic appliances in that it moves the upper first permanent molars substantially to the posterior because of the neurologically stimulated anchorage which produces a distalizing, posterior force component in the maxilla equal to the forward stretching, growth stimulating force of the mandibular arch and temporal mandibular joint. The appliance 10 also allows lower posterior alveolar development while holding the lower anterior teeth in position which reduces the usual deep overbite. Mandibular growth and maxillary retraction decrease the amount of original overjet. The construction of the appliance also allows vertical alveolar growth in the posterior parts of the mouth to occur faster and in greater differential to the anterior teeth which are fitted and stabilized in the appliance. This decreases the amount of original overbite.
DESCRIPTION OF OPERATION OF THE PREFERRED EMBODIMENT
After the orthopedic appliance 10 has been molded to fit the patient's mouth, it is secured against the roof of the patient's mouth by the action of Adams clasps 18 and ball clasps 24 on the teeth and the intimate fit of the appliance. Initially, the orthopedic appliance is adjusted to be retentive only with the mandible forward and the bite open. It should be noted that each patient's treatment is individualized, with some patients being required to wear the device for longer periods of time than other patients. An average treatment period lasts between 6-18 months depending on several factors, including the severity of the malocclusion, the age of the patient, the patient's response to treatment and the patient's cooperation in the counsel treatment. Even in the initially adjusted position, orthopedic appliance 10 is molded so that when the mandible is in a closed position it will be forced forward of its pre-treatment position relative to the maxillary arch.
After approximately one month, the molar distalizing springs 22 and expansion screws 40, 42 are activated. Typically, at one month intervals, the patient removes the orthopedic appliance 10, and using a small tool such as the allen wrench or key as described above, turns each expansion screw 40,42 within assembly 20 to effect a posterior-anterior expansion of approximately 1/4 millimeter. Lateral expansion of appliance 10 with screw 40 is performed as needed and directed by the patient's orthodontist. Each successive month for a total of 6-18 months depending upon the patient's response to treatment, the patient turns each expansion screw 40,42 approximately 1/4 millimeter per month, resulting in an aggregate of approximately 11/2-41/2 millimeters of expansion between frontal portion 12 and first and second side portions 14,16. Occasionally, use of the appliance 10 is discontinued for a short period of time, typically 3-6 months, so that the orthodontist can evaluate growth changes in the mandible and maxilla prior to using fixed appliances. The appliance 10 may be used in conjunction with fixed appliances where the malocclusion is especially difficult to treat or where other positional irregularities exist. The gradual expansion of appliance 10 avoids patient discomfort and possible periodontal necrosis and root resorption which might result from an immediate expansion to the maximum extent allowed by expansion screw assemblies 20. When full expansion is reached, the lower jaw or mandible has moved with respect to the upper jaw to a position beyond the construction bite, through a series of successively more forward positions relative to the maxilla. The orthopedic appliance 10 must usually be worn by the patient for approximately 6-18 months to achieve the result of a Class I occlusion. During this period, the upper teeth are moving posteriorly relative to the mandible and the mandible is moving forward.
The present invention is designed to correct Class II malocclusions by changes in the muscular and structural growth of the temporal mandibular joint. For instance, during the initial three-month period after insertion of the orthopedic appliance, there is a rapid change about the mandibular condyle and muscle function. Due to the position of the frontal portion 12 of appliance 10 beyond the previously established position of the mandible, the skeletal and muscular growth changes can result in permanent movement anteriorly of the mandible relative to the maxilla. This anterior movement of the mandible even occurs with the expansion screw assemblies closed.
After the treatment period is completed and appliance 10 is no longer used, the mandible generally moves posteriorly about one millimeter which generally results in full correction of the mandibular-maxilla relationship.
The patient is instructed to wear the orthopedic appliance at all times during the treatment period except when eating, engaging in active sports and brushing the teeth. The appliance 10 is designed so that at all times of engagement the appliance is active, even when the patient moves his or her jaws, swallows or talks. The activation of the appliance 10 exerts a gentle pressure on the teeth and dental arches. This orthopedic appliance 10 is designed to fit intimately in the mouth and be capable of easy and frequent removal and replacement by the patient, much like a dental plate. This precise fit of the lower incisors forward into the appliance makes the patient to close his jaws together in the new relationship. This is a distinct advantage over the prior art.
In light of the foregoing, it should be apparent that many variations are possible within the scope of the present invention. For example, the orthopedic appliance may be configured to include various orthodontic attachments such as labial wires and individual tooth moving springs so that the orthopedic appliance of the present invention performs orthodontic corrections at the same time as the Class II malocclusion is treated. The appliance may be adapted for use in Class II, division 2 as well as Class I malocclusions. Also, the treatment period will be generally be the same for every patient although many variations are necessary for each individual patient. Accordingly, the foregoing drawings, discussion and description are merely meant to be illustrative of particular embodiments of the invention and not limitations upon the practice thereof. It is the following claims including all equivalents which define the scope of the invention.
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An orthopedic appliance for correcting Class II malocclusions comprises a frontal portion configured to engage the mandibular and maxillary frontal arches and first and second side portions, posterior to the frontal portion, each configured to engage at least some of the maxillary molars. A universal screw assembly interconnects the frontal portions and the first and second side portions and operate to independently adjust the lateral spacing of the side portions from one another and the anterior-posterior spacing of the frontal portion from the side portions. The appliance is expanded in stages to maximize the utilization of corrective lower jaw movements which result from securing the appliance in the patient's upper mouth.
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BACKGROUND OF THE INVENTION
1) Field of the Invention
The Application relates to a process for the preparation of pure melamine according to claim 1 .
2) Description of the Related Art
In the high-pressure processes for the preparation of melamine, in general urea melt and optionally gaseous ammonia are reacted without the presence of a catalyst, for example at temperatures between 325 and 450° C., preferably between 350 and 425° C., and pressures between 50 and 250 bar to give liquid melamine and off gas. The reaction off gas mainly comprises ammonia and carbon dioxide, with small amounts of gaseous melamine. In addition to unconverted urea, the liquid crude melamine also contains byproducts, such as, for example, melem, melam and further condensation products of melamine, which are undesired in the end product and therefore have to be separated off. The melamine byproducts are separated from melamine by utilizing the known fact that the byproducts hydrolyze with water, preferably in the presence of alkalis, to give oxoaminotriazine compounds, such as ammeline and ammelide. During the subsequent melamine crystallization, these are kept in solution so that the pure melamine crystallizes out selectively. In these melamine processes, the melamine melt from the high pressure part is worked up in a downstream low pressure part in the presence of water.
According to U.S. Pat. No. 3,132,143, for example, the reaction mixture from the high pressure synthesis reactor, consisting of the melamine melt and the off gas, is fed to a quencher in which the mixture is brought into contact with an aqueous solution saturated with ammonia and carbon dioxide, at from 100 to 200° C. and from 10 to 35 bar for from 10 to 60 min. On contact with the cool quench solution, the melamine is absorbed therein while the major part of the off gas is separated off. For the degradation of the byproducts, the melamine solution is allowed to reside for from 20 to 50 min, the NH 3 and CO 2 contained is then removed with the aid of steam and, after addition of alkali-containing mother liquor and filtration of insoluble products, the melamine crystallizes out.
A disadvantage of this process is the fact that the melamine off gas is separated from the melamine only in the quencher and is thus obtained at a low pressure level and in a state which is not anhydrous. Since the off gas mainly comprises NH 3 and CO 2 , considerable amounts of CO 2 are introduced into the wet part of the plant. CO 2 which has already been separated off is even recycled into the melamine process via the CO 2 -containing quench liquid, with the result that the CO 2 content of the melamine solution is increased and hence the pH of the solution is reduced. This is disadvantageous in particular for the byproduct degradation preferably taking place in the alkaline range during the residence in the quencher, since this takes place slowly and incompletely under these conditions. The total CO 2 is stripped from the melamine solution only in the steam stripper of the wet part. This is also very energy-consumptive.
WO 00/29393 A1 or WO 03/045927 A1 describes melamine preparation processes in which the melamine melt is separated from the reaction off gas in the high pressure reactor itself. The off gas is obtained in anhydrous form and at high pressure and is recycled into the urea plant. The melamine melt fed for further working-up accordingly already contains a CO 2 content reduced by the proportion of off gas. Subsequently, the CO 2 dissolved in the melamine melt is removed from the melt, for example by passing through NH 3 . The melamine melt pretreated in this manner is then fed to the quencher, in which the melamine melt is converted into a melamine suspension or solution by contact with an aqueous, alkali-containing solution. In order to accelerate the byproduct degradation and to keep oxoaminotriazine compounds formed thereby, ammeline and ammelide, in solution, NaOH is added to the melamine solution before it is allowed to reside for byproduct degradation. Dissolved NH 3 still present is then stripped out and the melamine finally crystallizes out. A disadvantage of these processes is the fact that considerable amounts of CO 2 are still present in the melamine suspension or solution discharged from the quencher. Said amounts arise because of incomplete CO 2 removal in the high pressure part and as a result of hydrolytic decomposition of unconverted urea and melamine byproducts in the quencher. The total CO 2 present must be neutralized by adding NaOH. Only on further addition of NaOH does the pH increase. A high pH is required for rapid byproduct degradation during the subsequent residence of the melamine solution. This results in very large amounts of NaOH for the desired high melamine purity with low byproduct contents, which amounts are undesired for economic and logistical reasons.
It was accordingly the object to provide a melamine process which has a reduced NaOH consumption in combination with the same energy characteristics of the plant and the same quality of the end product melamine.
SUMMARY OF THE INVENTION
According to the invention, this object is achieved by quenching the melamine melt with water having a purity of more than 95% by weight and by removing the CO 2 and NH 3 , present in the melamine solution, before the addition of NaOH and before allowing residence for the byproduct degradation.
The present invention accordingly relates to a process for the preparation of pure melamine by working up a melamine melt obtained from a high pressure process and freed from the reaction off gases, in which
a) the melamine melt is quenched with water having a purity of more than 95% by weight, b) NH 3 and CO 2 are then removed from the melamine solution obtained and c) alkali is then added to the melamine solution and said solution is then allowed to reside, d) whereupon pure melamine is obtained by crystallization.
According to the invention, the total CO 2 , on the one hand entrained from the high pressure part and on the other hand formed in the quencher itself by hydrolysis, is removed from the melamine solution directly after the quenching with water having a purity of 95% by weight. Thus, alkali is subsequently added to a virtually CO 2 -free melamine solution, which leads to an immediate pH increase in the melamine solution. Since a high pH is required for rapid byproduct degradation during the subsequent residence, the same melamine quality as in the known comparative processes is achieved in the process according to the invention with smaller amounts of alkali.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a block diagram of the process of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
In the present process, any melamine melt originating from a high pressure process can be used after the reaction off gases have been separated off. Particularly pure melamine is obtained if the melamine melt is prepurified before the quenching, in the high pressure part of the melamine plant. For example, it is possible partly to remove byproducts present in the melt by cooling and/or residence of the melamine melt under high-ammonia pressure. It is advantageous to use ammonia-saturated melamine melt in the present process.
In a preferred embodiment, the CO 2 dissolved in the melamine melt is substantially removed before the quenching. This is effected, for example, by treatment of the melamine melt with gaseous ammonia. In this way, only relatively small proportions of CO 2 have to be removed from the melamine solution in the wet part after the quenching, which is advantageous with respect to energy.
The melamine melt to be worked up according to the present process is fed to the quencher at a temperature of from about 330 to 400° C., preferably from about 330 to 380° C., particularly preferably from about 330 to 360° C., and a pressure of from about 50 to 600 bar, preferably from about 50 to 250 bar, particularly preferably from about 70 to 170 bar.
In the quencher, the quenching of the melamine melt is effected with water having a purity of more than 95% by weight, with the result that the melamine melt is converted into a melamine solution.
Advantageously used water is boiler feed water and/or condensed steam. It is furthermore possible to use the worked-up and purified waste water of the melamine plant for quenching the melamine melt in the quencher.
The quenching of the melamine melt is advantageously effected at from 170 to 220° C., particularly preferably at from 180 to 200° C. The increased temperature during quenching makes it possible to obtain a more highly concentrated melamine solution owing to the greater melamine solubility. This permits smaller apparatus volumes in the wet part and has energy advantages in the removal of NH 3 and CO 2 as a result of the recycling of small amounts of water. Unconverted urea or intermediates is or are hydrolyzed in the quencher to give NH 3 and CO 2 . The exact temperature in the quencher can be established via the ratio of quench water to melamine melt and/or via the quench water temperature. The pressure in the quencher is, for example, the equilibrium pressure established at the respective temperature.
It is advantageous if the melamine solution obtained during the quenching has a melamine concentration of from 10 to 40% by weight, preferably from 20 to 30% by weight, particularly preferably 25% by weight. In this case, the ratio of quench water to melamine melt is about 3 t of quench water/t of melamine melt. NH 3 and CO 2 are then removed from the melamine solution discharged from the quencher. This is advantageously effected at virtually the same temperature as the quenching or at a higher temperature than the quenching. This ensures that the hydrolysis beginning in the quencher can be continued and the resulting CO 2 and NH 3 can be separated off immediately. The temperature is chosen to be so high that there is no danger with regard to crystallization of melamine during the removal of NH 3 and CO 2 . After the CO 2 and NH 3 removal, a purified melamine solution having about the same melamine concentration as at the quencher discharge is obtained. For example, the melamine concentration is about 25% by weight and the temperature about 200° C.
It is advantageous if the removal of NH 3 and CO 2 from the melamine solution is effected in a rectification column, NH 3 and CO 2 being stripped from the melamine solution with steam and being recovered in the form of a liquid which is as concentrated as possible. This has the advantage that, when the recovered contents are recycled in a urea plant or into the liquid fertilizer area, the energy used in the respective plant is not adversely affected by an excessively great water supply. The recovery is effected, for example, as liquid NH 3 with up to about 20% by weight of CO 2 or as ammonium carbonate liquor or in the form of two fractions as ammonium carbonate liquor and as liquid NH 3 .
Before the residence of the purified melamine solution for byproduct degradation, alkali is added to the melamine solution. The alkali used may be, for example, NaOH or KOH. NaOH, for example an aqueous NaOH solution having an NaOH concentration of about 50% by weight, is preferably used. The amount of alkali is from about 30 to 60 kg, preferably from 40 to 50 kg of 50% strength NaOH per t of melamine. The addition of alkali results in an increase in the pH, a pH between pH 9 and 12 being advantageous. A high pH is desirable for sufficiently rapid byproduct degradation.
Advantageously, the purified, virtually NH 3 - and CO 2 -free melamine solution, which has a melamine concentration of from about 10 to 4.0% by weight, preferably from 20 to 30% by weight, particularly preferably 25% by weight, is diluted to a melamine concentration of 5-20% by weight, preferably about 8% by weight, before the residence. Starting from 170 to 220° C., preferably from 180 to 200° C., the temperature of the melamine solution is reduced thereby to 120 to 200° C., preferably to 125 to 170° C., particularly preferably to 130° C. The dilution and cooling of the melamine solution result in a simple mode of operation for the subsequent melamine working-up steps.
It is advantageous if the dilution and cooling are effected by adding a solution containing recycled crystallization mother liquor. Since the crystallization mother liquor is alkali-containing, the fresh alkali supply can be reduced in this way. Moreover, the melamine yield of the plant increases as a result of the recycling and the amount of waste water to be worked up decreases.
It is possible to carry out the alkali addition and the addition of the dilution and cooling solution simultaneously. For example, alkali and dilution and cooling solution can be mixed and then fed together to the melamine solution. The advantage of thorough mixing and homogeneous distribution of the individual streams is achieved thereby. It is furthermore possible for the alkali addition and the addition of the dilution and cooling solution to be effected separately from one another in any desired sequence.
After the alkali addition, residence of the melamine solution is effected. Byproducts, such as, for example, melem and melam, are degraded thereby. The residence time is advantageously from 5 to 60, preferably from 20 to 40, min. In this way, the undesired melamine hydrolysis taking place simultaneously with the byproduct degradation can be kept low.
After the byproduct degradation, the melamine crystallizes out from the melamine solution, optionally after a pH adjustment. This is effected, for example, by temperature reduction and/or application of a vacuum. After subsequent filtration and drying, pure melamine is obtained.
The melamine obtainable by the present process has a purity of at least 99.8% and can be fed for any desired further processing.
EXAMPLE 1
NaOH Consumption in a Melamine Process According to the Prior Art
The crude melamine melt produced in the reactor is separated from the reaction off gases, and the melamine melt is then treated by passing through NH 3 and then introduced into a quencher. Since the melamine melt contains 1.5% by weight of CO 2 , 15 kg of CO 2 per t of melamine melt are introduced into the quencher.
In the quencher, the melamine melt is brought into contact with NaOH-containing liquid. According to the equation
2 NaOH+CO 2 →Na 2 CO 3 +H 2 O
the NaOH reacts with the CO 2 present to give Na 2 CO 3 and is therefore not available for the pH increase desired for the byproduct degradation.
Since 2 moles of NaOH are required per mole of CO 2 , 54.5 kg of 50% strength NaOH are required per t of melamine melt from the synthesis part, simply for destroying the CO 2 introduced with the melamine melt into the quencher.
A further 45.5 kg of 50% strength NaOH/t of melamine melt are required for the byproduct degradation, i.e. the alkaline byproduct hydrolysis until the desired melamine purity is reached.
Accordingly, the resulting total NaOH consumption is 100 kg/t of melamine melt.
EXAMPLE 2
NaOH Consumption in the Process According to the Invention
A melamine melt which originates from a high pressure process and has been freed from the reaction off gases is treated with gaseous ammonia prior to quenching, in order to remove dissolved CO 2 substantially from the melamine melt. The melamine melt treated in this manner is fed to the quencher at a temperature of 350° C. and a pressure of 150 bar. The quenching is effected at 200° C. with boiler feed water. 3 t of quench water are added per t of melamine melt, which results in a melamine solution having a concentration of 25% by weight. NH 3 and CO 2 are then stripped from the melamine solution with steam at 200° C. The solution containing 25% by weight of melamine is diluted with recycled crystallization mother liquor to a melamine concentration of 8% by weight, the temperature of the solution being reduced to 130° C. 45.5 kg of 50% strength NaOH solution per t of melamine melt fed in are added for the byproduct degradation of the melamine solution, and the solution is allowed to reside for 30 min. The melamine is then crystallized out by temperature reduction, and the crystalline melamine is filtered and dried.
Since, in the process according to the invention, the NaOH is not fed in until after the complete removal of CO 2 , the total amount of NaOH fed in is available only for the byproduct degradation. Accordingly, 54.5 kg of 50% strength NaOH, which are required in the comparative process for the CO 2 neutralization, are saved per t of melamine melt. In the melamine process according to the invention, an NaOH saving of at least half compared with a known comparative process is therefore achieved with the same melamine quality.
In FIG. 1 , an embodiment of the process according to the invention is described by way of example.
The melamine melt which originates from a high pressure process and has been freed from the reaction off gases and was treated with gaseous ammonia prior to quenching is introduced into a quencher. NH 3 and CO 2 are then stripped from the melamine solution in a rectification column. The NH 3 and CO 2 stripped off are removed for further use. The melamine-containing solution is then diluted with crystallization mother liquor. An alkali-containing solution is added to the dilute melamine solution for byproduct degradation, and the solution is allowed to remain in a residence tank. The byproducts are then separated off and the melamine is crystallized out, filtered and dried.
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The invention relates to a method for producing pure melamine by preparing a melamine melt, which is obtained in a high pressure process and from which the reaction gases are removed. Said method is characterized in that the melamine melt is quenched by water with a purity in excess of 95 wt. %, that NH 3 and CO 2 are subsequently removed from the obtained melamine solution and that alkali is added to said melamine solution and the mixture is then left to rest, whereby pure melamine is obtained by crystallization. Thus a melamine can be obtained with the same quality as that produced in known comparative methods, using smaller quantities of alkali.
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BACKGROUND OF THE INVENTION
This invention relates to cards in which fibrous material in the form of a thin layer is processed by a series of surfaces driven to move relative to each other and provided with a plurality of points of various shapes, inclination and rigidity, in which the fibrous material is opened into individual fibres, the impurities and trash are removed, and the fibres are mixed together to form a fibre sliver which is collected in large cans to be fed to the subsequent processing stages.
SUMMARY OF THE INVENTION
The present invention relates in particular to the transfer of the sliver from the carding unit to the device for packaging the sliver in the collection can.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a fragmentary perspective view of a carding unit, and illustrates a device for monitoring and regulating the tension of a sliver including a pivotal bar 11 beneath which the sliver passes and a sensor for detecting the rotary movement of the bar which is reflective of the tension of the sliver.
FIG. 2 is a fragmentary enlarged view of the sliver tension monitoring and regulating device, and illustrates details thereof.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the carding unit 1 the fibres separated and mixed together in the carding operation are formed into a web having sufficient consistency to be drawn through a condenser by a roller unit 2, also known as a drafting unit. This sliver is fed to the collection unit 3 which pulls it from the carding unit by means of two rollers (not shown in the figure) and packages it into cans 4 by means of a rotary distributor plate which deposits it inside the can in the form of superposed turns. The rotary distributor 5 is eccentric to its support plate 6 which lies above the can 4 being filled. Collecting the sliver in cans for its feed to subsequent processes means that carding is independent of the subsequent operations.
The sliver produced by carding has a low resistance to traction and must be adequately processed. For this, its packaging in cans as superposed spirals enables it to be subsequently extracted without generating tensions which cannot be withstood by virtue of the low strength of the sliver. For correct transfer of the sliver between the two units, the linear speed with which it leaves the roller unit 2 of the carding unit must be slightly less than that with which it is drawn by the rollers located in the unit by which it is collected in the can 4, so producing a slight drafting effect.
The present invention relates specifically to the control of this transfer and in particular to the monitoring and regulation of the tension generated in the sliver by the two roller units in sequence.
In the known art the sliver is generally monitored by a normal yarn feeler which senses the presence or absence of the sliver, ie its continuity or its breakage, in this latter case it causing stoppage of the card/collection assembly. In this respect it represents a production loss and requires the sliver continuity to be restored by the action of the operator.
The object of the present invention is the preventive monitoring of the sliver tension, in order to be able to act to correct any tension excesses or deficiencies before they give rise to breakages or other problems. Such unbalance can be a symptom not only of mere operational inaccuracy of the rollers but can also indicate more complicated problems, which merit timely preventive action.
To illustrate with greater clarity the characteristics and advantages of the present invention, a typical embodiment thereof is described hereinafter with reference to FIGS. 1 and 2, by way of non-limiting example.
The sliver tension monitoring device 10, which constitutes a very important characteristic of the present invention and is described hereinafter with reference to the enlarged view of FIG. 2, is positioned at the exit of the rollers 2 of the carding unit 1 along the path of the sliver 7 towards the guide pulleys 8a, b, c of the collection unit 3.
The device 10 consists of an arched bar 11 of rounded cross-section enabling the sliver to travel in a direction transverse to it in moving in accordance with the arrow A from the rollers 2 to the pulleys 8, and pivoted on the pivot 12 to rotate about its axis 13. The sliver 7 is deviated by the deviating bar 11 in its path towards 8 to form a loop the width of which depends on its tension. A rod 14 is positioned on the opposite side of the pivot 12 to the arched bar 11 in a manner coplanar with this latter, to undergo rotational movements into positions indicated by the angle α and coherent with the corresponding movements of the bar 11. Said bar 11 and the rod 14 hence form a two-armed lever pivoted at 12. At the opposite end to the bar 11, the rod 14 is provided with an opposition spring 15 which provides a resistance to its movement deriving from the action of the sliver, to an extent based on its elastic characteristic. The rod 14 can also be provided with counterweights, not shown in FIG. 2, which are slidable and fixable along it in order to preset the bar/rod rocker assembly at values determined by its rotary momentum. The rotational movements of said rod 14 are measured by the position sensor 16, for example a transducer generating a signal corresponding to the angular position α which the rod 14, combined with the bar 11, assumes on the basis of the tension of the sliver 7. It is apparent that an increase in the sliver tension results in the bar 11 rising by rotating anticlockwise in the direction of the arrow B, whereas a decrease in the sliver tension results in the bar 11 lowering by rotating clockwise in the direction of the arrow C.
The sensor 16 is connected to the control unit 17 for the overall carding and collection machine and receives from it the limiting values of the angle α, for example α1 and α2 measured with respect to a reference line 18 preferably lying in the rotational plane of the rod 14 and passing through the intersection of the axis 13 with said plane, these angles corresponding to the maximum and minimum allowable tension for the sliver. The connection line 19 is used to transmit the relevant data in real time.
According to a modified embodiment of the present invention, the sensor 16 for measuring the angular deviation of the sliver can be replaced by a sensor for measuring the angular momentum generated on the pivot 12, for instance on a transducer 20 which generates a signal corresponding to the torsional angular momentum τ generated by the sliver 7 under tension deviated about the bar 11, which must be monitored and remain for example between limiting values τ1 and τ2 corresponding to the maximum and minimum allowable tension for the sliver. In all cases the sliver tension is measured by sensors on the basis of the effect induced by this on the bar 11 in the direction of rotation indicated by the arrows B and C.
The signals generated by said sensors are transmitted to the control unit 17, which continuously compares the received values with the allowable limiting values which have been fed into it, for example angular position α or angular momentum τ values, and corresponding to the maximum and minimum allowable sliver tension in its portion 7. Said control unit is provided with intervention means to consequently implement the necessary actions. For example, if these values are outside the range of allowable values, it halts the carding/collection machine, to allow adjustment and inspection before the sliver breaks. Alternately, it could change the speed of the collection unit to adapt it to the carding rate, within the limits of an allowable adjustment range.
At the rod 14 there is provided a rod stop fork 21, to be mounted during a controlled halt of the machine, after which the sliver transfer by the rollers ceases, its tension falls and the signal generated by the connected sensor loses significance.
The monitoring device according to the present invention can also be used as a yarn feeler to sense the presence of sliver along the path 7. Sliver breakage results in the sliver tension dropping to zero, which is obviously outside the range of allowable values. It is also advantageous because of its attenuation effect on any sliver movement irregularities, provided the tension remains within the allowable tension range during these. The loop in the path 7 at the bar 11 forms a "reserve" of sliver to be accumulated and returned during these irregularities. A further advantage of the present invention is the effect of making the sliver can collection unit geometrically independent of the carding unit. In this respect it can be located in the most convenient position relative to the carding unit for any given case, as the tension along the free portion of the sliver is monitored. The collection unit can also be easily moved from one carding unit to another.
Although a preferred embodiment of the invention has been specifically illustrated and described herein, it is to be understood that minor variations may be made in the apparatus without departing from the spirit and scope of the invention, as defined the appended claims.
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A device for monitoring and regulating the tension in the sliver produced by a carding unit and transferred from this along a path to a unit for its collection into cans for further processing, comprising a deviator bar pivoted on a pivot and an oppositely located rod provided with an element which opposes the rotary movement of the bar deriving from the variations in tension of the sliver deviated by it, the sliver tension being measured by sensors on the basis of the effect induced by the sliver on the bar, the relative signals being transmitted to the control unit which compares the values received with the allowable limiting values and implements the consequent interventions.
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BACKGROUND OF THE INVENTION
[0001] 1. Technical Field
[0002] The present invention relates in general to hybrid drill bits and, in particular, to an improved system, method, and apparatus for a hybrid drill bit having a combination of rolling cones and fixed cutter elements for cutting at a center of the drill bit.
[0003] 2. Description of the Related Art
[0004] In the prior art, some drilling bits use a combination of one or more roller cones and one or more fixed blades. Some of these combination-type drill bits are referred to as hybrid drill bits. Previous designs of hybrid drill bits, such as U.S. Pat. No. 4,343,371, to Baker, III, have provided for the roller cones to do most of the formation cutting, especially in the center of the hole or bit. Other types of combination drill bits are known as “core bits,” such as U.S. Pat. No. 4,006,788, to Garner. Core bits typically have truncated roller cones that do not extend to the center of the bit and are designed to remove a core sample of formation by drilling down but around a solid cylinder of the formation before being removed.
[0005] Another type of hybrid drill bit is described in U.S. Pat. No. 5,695,019, to Shamburger, Jr., wherein the roller cones extend almost entirely to the center. Fixed cutter inserts 50 ( FIGS. 2 and 3 ) are located in the dome area 2 or “crotch” of the bit to complete the removal of the drilled formation. Still another type of hybrid bit is sometimes referred to as a “hole opener,” an example of which is described in U.S. Pat. No. 6,527,066. A hole opener has a fixed threaded protuberance that extends axially beyond the roller cones for the attachment of a pilot bit that can be a roller cone or fixed cutter bit. In these latter two cases the center is cut with fixed cutter elements but the fixed cutter elements do not form a continuous, uninterrupted cutting profile from the center to the perimeter of the bit.
[0006] Although each of these drill bits is workable for certain limited applications, an improved hybrid drill bit with enhanced drilling performance would be desirable.
SUMMARY OF THE INVENTION
[0007] One embodiment of a system, method, and apparatus for a hybrid drill bit comprises both roller cones and fixed blades. Some of the fixed cutting elements on the fixed blades are located at and near the axial center of the bit body to cut formation at the axial center. The roller cone cutting elements and the fixed cutting elements combine to define a cutting profile that extends from the axial center to the radial perimeter. The fixed cutting elements form the cutting profile at the axial center and the perimeter, while the roller cone cutting elements assist the fixed cutting elements in the midsection of the cutting profile between the axial center and the perimeter.
[0008] The midsection comprises a nose section and a shoulder section. The nose and shoulder sections are known to be the most vulnerable parts of a fixed cutter bit and are subject to extreme loading and wear. The nose is the leading part of the overall profile and the shoulder must resist side loading and lateral vibrations. In one embodiment, some of the roller cone cutting elements and the fixed cutting elements are axially aligned at the nose of the bit.
[0009] The foregoing and other objects and advantages of the present invention will be apparent to those skilled in the art, in view of the following detailed description of the present invention, taken in conjunction with the appended claims and the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] So that the manner in which the features and advantages of the present invention, which will become apparent, are attained and can be understood in more detail, more particular description of the invention briefly summarized above may be had by reference to the embodiments thereof that are illustrated in the appended drawings which form a part of this specification. It is to be noted, however, that the drawings illustrate only some embodiments of the invention and therefore are not to be considered limiting of its scope as the invention may admit to other equally effective embodiments.
[0011] FIG. 1 is a bottom view of one embodiment of hybrid drill bit constructed in accordance with the present invention;
[0012] FIG. 2 is a side view of the hybrid drill bit of FIG. 1 and is constructed in accordance with the present invention;
[0013] FIG. 3 is a side view of the hybrid drill bit of FIG. 1 and is constructed in accordance with the present invention; and
[0014] FIG. 4 is composite rotational side view of the roller cone inserts and the fixed cutting elements on the hybrid drill bit of FIG. 1 and is constructed in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0015] Referring to FIGS. 1-3 , one embodiment of a system, method, and apparatus for a hybrid drill bit is disclosed. The drill bit 11 comprises a bit body 13 having an axis 15 that defines an axial center of the bit body 13 . A plurality (e.g., two shown) of roller cone support arms 17 extend from the bit body 13 in the axial direction. The bit body 13 also has a plurality (e.g., also two shown) of fixed blades 19 that extend in the axial direction. The number of each of arms 17 and fixed blades 19 is at least one but may be more than two. In one embodiment, the centers of the arms 17 and fixed blades 19 are symmetrically spaced apart from each other about the axis 15 in an alternating configuration.
[0016] Roller cones 21 are mounted to respective ones of the arms 17 . Each of the roller cones 21 is truncated in length such that the distal ends of the roller cones 21 are radially spaced apart from the axial center 15 ( FIG. 1 ) by a minimal radial distance 23 . A plurality of roller cone cutting inserts or elements 25 are mounted to the roller cones 21 and radially spaced apart from the axial center 15 by a minimal radial distance 27 . The minimal radial distances 23 , 27 may vary according to the application, and may vary from cone to cone, and/or cutting element to cutting element.
[0017] In addition, a plurality of fixed cutting elements 31 are mounted to the fixed blades 19 . At least one of the fixed cutting elements 31 is located at the axial center 15 of the bit body 13 and adapted to cut a formation at the axial center. In one embodiment, the at least one of the fixed cutting elements 31 is within approximately 0.040 inches of the axial center. Examples of roller cone cutting elements 25 and fixed cutting elements 31 include tungsten carbide inserts, cutters made of super hard material such as polycrystalline diamond, and others known to those skilled in the art.
[0018] As shown in FIG. 4 , the roller cone cutting elements 25 and the fixed cutting elements 31 combine to define a cutting profile 41 that extends from the axial center 15 to a radially outermost perimeter 43 with respect to the axis. In one embodiment, only the fixed cutting elements 31 form the cutting profile 41 at the axial center 15 and the radially outermost perimeter 43 . However, the roller cone cutting elements 25 overlap with the fixed cutting elements 31 on the cutting profile 41 between the axial center 15 and the radially outermost perimeter 43 . The roller cone cutting elements 25 are configured to cut at the nose 45 and shoulder 47 of the cutting profile 41 , where the nose 45 is the leading part of the profile (i.e., located between the axial center 15 and the shoulder 47 ) facing the borehole wall and located adjacent the radially outermost perimeter 43 .
[0019] Thus, the roller cone cutting elements 25 and the fixed cutting elements 31 combine to define a common cutting face 51 ( FIGS. 2 and 3 ) in the nose 45 and shoulder 47 , which are known to be the weakest parts of a fixed cutter bit profile. Cutting face 51 is located at a distal axial end of the hybrid drill bit 11 . At least one of each of the roller cone cutting elements 25 and the fixed cutting elements 31 extend in the axial direction at the cutting face 51 at a substantially equal dimension and, in one embodiment, are radially offset from each other even though they axially align. However, the axial alignment between the distal most elements 25 , 31 is not required such that elements 25 , 31 may be axially spaced apart by a significant distance when in their distal most position. For example, the bit body has a crotch 53 ( FIG. 3 ) defined at least in part on the axial center between the arms 17 and the fixed blades 19 .
[0020] In one embodiment, the fixed cutting elements 31 are only required to be axially spaced apart from and distal (e.g., lower than) relative to the crotch 53 . In another embodiment, the roller cones 21 and roller cone cutting elements 25 may extend beyond (e.g., by approximately 0.060-inches) the distal most position of the fixed blades 19 and fixed cutting elements 31 to compensate for the difference in wear between those components. As the profile 41 transitions from the shoulder 47 to the perimeter or gage of the hybrid bit 11 , the rolling cutter inserts 25 are no longer engaged (see FIG. 4 ), and multiple rows of vertically-staggered (i.e., axially) fixed cutting elements 31 ream out a smooth borehole wall. Rolling cone cutting elements 25 are much less efficient in reaming and would cause undesirable borehole wall damage.
[0021] The invention has several advantages and includes providing a hybrid drill bit that cuts at the center of the hole solely with fixed cutting elements and not with roller cones. The fixed cutting elements are highly efficient at cutting the center of the hole. Moreover, due to the low cutting velocity in the center, the super hard material or polycrystalline cutting elements are subject to little or no wear. The roller cones are configured to enhance the cutting action of the blades in the most difficult to drill nose and shoulder areas, which are subjected to high wear and vibration damage in harder, more abrasive formations. The crushing action of the tungsten carbide roller cone inserts drives deep fractures into the hard rock, which greatly reduces its strength. The pre-fractured rock is easier to remove and causes less damage and wear to the fixed cutting elements. The perimeter or gage of the borehole is generated with multiple, vertically-staggered rows of fixed cutter inserts. This leaves a smooth borehole wall and reduces the sliding and wear on the less wear-resistant rolling cutter inserts.
[0022] While the invention has been shown or described in only some of its forms, it should be apparent to those skilled in the art that it is not so limited, but is susceptible to various changes without departing from the scope of the invention.
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A hybrid drill bit having both roller cones and fixed blades is disclosed. The cutting elements on the fixed blades form a continuous cutting profile from the perimeter of the bit body to the axial center. The roller cone cutting elements overlap with the fixed cutting elements in the nose and shoulder sections of the cutting profile between the axial center and the perimeter. The roller cone cutting elements crush and pre-fracture formation in the weak and highly stressed nose and shoulder sections.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a sewing machine mounted with a support frame drive unit for moving a workpiece cloth.
2. Description of the Prior Art
The sewing machine detachably mounted with a support frame drive unit (hereinafter referred to simply as "drive unit") has been described in Japanese Laid-Open Patent Publication No. HEI-4-364887. In this Laid-Open Patent Publication, as shown in the explanatory diagrams shown in FIGS. 9(a) and 9(b), a workpiece cloth is supported by an embroidery frame 102 on the drive unit 100. The embroidery frame 102 is attached to a support portion. This support portion is moved in the front-and-back direction by a Y-direction movement mechanism 104. The Y-direction movement mechanism 104 moves in the left-and-right direction according to an X-direction movement mechanism. The Y-direction movement mechanism 104 is exposed on the external part of the drive unit 100, while the X-direction movement mechanism is provided inside the drive unit 100. Thus, when the drive unit 100 is removably mounted on the sewing machine, the embroidery frame 102 can be moved forward and backward or left and right beneath the vertically moving sewing machine needle.
Recently, large embroidery patterns have become fashionable. Thus, the movement ranges of the X-direction movement mechanism and the Y-direction movement mechanism 104 have been expanded along with the embroidery frame 102. The drive unit 100 itself has been made larger in order to accommodate these larger embroidery patterns. However, since a considerable amount of space is required to store the sewing machine when it is mounted with the drive unit 100, in some cases it is more suitable to separate the two. In addition, the sewing machine is sometimes stored with the embroidery frame 102 attached to the drive unit 100 to eliminate both the possibility of losing the embroidery frame 102 and the trouble required to remove and attach the same from the drive unit 100.
However, when the sewing machine is stored with the embroidery frame 102 attached to the drive unit 100, as described above, the area in which the embroidery frame 102 and drive unit 100 overlap is small, and the surface area (seen from above, as in FIG. 9(a)) occupied by the embroidery frame 102 and the drive unit 100 is large. Thus, a large area is occupied by the drive unit 100. A very large amount of space will be necessary particularly if a large embroidery frame 102 is attached to the drive unit 100.
The dimensions X1 and Y1 of FIG. 9(a), for example, are longer than the respective dimensions X2 and Y2 of FIG. 9(b). Thus, the drive unit 100 in the state shown in FIG. 9(a) requires more width and depth than the drive unit 100 shown in FIG. 9(b).
Hence, if the drive unit 100 is set next to a wall or other objects, the embroidery frame 102 and the drive unit 100 must be positioned in such a way as not to bump against the wall or other objects. In addition, the drive unit 100 might not fit into an area if a part attached externally to the drive unit 100 that moves with the embroidery frame 102 (the Y-direction movement mechanism 104, for example) is not in a suitable position.
SUMMARY OF THE INVENTION
In view of the above descriptions, it is an object of the present invention to provide a sewing machine with a support frame drive unit that can easily be stored.
To achieve the above and other objects, there is provided, according to one aspect of the invention, a sewing machine that includes a sewing machine body, a needle vertically movable for stitching a workpiece cloth, a support frame for supporting the workpiece cloth, a support frame drive unit, and a control means. The support frame drive unit has a frame movement mechanism for moving the support frame with respect to the needle. The support frame drive unit is detachably connected to the sewing machine body. The control means controls the frame movement mechanism so as to reduce an area occupied by the support frame drive unit and the support frame.
A manual operation button is further provided, which, when pressed, inputs a start instruction into the control means for causing the control means to start reduction of the area occupied by the support frame drive unit and the support frame.
A storage means is also provided for storing an updated position of the support frame and a predetermined storage position. When the manual operation button is pressed, the frame movement mechanism moves the support frame from the updated position to the predetermined storage position. The storage means comprises a nonvolatile memory for storing the updated position of the support frame, whereby the updated position of the support frame remains unerased even if the sewing machine is powered off.
The storage means may store a plurality of different predetermined storage positions. In this case, when the manual operation button is pressed, the frame movement mechanism moves the support frame from the updated position to a selected one of the plurality of different predetermined storage positions.
There is also provided a set of manual frame movement keys for moving the support frame with respect to the needle. Also, a display is provided for displaying a positional relationship between the support frame drive unit and the support frame. A position to which the support frame drive unit is moved is settable with the set of manual frame movement keys while viewing the positional relationship between the support frame drive unit and the support frame displayed in the display. The frame movement mechanism moves the support frame to the position to reduce the area occupied by the support frame drive unit and the support frame.
When the support frame drive unit detached from the sewing machine body is to be stored in a storage container having an inner accommodating space, the control means controls the frame movement mechanism to move the support frame in a position where the support frame drive unit and the support frame are fittedly insertable into the inner accommodating space of the storage container.
According to another aspect of the invention, there is provided a sewing machine system that includes a needle vertically movable for stitching a workpiece cloth, a support frame for supporting the workpiece cloth, a support frame drive unit having an installation portion for installing the support frame and a support frame drive unit having a frame movement mechanism for moving the support frame with respect to the needle and the installation portion, a sewing machine body to which the support frame drive unit is detachably mounted, a storage container for containing the support frame drive unit after the support frame drive unit is detached from the sewing machine body, and control means for controlling the frame movement mechanism so as to provide the support frame drive unit in a predetermined condition for insertion into the storage container.
According to still another aspect of the invention, there is provided a sewing machine that includes a needle vertically movable for stitching a workpiece cloth, a support frame for supporting the workpiece cloth, a support frame drive unit having a frame movement mechanism for moving the support frame with respect to the needle, a sewing machine body to which the support frame drive unit is detachably mounted, setting means for setting a stop position of the frame movement mechanism, memory means for storing the stop position set by the setting means, and control means for stopping the frame movement mechanism according to the stop position stored by the memory means.
BRIEF DESCRIPTION OF THE DRAWINGS
The particular features and advantages of the invention as well as other objects will become apparent from the following description taken in connection with the accompanying drawings, in which:
FIG. 1 is a diagram showing a sewing machine of the present invention in a state not suitable for storage;
FIG. 2 is a diagram showing a sewing machine of the present invention in a state suitable for storage;
FIG. 3 is a diagram showing the state of a sewing machine of the present invention in which the surface area of the drive unit and the embroidery frame has been decreased;
FIG. 4 is an electrical block diagram for a sewing machine of the present invention;
FIG. 5 is a flowchart of the present invention;
FIG. 6 is a diagram showing the display screen on a sewing machine of the present invention;
FIG. 7 is a diagram showing a storage container for a sewing machine and drive unit of the present invention;
FIG. 8 is a diagram showing a storage container for a sewing machine and drive unit of the present invention;
FIG. 9(a) is a diagram showing a drive unit in a state not appropriate for storage;
FIG. 9(b) is a diagram showing a drive unit in a state appropriate for storage; and
FIG. 10 is a diagram showing display screens on a sewing machine that relates to claim 5 of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
A sewing machine according to a preferred embodiment of the present invention will be described while referring to the accompanying drawings.
First the configuration of a sewing machine 10 will be described. A shuttle mechanism (not shown in the diagrams) well known in the art is provided inside the bed portion 12, which is the base of the sewing machine 10. A column portion 14 is vertically provided on the right side of the bed portion 12. The left side portion of the bed portion 12 is configured to be mountable by a support frame drive unit 16 (hereinafter referred to as "drive unit 16") to be described later. A liquid crystal display (LCD) 20 is provided on the front of the column portion 14. A touch panel 18 is attached to the LCD 20. An arm portion is formed from the top of the column portion 14 to extend out over the bed portion 12. A sewing needle 22 is provided on the arm portion above the shuttle mechanism in such a way as to move vertically in cooperative operation with the shuttle. The shuttle mechanism and the sewing needle 22 are driven in synchronism with a sewing machine motor 24 and other drive motors internal to the sewing machine 10.
As shown in FIG. 4, the display of the LCD 20 is controlled by a CPU 26 of the control unit based on data stored in a ROM 28, internal memory. The sewing conditions of the sewing machine 10 are input into the CPU 26 by pressing buttons on the touch panel 18 according to information displayed on the LCD 20. The CPU 26 follows the program stored in the ROM 28 according to the conditions input, controlling the sewing machine motor 24 and the like. A RAM 30 internal to the sewing machine 10 is used by the CPU 26 for such controlling operations. According to the program stored in the ROM 28, a user can select embroidery patterns and issue an accommodation command by pressing buttons on the touch panel 18. A command for the sewing machine 10 to begin sewing is input to the CPU 26 when the user pushes the start/stop switch 32.
Recently, there has been a demand for large embroidery patterns or many embroidery patterns. However, since the internal memory of the sewing machine 10 is limited, the sewing machine 10 has been configured to accept a card ROM 34, which is an external memory medium. The CPU 26 sequentially reads embroidery data from the card ROM 34 and then controls the sewing machine motor 24 and the drive unit 16 according to that data. In addition, a nonvolatile memory 25 is provided inside the sewing machine 10 that sequentially stores the positions of the embroidery frame 36 and holds the position data even when the power source of the sewing machine 10 is turned off.
Next, the drive unit 16, which is removably mounted in the sewing machine 10, will be described.
The drive unit 16, which is L-shaped when viewed from the top, can be removably fitted into the bed portion 12. A Y-direction movement mechanism 38 is provided on the top surface of the drive unit 16. An embroidery frame 36 for supporting a workpiece cloth is removably attached to the Y-direction movement mechanism 38. When the drive unit 16 is mounted in the sewing machine 10, the CPU 26 controls a Y-direction movement motor 40 of the Y-direction movement mechanism 38, which moves the embroidery frame 36 in the front-and-rear direction, i.e., Y-direction, relative to the sewing machine 10. An X-direction movement mechanism is provided inside the drive unit 16 for moving the Y-direction movement mechanism 38 in the left-and-right direction relative to the sewing machine 10. When the drive unit 16 is fitted into the sewing machine 10, the CPU 26 controls an X-direction movement motor 44 of the X-direction movement mechanism. A detailed description of these devices will be omitted here as the same devices are described in Japanese Laid-Open Patent Publication No. HEI-4-364887.
Next, operations for arranging the drive unit 16 in a condition for storage will be described with reference to the flowchart in FIG. 5.
The user fits the drive unit 16 and inserts the card ROM 34 into the sewing machine 10 and turns on the power source for the sewing machine 10. The CPU 26 displays on the LCD 20 the initial screen shown in FIG. 6 for selecting a category of embroidery patterns (S10). When a category is chosen (S14: yes), a screen for selecting embroidery patterns in that category is displayed (S16), allowing the user to choose a desired pattern. When a selection is made (S20: yes), the selected pattern is displayed (S22). At this point, if the user presses the start/stop switch 32 (S26: yes), the CPU 20 will drive the sewing machine motor 24, Y-direction movement motor 40, X-direction movement motor 44, and the like, based on data in the card ROM 34 (S30), causing the sewing needle 22 and embroidery frame 36 to move with respect to one another. The CPU 26 automatically and sequentially stores in the nonvolatile memory 25 the current positions of the embroidery frame 36 with respect to the sewing needle 22, in order that the current position is always saved even if the power is turned off.
After the sewing process is completed, if the surface area occupied by the drive unit 16 and embroidery frame 36 is large (as shown in FIG. 9(a)), in other words, if the drive unit 16 is in a state not appropriate for storage, the user presses the return key to again display the initial screen in the LCD 20 (S24: yes: S18: yes) and presses the portion on the lower part of the screen equivalent to a storage key 48 (S12: yes). The CPU 26 will determine that a command has been input to decrease the surface area occupied by the drive unit 16 and the embroidery frame 36 for storage.
Next, the CPU 26 calculates the amount of drive needed to move the embroidery frame 36 from its current position, which is stored in the nonvolatile memory 25, to the position stored in the ROM 28 (position of the embroidery frame 36 when the drive unit 16 is prepared for storage) (S32). The CPU 26 then drives the Y-direction movement motor 40 and the X-direction movement motor 44 based on the calculation obtained in step S32, moving the embroidery frame 36 (S36) to minimize the surface area occupied by the drive unit 16 and the embroidery frame 36, as shown in FIG. 2 and FIG. 9(b). The drive unit 16 is now in a state appropriate for storage. The user removes the drive unit 16 from the sewing machine 10 and stores the drive unit 16, which is now in a state specified for storage, in a specified repository. Note that the embroidery frame 36 is only moved when the sewing needle 22 is raised above a specified level to prevent damage to the sewing needle 22.
Even if the sewing machine 10 stops unexpectedly and must be turned on again, the drive unit 16 can be accurately positioned in the storage state, because the position of the embroidery frame 36 is continually being stored.
The drive unit 16 is tested at the factory to verify that it operates properly with the sewing machine 10 and is packaged and shipped only if the operations are normal. Due to the various tests conducted on the drive unit 16, the Y-direction movement mechanism 38 has not always come to a stop in a specified position once the tests are completed. Shock absorbing members are provided in the packaging box to absorb impacts during shipment. These shock absorbing members contact with the drive unit 16 and are formed and positioned to prevent the drive unit 16 from bouncing around in the box. In most cases, the shock absorbing members must be arranged in predetermined positions in relation not only to the drive unit 16, but to the stopped position of the Y-direction movement mechanism 38. Hence, operation efficiency is low because the user must position the Y-direction movement mechanism 38 using manual operation keys for moving the frame of the sewing machine 10. Therefore, if the user coordinates the stopped position of the Y-direction movement mechanism 38 and the state required to store the drive unit 16 in the box according to the sewing machine described in the embodiment above, the storage operation is made more efficient.
Sometimes the repository for the drive unit 16 is adjacent to other articles, forcing the opening through which the drive unit 16 is inserted into the repository to be of a fixed formation. That is, the positions of the embroidery frame 36 and Y-direction movement mechanism 38 on the drive unit 16 must be specified. Hence, if the drive unit 16 was originally inserted into the repository, the user can accurately reinsert the drive unit 16 into the repository after sewing, by putting the drive unit 16 of the sewing machine described above into a storage state. Storing of the drive unit 16 is made easy, because it can be automatically arranged into a suitable state for storage.
In the embodiment described above, the position of the embroidery frame 36 shown in FIG. 2 is described as the storage position. However, the storage position may not be such a position but a different position may be selected for the operator's convenience. For example, the storage position may be so determined that the Y-direction movement mechanism 38 is in the leftmost position and the embroidery frame 36 is the rearmost position.
In the embodiment described above, the surface area of the drive unit 16 and the embroidery frame 36 is made smallest for storage, but the embroidery frame 36 may be moved to a position where the surface area of the drive unit 16 and the embroidery frame 36 could simply be reduced, instead. For example, the embroidery frame 36 could be moved from the position shown in FIG. 1 to that shown in FIG. 3, thereby reducing the width in the front-to-rear direction.
Also, the predetermined storage position described in the embodiment above is fixed at one position, but the user could change the storage positions of the embroidery frame 36 and the Y-direction movement mechanism 38 to any positions that will suit the repository for the drive unit 16. Then, the embroidery frame 36 and the Y-direction movement mechanism 38 will automatically move to the positions set by the user when the user presses the storage key 48.
When the frame movement manual keys 60 are displayed on the LCD 20 as shown in FIG. 10, for example, a set storage position key 62 could be configured to cause the display to change to the lower screen in the diagram when pressed, at which time the storage condition of the drive unit 16 could be set by manipulating the frame movement manual keys 60 while referring to the display. When performing this storage condition setting, the embroidery frame 36 could be configured either to actually move or not to move in response to the frame movement manual keys 60. If the embroidery frame 36 does not actually move at this time, then the storage condition display portion 64 will move in response to the frame movement manual keys 60. Next, data for a new position of the embroidery frame 36 that can be used when storing the drive unit 16 is stored in the nonvolatile memory 25 when the setting complete key 68 is pressed. In this way, various stop positions for the embroidery frame 36 can be set to prepare the drive unit 16 for storage. Although only one type of storage condition was described in the embodiment above, the user could set a plurality of storage conditions and select any one of them as the need arises.
In the embodiment described above, the storage key 48 is displayed only in the initial screen, but the same could be displayed in other screens, such as the pattern select screen, as well. In particular, displaying the storage key 48 at the end of a sewing process would eliminate the extra steps required to return to the initial screen. Also, the process of placing the drive unit 16 in a condition for storage could be linked to the operation of turning off the power switch on the sewing machine 10. This operation would require that the sewing machine 10 had been stopped in a normal state.
In the embodiment above, reduction of the drive unit 16 for a repository was described. Next, storage of the drive unit 16 in a storage container 50 for containing the drive unit 16 will be described.
When manufacturing the storage container 50 for containing the drive unit 16, the storage container 50 would be very large if the width of the storage space is set at the maximum width of the drive unit 16 (the portion containing the Y-direction movement mechanism 38 is at maximum width: Wmax). It is desirable to minimize the size of the storage container 50.
When storing the drive unit 16 in a storage container 50 while the embroidery frame 36 is still attached, the position of the Y-direction movement mechanism 38 for storage is specified, and a storage space (inside the protrusion portion 50a) is formed for storing only the drive unit 16 and the embroidery frame 36 in the position specified. In this way, the storage container 50 can be made smaller than in a condition made suitable for all stop conditions of the embroidery frame 36. The positions of the Y-direction movement mechanism 38 and the embroidery frame 36 can be specified according to the sewing machine 10 of the embodiment described above. In this way, the drive unit 16 can be reliably stored. Moreover, this method prevents the Y-direction movement mechanism 38, embroidery frame 36, and storage container 50 from being damaged by contact with each other and prevents the embroidery frame 36 from dropping out of the drive unit 16.
Further, if the embroidery frame 36 is removed from the drive unit 16 anyway when storing the drive unit 16 in the storage container 50, the storage space other than that taken up by the Y-direction movement mechanism 38 can be set to the width Wh of the main part of the drive unit 16. Hence, a small storage container 50 can be achieved, by providing a storage space of width Wmax for only the portion designed to contain the Y-direction movement mechanism 38, while the remaining portions are provided at width Wh. The position of the Y-direction movement mechanism 38 is similarly specified according to the sewing machine 10 described above. In this way, the drive unit 16 can be reliably stored in the storage container 50. Moreover, this method prevents damage caused by contact between the Y-direction movement mechanism 38 and the storage container 50.
Further, the storage container 50 for the drive unit 16 and the storage container 50b for the sewing machine 10 can be formed as one unit, as shown in FIG. 8. In this case, an opening portion for inserting the sewing machine 10 is formed on the lower surface, and a front surface portion 50c on the storage container 50 can be opened and closed for inserting the drive unit 16.
As can be appreciated from the above description, storage space for the support frame drive unit can be made small by reducing the area occupied by the support frame drive unit and the support frame. In addition, storage is facilitated by leaving the support frame attached, thereby reducing the trouble of removing the support frame and the possibility of losing the same.
When the need arises, the user can input a command to begin reducing the area occupied by the support frame drive unit and the support frame. The support frame drive unit can then be smoothly stored, providing there are no obstructions in the storage area.
The support frame drive unit can be detached from the sewing machine and stored in a storage container designed for containing the support frame drive unit. Also, the support frame drive unit can be inserted into the storage container while mounted with the support frame. This method prevents damage caused by contact between the support frame and the storage container and prevents the support frame from dropping out of the support frame drive unit. Further, the process of arranging the support frame in a position suitable for storage is greatly reduced.
The stop condition of the support frame drive unit is set by the user, enabling the support frame drive unit to conform to many storage conditions.
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A sewing machine having an embroidery frame and a drive unit for driving that frame with respect to the sewing needle, wherein the area occupied by the frame and drive unit can be reduced for storage. To do this, the user presses a storage button on an LCD touch panel screen. The CPU determines that a command has been given to reduce the area of the frame and drive unit for storage; calculates the amount of drive necessary to move the embroidery frame from its current position stored in nonvolatile memory to the position used for storing the drive unit; and controls drive motors to move the embroidery frame the distance calculated, reducing the overall area occupied by the frame and drive unit.
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This is a continuation of application Ser. No. 926,512, filed July 20, 1978 now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to the pipeline charging of preheated coal into coke ovens and the problems incurred by the presence of coal fines in such a system and the recovery of those coal fines.
2. Description of the Prior Art
In the known methods for controlling and recovering coal fines in a preheated pipeline coal charging system, the preheated and pressurized coal is directed firstly through a primary cyclone into which the larger particles of coal are deposited. The balance of the fluid, composed of varying sizes of coal fines and not gases, next passes through a secondary cyclone system where the bulk of the fine solids entrained in the hot gases are deposited. The hot gases, carrying less than 0.5% of the original coal charged, are then piped through a scrubber, where the balance of the entrained coal fines are removed and reclaimed.
About 90% of the coal particles are deposited in the primary cyclone with most of the balance of 10% being deposited in the secondary cyclone system. The coal deposited in the primary cyclone is almost entirely larger than 100 mesh size. The finer coal, deposited in the secondary cyclone system, is of a fine mesh ranging in size from about 100 mesh (150 microns) down to smaller than 400 mesh, with the bulk of these fines, more than 90%, being less than 325 mesh (44 microns) in size.
The coal from both the primary cyclone and the secondary cyclone system is fed into a conveyor system which, in turn, feeds the coal to a distribution bin. The coal from the distribution bin, still at an elevated temperature, is then pumped into coke ovens via pipelines. Thus the pipeline charging of the coke ovens is complete. Most of the high pneumatic pressure or steam pressure used to pump the coal through is bled off from the pipeline prior to the coke oven and is channeled to the by-product train; the balance passes through the coke oven and then into the by-product train.
Problems have developed in this system of pipeline charging. The finer particles of coal, recovered from the secondary cyclone system, develop into "carry-over" when introduced into the coke ovens as the oven is being charged. As this fine coal enters a hot coke oven, a portion of it rapidly devolatilizes into gases, causing, consequently, a high velocity in the gases that are discharged into the gas collecting system. This high exit velocity of rapidly devolitilized gases carries a larger quantity of entrained fine coal particles than is found with conventional coke oven charging systems. This increased quantity of coal fines has been found to overload the charging liquor systems of pipeline charged coke ovens. Also, the fine coal particles that are blown out of the oven are accompanied by fine tar droplets that result from the coal devolitilization. The mixture tends to compact in such places as the standpipes and the charging mains. This accumulation significantly reduces the efficiency of the coke oven by-products system and is difficult and costly to remove.
The result of these problems is a relegation of the coal fines collected in the secondary cyclone system to the status of low grade boiler fuel in an effort to eliminate fine particles of less than 100 mesh from the system. Due to the increasing scarcity of metallurgical grade coal and the commensurate increasing cost thereof, the use of that coal for low grade boiler fuel is quite uneconomical. A method for utilizing these coal fines in coking operations in a manner which eliminates the problems described previously is needed.
SUMMARY OF THE INVENTION
The present invention is directed to a method by which the coal fines from the secondary cyclone of a size of 325 mesh (44 microns) or smaller can be recovered and reintroduced into the pipeline charging system in such a form that those coal fines will not choke the coke oven off-gas system nor overload the charging liquor system. The method utilizes an advantage presented by the elevated temperature state of the coal fines in the secondary cyclone system.
Coal fines in the secondary cyclone system have a degree of elevation of temperature such that when the coal fines come into contact with liquified hydrocarbons, such as bunker C oil or coal tar, the viscosity of such fluids is reduced and an affinity of such liquids for the source of the heat is enhanced.
The coal fines are extracted from the secondary cyclone system and deposited into a means for mixing those coal fines with a liquid hydrocarbon solution. The means for mixing insures that each coal fine particle is thoroughly coated with liquid hydrocarbon which acts as a binder. Optionally, other types of binders, not hydrocarbon based, may be used, such as spent sulfite liquors from the wood processing industry.
The coated coal fines are then extracted from the means for mixing and processed through a means of compaction which squeezes the coated coal fines, forcing them to become a dense stratified mass. The coal fines become bonded together, or agglomerated.
The agglomeration of the coal fines into larger sized particles of coal produces a form which can now be reintroduced directly into the pipeline charging system at a size in excess of 100 mesh, thus eliminating the problems produced by the coal fine of less than 325 mesh. The structural integrity of the agglomerated coal fines is sufficient to prevent breakup during the pipeline charging operation, to withstand the turbulance of fluid coal pumped through the pipelines. The velocity of the off-gases from charging are equivalent to those encountered in conventional coke oven charging.
Accordingly, the principal features of this invention are the elimination of coal fine choking of the charging off-gas system and the elimination of the overloading of the charging liquor system, thus allowing the economical and efficient utilization of metallurgical grade coal fines of less than 325 mesh size in the production of coke in a pipeline charging coke oven battery.
These and other features of this invention will be more completely disclosed and described in the following specification, the methods claimed and the accompanying diagramatic drawing.
BRIEF DESCRIPTION OF THE DRAWINGS
The sole FIGURE in the drawing is an illustrated flow diagram of an embodiment of a method in accordance with the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Metallurgical grade coal, commonly used in the coke manufacturing process, is fed, usually in a wet state, into a preheater, generally designated by the numeral 10. The coal is pre-pulverized before entry into the preheater. Preheat gas is introduced into the preheater 10 from a combustion chamber, generally designated by the numeral 12, where it mixes with and preheats the coal. The preheat gas is at an average temperature of 1400° F., ranging from 1200° to 1600° F., and at an average velocity of 80 feet per second. The combustion chamber 12 is generally fired by a mixture of coke oven gas, air and recycle gas with small amounts of entrained coal dust.
The coal introduced into the preheater 10 is entrained in superheated gas from the combustion chamber 12, the combination of which produces a very turbulent fluid which serves to break up the coal by striking the particles thereof against each other. Also, the rapid flashing into steam of the water content in the coal probably causes the coal particles to literally explode, further breaking up the particles into smaller pieces.
The velocity of the preheat gas conveys the preheated coal upwardly into a disburser, generally designated by the numeral 14, which further tends to evenly distribute coal particles within the preheat gas. The preheated and sized coal particles become suspended in the preheat gas. Alternately, it is possible to eliminate the disburser, the previous mixing of the coal particles in the preheat gas being sufficient.
The velocity of the preheat gas carries the coal upwardly, through a conduit, from the disburser 14 to a primary cyclone, generally designated by the numeral 16. In the primary cyclone 16 the larger particles of coal, almost entirely larger than 100 mesh size, are separated from the gas flow to the extent that the motive preheat gas, at this point, contains only fine particles of coal dust or coal fines.
The preheat gas with entrained coal fines exits the primary cyclone 16, upwardly through a conduit, to a series of secondary cyclones or a secondary cyclone system, generally designated by the numeral 18. The individual secondary cyclones 20, 21, 22, 23, 24, 25, 26 and 27 are arranged in parallel such that most of the finer particles of coal are separated from the motive preheat gas thereby. The secondary cyclone system 18 serves to remove all but 0.5% of the entrained coal from the preheat gas.
A portion of the preheat gas, about half, mixed with a proportionate half of the 0.5% residue of the coal fines, is circulated back to the combustion chamber 12 as recycle gas. The balance of the preheat gas, along with the balance of the 0.5% residue of the coal fines, is conducted through a scrubber, not shown, where that balance of the coal fines is removed. The scrubbed gas is then expelled to the atmosphere through an exhaust stack, also not shown.
The coal particles that have been deposited in the primary cyclone 16 are metered into a primary conveyor, generally designated by the numeral 28, which transports those coal particles to a distribution bin, generally designated by the numeral 30.
The coal particles that have been deposited in the secondary cyclone system 18, about 90% of which are smaller than 325 mesh (44 microns), are metered into a mixer, generally designated by the numeral 34. An inexpensive readily available liquid hydrocarbon, such as coal tar, is also fed, in a solvent solution, into the mixer. Alternatively, non-hydrocarbon liquid can be used such as, for example, spend sulfite liquor, a waste product of the wood processing industry. The heat from the preheated coal fines serves to reduce the viscosity of the coal tar, increasing its wetability to the point where it readily coats the coal fines. The mixture of coal tar and coal fines, which gives the appearance of wet coal, is driven through the mixer by an auger, generally designated by the numeral 36. The auger 36 forces the coal-tar mixture of coal tar and coal fines into a compactor, generally designated by the numeral 38. Preferably, the compactor contains a set of smooth closely-set rolls, generally designated by the numeral 40, rotating in reverse directions and aligned parallel to each other, although briquetting, pelletizing or prilling agglomeration methods may be used. The coal-tar mixture is fed through the rolls 40 as they rotate. The rotation of the rolls 40 squeezes the coal-tar mixture, compressing the coated coal fines into a sheet. The sheet of coal fines breaks up immediately, as it exits the compactor, into chips or flakes equivalent to the coal particles already being fed into the distribution hopper 30. The size of the flakes can be varied by spacing the rolls at different distances apart and/or adding a flake-breaking disintegrator 42.
The flakes are metered into a secondary conveyor 32 which transports them into the primary conveyor 28 which, in turn, transports them to the distribution hopper 30.
All of the coal in the distribution hopper 30 is conveyed through a pipeline, under high superheated steam pressure, into coke ovens, not shown.
According to the provisions of the patent statute, the principle, the preferred method and the mode of operation of the present invention have been explained and what is considered its preferred embodiment have been illustrated and described. However, it is to be understood that, within the scope of the appended claims, the present invention may be practiced otherwise than as specifically illustrated and described.
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Coal fines developed from the processing of coal through a preheating system are accumulated in a secondary cyclone system. The coal fines, at an elevated temperature, are mixed with a hydrocarbon organic binder and compressed into larger particles of sufficient structural integrity and mass to be fed directly through pneumatic pressure coke oven coal charging lines without significant size reduction, resulting in the elimination of fine coal build-up in one coke oven standpipes and charging mains as well as overloading of the charging liquor system.
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FIELD OF THE INVENTION
The invention relates to a vessel comprising a hull having a turret, a cavity in the turret and a mooring buoy releasably attached in the cavity, the buoy comprising a buoyant body and carrying a number of risers extending to a subsea hydrocarbon well and a number of anchor lines connected to the sea bed, wherein upon connection of the buoy to the cavity, the buoy is attached to a pulling member connected to a winch on the vessel for lifting of the buoy.
BACKGROUND OF THE INVENTION
Such a disconnectable mooring system is disclosed in U.S. patent application US2007/155259. The known system includes a buoy that is provided with a conical outer casing and a corresponding conical cavity or receptacle on the vessel's turret structure, which cavity has a cone shape corresponding to the conical outer casing of the buoy member. The turret structure includes a turntable carrying conduits to be connected to the risers, wherein the turntable is supported on a bearing assembly in a manner allowing rotation with respect to the turret structure to align the conduits with the risers on the buoy only after the buoy is received and locked in the cavity of the turret structure. In this publication it is shown that only a main turret upper roller ball bearing assembly supports the turntable; this assembly includes three mutually movable parts that are directly interconnected to each other. In fact, this upper turret bearing assembly consists of 2 roller ball bearings that are directly placed on top of each other and interconnected via one common inner bearing housing member. This upper bearing assembly has therefore become a very critical and essential part of a weathervaning system. A disadvantage of this combined and interconnected roller ball bearing assembly is that if one or more roller balls fails, the complete assemble has to be changed out, meaning that the turret system cannot function anymore as a weathervaning system. This change out cannot be done offshore.
The known combined roller bearing system, due to the fabrication limitations, is limited to about only 8 meters, so that it not suitable for large disconnectable turret-buoy systems with for example 20 or more risers connected to the buoy.
Another patent publication that describes a disconnectable mooring system that is provided with two separate bearing systems, one of which is used only for rotating a turntable in order to align the manifold pipe ends with the riser ends of a connected buoy, is U.S. Pat. No. 5,651,708. This patent shows a disconnectable buoy that is provided with a bearing system that stays with the boy when disconnected. The buoy is rotatable connected to the moonpool of a vessel under the waterline without the use of a turret. An additional upper bearing system is disclosed at deck level, which supports a turntable with manifold, so that after the buoy is connected directly to the moonpool of the vessel, the turntable can be aligned with the risers of the connected buoy. The turntable is supported by the bearing system, so that even during production when hydrocarbons are received through the flexible piping connecting the manifold and the buoy, the turntable can be rotated at all times and be aligned with the buoy. When the twisting angle in the flexible piping between the buoy and the turntable is exceeded, the turntable is rotated by means of a connected motor driven pinion to a new position neutralizing the twisting. This system is therefore not advantageous for disconnectable turret-buoys systems sized to receive numerous of risers, and of course is not possible when using only hard piping.
Another disconnectable mooring system is described in U.S. patent publication US5823131. This patent discloses a disconnectable riser buoy for supporting only risers or riser lines, but with no mooring lines attached to it.
This riser buoy can be docked within a rotatable turret placed in a moonpool of a floating vessel and carries risers that are connected to flow paths, which are removably coupled to vessel product lines at a position above sea level. When the riser buoy is disconnected from the turret, it is maintained at a submerged depth in the sea by a weight attached to a buoy anchor leg that can be lowered down to the sea floor or raised within the turret. The turret is directly anchored to the sea floor via multiple mooring lines that are connected to the lower turret. When the riser buoy is released, the weight connected to the riser buoy, once resting on the sea floor, will moor the riser buoy and as such limit the excursions of the risers within acceptable limits. Further, as the mooring legs are directly connected to the turret, the riser buoy has only sufficient buoyancy to support the risers.
Another major aspect of this concept is that in order to dock the riser buoy, a retrieval line is pulled upwardly via a winch until the weight contacts the buoy. Then, buoy and weight are hooked up together, the weight being in contact with the bottom of the riser buoy and both riser buoy and weight are placed within the moonpool of the vessel. The main purpose of this system is to allow for hook-up of a pre-installed riser buoy before installation of the vessel and prior to connecting the mooring lines to the turret takes. The known mooring system does not function as a quick disconnectable system that is suitable to be used in cyclone areas or ice infested waters as the mooring legs stays connected to the turret. Also hook-up of both the riser supporting buoy and the weight together is only possible for relatively small buoys and weights and not for large buoys with large connected weights, as this would require a winch capacity exceeding the capacity of winches available in the field and involving the danger of creating large snap-loads in the hauling-in line that connects the buoy and the winch. This results in large winches that are designed to withstand such snatch loads.
In these known systems the capability to reconnect a buoy to a turret is mainly limited by the sea state and winch capacity. When the buoy is brought upwards to the turret for reconnection purposes, the heave motions of the buoy are coupled to those of the vessel when the buoy approaches its connect position. If the sea states are too large, snatch loads and buoy acceleration forces are exerted on the connection lines that exceed the strength of available reconnection lines. This is especially the case for large size buoys, for instance carrying 20 risers or more.
It is therefore an object of the present invention to provide a disconnectable turret-mooring buoy design having an increased reconnection capability even in severe sea states of for example up to 6 m significant wave height.
It is a further object of the present invention to provide a quick disconnectable and easy connectable mooring buoy system for a large numbers of risers and mooring legs, in which snatch loads on the pull-in line are reduced.
It is a further object of the present invention to provide a disconnectable mooring buoy system, which can operate with winches or reconnection chain jacks of reduced size.
The system according to the invention should readily connect and disconnect even in very severe environmental conditions to a floating vessel, for example a floating production unit (FPU or FPSO), using a conventional pull-in line, such as a chain. The buoy should provide accommodation for a large number of risers, for example at least 20 risers and 10 umbilicals, in a turret to which the mooring buoy can be connected. The system according to the present invention should ensure a high availably of the system under all weather conditions and minimize the down time before reconnection even considering the constant severity of the environment.
SUMMARY OF THE INVENTION
Hereto a vessel in accordance with the present invention is characterized in that each anchor line and/or riser at its upper end is connected to a stopper member, the stopper member being attached to the pulling member, wherein during lifting the chains and stopper member are movable relative to the buoyant body in a length direction of the anchor lines and/or risers, and wherein after connection of the buoyant body to the cavity the stopper member is engaged with an abutment member on the buoyant body to support the anchor line and/or riser weight off the body.
Because the heave-induced motions of the buoyant body of the buoy are during connection decoupled from the risers of the lateral mooring system and/or from the riser system, the maximum tension in the pull-in line or reconnection chain or cable is only determined by the lateral mooring system and riser system components, which involve known entities such as pretension, vertical stiffness and dynamic behaviour. These components can be modified and optimized with a larger degree of freedom as by the decoupling, the maximum tension in the pull-in line during reconnection is reduced. This is also important for the chain jack or winch design in case the pull in line is formed by a chain.
Because the maximum tension in the pull-in line is no longer influenced by the mass and added mass of the buoyant body, which is frequency dependent, large dynamic loads in the pull-in line are avoided. Therefore, the size of the buoyant body can be increased without restrictions in order to accommodate larger riser systems in case the system is pulled in through the mooring line fairleads on the buoy or to accommodate larger mooring systems in case the system is pulled in through the riser porches on the buoy.
Dynamic tension amplification in the pull-in line during reconnection, will be significantly reduced due to the relatively low vertical stiffness and added mass of the lateral mooring system. This will allow a larger reconnection seastate.
During disconnecting the buoy from the cavity, the decoupling mechanism according to the invention will not be active as the lateral mooring line fairleads will rest on the buoyant body and no relative motions will be allowed. The mooring line pretension and riser hung weight results in a vertical payload that after disconnecting the buoy from the cavity in the hull of the vessel, will bring the buoy to the predetermined water depth, in a way similar to that of known mooring buoys.
In an embodiment the buoyant body comprises one or more substantially vertical channels with at a lower end anchor line/riser guides for guiding the anchor lines and/or risers through the at least one channel in a vertical direction from a lower end of the buoyant body to an upper end of the buoyant body, the anchor lines and/or risers being at the upper end of the buoyant body connected to the stopper member which is engageable with an abutment member at the top of the buoyant body for preventing movement of the stopper member into the at least one channel.
Upon reconnecting the buoy, the anchor lines and/or risers are lifted via the pull-in line, while the buoyant body rises upwards in view of its buoyancy and is able to move relative to the anchor lines and/or risers. This decouples the heave movements of the buoyant body from the pull-in line and reduces snatch load on the pull-in line. After connection of the buoyant body to the cavity in the hull of the vessel, the weight of the anchor lines and/or risers comes to hang from the buoyant body because these descend in the buoyant body until the stoppers are engaged with the abutment members on the buoyant body.
The stopper member may comprise a circular frame attached to the pulling member. The anchor lines and/or risers may be suspended from the frame and the lower end of the buoy may be provided with guides comprising sheaves that are placed on a circular frame at the bottom of the buoy. The buoyant body of the buoy that is to be latched into the cavity upon reconnection may comprise substantially vertical channels and the anchor lines and/or risers are deflected from their natural angle to extend in a substantially vertical orientation by the sheaves, the buoyant body during upward travel of the buoy being able to move up and down relative to the anchor lines and/or risers.
The buoyant body may comprise a number of substantially vertical frame members extending through vertical channels to a lower part of the buoyant body, wherein anchor lines and/or risers are attached to the frame members and are displaceable in a vertical direction together with the frame members, the lower end of the frame members terminating in an abutment member for engaging with the buoyant body and defining the lower position of the stopper member relative to the buoyant body.
The frame members can move up and down the vertical channels during raising of the buoy into the cavity via the pulling member that is attached to the frame member while the buoyant member is allowed to rise upwards in view of its buoyancy. After connection of the buoyant body to the cavity, stoppers on the vertical frame members are in their lowermost position abutting against the abutment member of the buoyant body.
In again an alternative embodiment, the buoyant body comprises a number of tracks, the pulling member comprising a number of lines running from the top of the buoyant body to each anchor line and/or riser via the tracks and connected to the stopper members which may be displaced over a length of the tracks, the buoyant body comprising a lower abutment member with which the stopper members may be engaged.
The pulling member is via the lines directly connected to the anchor lines and/or risers and pulls the lines or risers upwards, while the buoyant body can travel up and down along the lines during connection for decoupling the buoyant body movement from the anchor lines and/or risers.
In order to prevent yaw motions relative to the anchor lines and risers when the buoy is in its submerged, disconnected state, a lower abutment member on the buoyant body can engage in a non-rotatable manner with stopper members.
In an alternative embodiment, the snatch loads in the pull-in line are reduced by connecting the pull-in line to the buoy via a compression device. The compression device may comprise a resilient member such as rubber pads or a spring, and pulls downward on the pull-in line when the pull-in line goes slack due to downward heave movements of the vessel. In this way the pull-in member remains taut and snatch loads are reduced.
The compression device may comprise a lower flange and a compression spring extending between the flanges, the pulling member being attached to the lower flange, the upper flange being engageable with a stop member upon lifting of the buoy, the spring being compressible by upward movement of the lower flange by the pulling device.
In order to prevent the pull-in line from damaging the top of the buoy when the pull-in line goes slack upon connection and/or disconnection of the buoy to the cavity, the pull-in line may near a top part of the buoyant body be provided with a flexible sheath. In case the pull-in line is formed by a chain, the sheath may be in the form of a flexible hose slightly larger than the chain width to keep the chain at a distance from the buoy when the pull-in line goes slack.
BRIEF DESCRIPTION OF THE DRAWINGS
Some embodiments of a vessel in accordance with the present invention will be explained in detail with reference to the accompanying drawings. In the drawings:
FIG. 1 shows a schematic cross-sectional view of a vessel according to the present invention,
FIG. 2 shows a detail of the upper part of the buoy of FIG. 1 on an enlarged scale,
FIG. 3 shows an embodiment of a movable connection of the buoyant body to the anchor lines that are comprised in vertical channels,
FIGS. 4 a and 4 b show an alternative embodiment of a movable connection of the buoyant body to the anchor lines via vertical frame members,
FIG. 5 shows a further embodiment of a movable connection of the buoyant body to the anchor lines via pulling cables running in channels in the buoyant body, and
FIG. 6 shows an embodiment according to the invention of a resilient shock absorber attached to the pull-in line.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a sectional view of a disconnectable turret mooring system according to the present invention.
The system consists of a cylindrical turret structure 1 located within a cylindrical moonpool 2 integrated into the hull 3 of a vessel 14 , which for example could be a FPU or FPSO. The turret bearing system connecting and aligning the turret to the moonpool of the vessel consists of a large diameter top bogie bearing 4 and (optionally) a bottom low friction pad radial bearing system 5 .
A large multi-deck superstructure 6 is located on top of the turret 1 and houses installation and production equipment, piping manifolds 7 and the fluid/gas swivel stack 8 for the incoming production fluids, exported fluids and the control/chemical umbilicals.
A steel frame is positioned above and around the superstructure. A casing 9 , which is connected to the vessel, supports the piping extending from the fluid swivel stack 8 to the FPU, provides access to the turret 1 from the vessel, drives the rotating part of the swivel and supports the wintering panels. The turret design allows for maintenance and repair in operation, which maximizes its availability over the full field design life.
The upper end of each anchor leg 10 , via which the vessel 14 is moored to the sea bed 15 , is directly connected to a low friction articulated universal joint on the hull of a mooring buoy 11 that is seated in a conical cavity 16 at the lower end of the turret 1 . Risers 12 that are connected to a sub sea hydrocarbon wellhead 15 are with their upper ends connected to a riser deck 17 of the buoy 11 . When the mooring buoy 11 is connected to the vessel or FPU, the upper end of the buoy is clamped into the cavity via hydraulic clamps 25 . The riser deck 17 is elevated above the maximum vessel draft level 23 . This will ensure that under all conditions, the piping equipment is kept permanently in a dry environment to ease access and maintenance.
The mooring buoy 11 has two different functions. Firstly, when the vessel 14 is connected to the buoy 11 , the buoy transfers the mooring loads of the anchor lines 10 which are connected to its outer shell. Secondly, when the vessel is disconnected from the mooring buoy 11 , the mooring buoy falls down to a depth at a predetermined distance below sea level and supports the anchor lines 10 and risers 12 at this depth. The pre-determined depth can be calculated for example 30-35 meters below water level so that the disconnected buoy stabilizes under the wave active zone. In ice and iceberg infested waters for example, the buoy could be stabilized at a distance of even more than 100 m below water level to avoid any contact with ice-bergs.
The mooring buoy structure 11 comprises a stiffened cylindrical shell with watertight internal bulkheads that divide the buoy into compartments. The center of the buoy incorporates a thick walled inner cylinder 18 to house and guide the hauling in or connecting cable 19 that is attached to a winch 20 . The top part of the buoy is fitted with an annular connecting ring on which structural connector ratchets 25 , 25 ′ that are placed within the turret can be locked. I-tubes 21 may in one embodiment be fitted in the center of the buoy, for risers and sub-sea umbilicals and are terminated at the bottom end of the buoy 11 to support the riser/umbilical bell-mouths. Risers bend stiffeners and bell-mouths are protected from ice drifting under the vessel hull by a conical skirt 13 at the bottom of the mooring buoy. Alternatively there also can be protection means against ice like a skirt or fence placed at the bottom of the vessel to protect the moonpool against ice ingress when the vessel is disconnected or to protect the buoy and risers when the mooring buoy is connected to the turret.
The buoyancy required for keeping the risers 12 and anchor legs 10 at the specified level in the disconnected state is provided by central compartments and compartments fitted on the buoy periphery.
The structural arrangement is such that it minimizes the contact between the buoy hull and the turret parts during disconnection, so that there is no risk of accidental flooding. Nevertheless the watertight buoy is compartmented in order to ensure sufficient buoyancy in case of accidental flooding of one compartment.
When the locking members, or hydraulic clamps 25 are disengaged, the buoy 11 is released from the cavity 16 and will sink to a predetermined depth below water level 23 . For reconnecting the buoy 11 to the vessel 14 , the vessel 14 will slowly approach the submerged mooring buoy 11 until a floating pick-up line, that is coupled to a part of the pull-in line 19 that remains attached to the buoy 11 and stored within cylinder 18 can be grappled. The two sections of the pull-in line 19 are then shackled together, the floating pick-up line is removed and the pull-in line 19 is returned over the side. In case of reconnection with ice above, connection of the pull-in line segments will be carried out directly in the dry part of the turret moonpool.
The traction winch 20 is operated such that the mooring buoy 11 is slowly lifted below the vessel 14 and into the cavity 16 of the turret until the buoy top flange will be in contact with the structural connector centralizer. The clamps 25 of the structural connector will be closed and the mechanical locks activated. The vessel is now securely reconnected and moored via the turret 1 to the anchor legs 10 of the mooring buoy 11 .
The anchor lines 10 extend upward through vertical channels 40 , 41 through the buoy 10 , along anchor line guides 42 , 42 ′ and 43 , 43 ′—which may comprise sheaves—, at the lower and upper ends of the buoy 10 to be deflected from an inclined orientation to a substantially vertical orientation. At their upper ends, the anchor lines 10 are connected to a frame 44 that is attached to the pull-in line 19 . The frame 44 forms a stopper member, which rests on abutment surface of the buoy 11 in the connected state shown in FIG. 1 such that the weight of the anchor lines 10 and risers 12 is supported by the buoy. During connection of the buoy 11 , the anchor lines are pulled upwards via the frame 44 and the buoy rises in view of its buoyancy. The buoy 11 can move relative to the anchor lines 10 , in view of the vertical channels 40 , 41 through which the anchor lines are movably guided via anchor line guides 42 , 42 ′, 43 , 43 ′. In this manner tension is maintained on the pull-in line 19 during heave-induced motions of the vessel 14 and snatch loads on the pull-in line- 19 are prevented. After attaching the buoy 11 into the cavity 16 , the frame 40 is supported on top of the buoy, which at its top comprises an abutment surface for supporting the frame 40 . Upon decoupling of the buoy 11 from the cavity 16 , the frame 40 remains rested against the top of the buoy and the buoy and anchor lines sink to a predetermined depth below water level 23 , preferably below the wave active zone.
The mooring buoy 11 is connected without any considerations about its rotational position. Only after the vessel 1 has been safely moored to the buoy 11 , a turntable 31 with the complete turret manifold 7 is rotated to match the piping orientation on the buoy, as has been shown in detail in FIG. 2 . The fact that the complete manifold 7 can be orientated with regard to the turret 1 will avoid performing the alignment of the manifold piping with the mooring buoy piping at a critical stage of the reconnection when the buoy 11 is connected to the traction winch 20 only and is not yet securely moored to the turret 1 .
As has been shown in more detail in FIG. 2 , in order to be rotated around a vertical axis, the manifold structure 7 in the turret 1 is unlocked, a temporary turntable bearing system 32 is activated by displacing it in a vertical direction, such that turntable 31 is lifted from turret land a turntable orientation motor is started. By slowly rotating the turntable 31 , the turret manifold 7 is brought into the correct orientation wherein manifold pipe ends are brought inline with the mooring buoy riser pipe ends. This operation will be monitored from the control panel of the motor and will be controlled from the manifold lower deck. Once the correct turntable orientation has been achieved the turntable manifold will be automatically locked and the temporary turntable bearing system deactivated by displacing the bearing wheels 32 hydraulically in a vertical direction by a few mm so that the lifted and orientated turntable 31 rests again on the turret 1 in a fixed rotational position.
The flow lines, or piping 35 , down stream of the fluid connectors 33 at the interface of the buoy 11 and the cavity 16 , will then be lowered back to their operating position. The fluid connectors 33 interconnecting the ends of the risers 12 and the piping 35 of manifold 7 will be closed and leak tested. Once the isolation valves are opened production can recommence. The umbilicals will be connected using a similar procedure.
In the embodiment that has been shown in FIG. 3 , the buoy 11 comprises a buoyant a body 57 having vertical channels 40 , 41 . The buoy 11 comprises at its lower end 47 a lower circular frame 45 carrying the chain sheaves 42 , 42 ′. The frame 45 can rotate relative to the buoyant body 57 around a vertical axis. At the upper end 48 of the buoy, the anchor lines 10 , 10 ′ are attached to the frame 44 via chain stoppers 49 , 49 ′. By rotation of the frame 45 , the sheaves 42 , 42 ′ remain aligned with the chain stoppers 49 , 49 ′. On the circular frame 44 resilient bumper devices 50 may be provided for contacting the reinforced abutment surface 51 at the top of the buoy 11 . In the connected state, when the buoy 11 is attached to the cavity 16 of the vessel, the bumper devices 50 contact the surface 51 to transfer the weight of the anchor lines 10 , 10 ′ and risers 12 to the buoy 11 . Also upon disconnection of the buoy 11 . from the cavity 16 , the bumper devices 50 are engaged with the upper buoy surface 51 .
FIGS. 4 and 4 a show an alternative embodiment in which the frame 44 comprises vertical frame members 55 , 55 ′ connected to a lower stopper 56 to which the upper ends of anchor lines 10 , 10 ′ are attached. The vertical frame members 55 , 55 ′ can move relative to they buoyant body 57 of the buoy 11 via vertical channels 59 , 59 ′. The vertical frame members 55 , 55 ′ and/or the stopper 56 come to rest on the buoyant body 57 of the buoy 11 in the disconnected state in a non-rotating manner such that no yaw rotation of the buoyant body 57 relative to anchor lines 10 , 10 ′ can occur. For preventing yaw motion of the frame 44 relative to the buoyant body 57 , the stopper 56 may comprise protrusions 60 fitting into recesses 61 on the buoyant body 57 .
FIG. 4 b shows the rigid cage-like construction of the frame 44 , the vertical members 55 , 55 and the stopper 56 at the lower end of frame 44 .
FIG. 5 shows an embodiment wherein an upper connector 65 is attached to cables 66 , 66 ′ extending in inclined channels 67 , 67 ′ in the buoyant body 57 of the buoy 11 . The cables 66 , 66 ′ are connected to stoppers 69 , 69 ′ attaching to the upper ends of anchor lines 10 , 10 ′. The stoppers 69 , 69 ′ can engage with a recess 70 on the buoyant body 57 to prevent yaw rotation of the buoyant body 57 relative to the anchor lines 10 , 10 ′.
FIG. 6 shows an embodiment wherein the pull-in line 19 is attached to a shock-absorbing device 71 , comprising a lower flange 76 , an upper flange 77 and a cylindrical compression spring situated between the flanges 76 , 77 . The pull-in line 19 is attached to the lower flange 76 . When the buoy 11 is pulled upwards by the pull-in line 19 , the upper flange 77 of the shock-absorption device 70 comes to rest against deck 79 and the upward force exerted on the lower flange 76 by the pull-in line 19 compresses the spring 78 . The buoy moves upwards while the spring 78 remains in its compressed stated. Release of the tension on the pull-in line 19 , for instance due to heave movements, causes the spring 78 to expand such that any slack in the pull-in line 19 is taken up. In the embodiment shown in FIG. 6 , the pull-in line goes slack when the buoy is connected to the cavity 16 of the vessel, or when the buoy 11 is allowed to descend after disconnection from the cavity, and the upper flange 77 comes to rest on deck 80 . The chain 19 may be collected in central compartment, or chain locker 80 .
Near the upper part of the buoy 11 , the chain 19 is provided with a sheath 81 , which may be formed by a flexible hose that is slightly larger than the chain width. The sheath 81 prevents the chain 19 from collapsing onto the op of the buoy 11 when the chain 19 goes slack and prevents the chain from damaging the top part of the buoy 11 .
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A vessel includes a hull with a turret, a cavity in the turret and a mooring buoy releasably attached in the cavity, the buoy including a buoyant body and carrying a number of risers, extending to a subsea hydrocarbon well and a number of anchor lines connected to the sea bed, wherein upon connection of the buoy to the cavity, the buoy is attached to a pulling member connected to a winch on the vessel for lifting of the buoy. Each anchor line and/or riser at its upper end is connected to a stopper member, the stopper member being attached to the pulling member, wherein during lifting, each anchor line and/or riser and the stopper member are movable relative to the buoyant body in a length direction of the anchor lines and/or risers, and wherein after connection of the buoyant body to the cavity, the stopper member is engaged with an abutment member on the buoyant body to support the anchor line and/or riser weight off the body.
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BACKGROUND OF THE INVENTION
This invention provides novel compositions of matter. This invention further provides novel processes for producing these compositions of matter. This invention further provides novel chemical intermediates useful in the above processes.
Particularly this invention provides novel analogs of some of the known prostaglandins which differ from corresponding known prostaglandins in that these prostaglandin analogs have a triple bond between C-13 and C-14, that is the C-13 to C-14 -moiety is -C.tbd.C-.
The known prostaglandins include the PGE compounds, e.g. prostaglandin E 1 (PGE 1 ), prostaglandin E 2 (PGE 2 ), prostaglandin E 3 (PGE 3 ), and dihydroprostaglandin E 1 (dihydro-PGE 1 ).
The known prostaglandins include PGF 301 compounds, e.g. prostaglandin F 1 .sub.α (PGF 1 .sub.α), prostaglandin F 2 .sub.α (PGF 2 .sub.α), prostaglandin F 3 .sub.α (PGF 3 .sub.α), and dihydroprostaglandin F 1 .sub.α (dihydro-PGF 1 .sub.α).
The known prostaglandins include PGF.sub.β compounds, e.g. prostaglandin F 1 .sub.β (PGF 1 .sub.β), prostaglandin F 2 .sub.β (PGF 2 .sub.β ), prostaglandin F 3 .sub.β (PGF 3 .sub.β), and dihydroprostaglandin F 1 .sub.β (dihydro-PGF 1 .sub.β).
The known prostaglandins include PGA compounds, e.g. prostaglandin A 1 (PGA 1 prostaglandin A 2 (PGA 2 ), prostaglandin A 3 (PGA 3 ), and dihydroprostaglandin A 1 dihydro-PGA 1 ).
The known prostaglandins include PGB compounds, e.g. prostaglandin B 1 (PGB 1 ), prostaglandin B 2 (PGB 2 ), prostaglandin B 3 (PGB 3 ), and dihydroprostaglandin B 1 (dihydro-PGB 1 ).
Each of the above mentioned known prostaglandins (PG's) is a derivative of prostanoic acid which has the following structure and carbon atom numbering ##STR1## See, for example, Bergstrom et al., Pharmacol. Rev. 20, 1 (1968), and references cited therein. A systematic name for prostanoic acid is 7-[(2β-octyl)-cyclopent-1α-yl]heptanoic acid.
PGE 1 has the following structure: ##STR2##
PGE 2 has the following structure: ##STR3##
PGE 3 has the following structure: ##STR4##
Dihydro-PGE 1 has the following structure: ##STR5##
PGF 1 .sub.α has the following structure: ##STR6##
PGF 2 .sub.α has the following structure: ##STR7##
PGF 3 .sub.α has the following structure: ##STR8##
Dihydro-PGF 1 .sub.α has the following structure: ##STR9##
PGF 1 .sub.β has the following structure: ##STR10##
PGF 2 .sub.β has the following structure: ##STR11##
PGF 3 .sub.β has the following structure: ##STR12##
Dihydro-PGF 1 .sub.β has the following structure: ##STR13##
PGA 1 has the following structure: ##STR14##
PGA 2 has the following structure: ##STR15##
PGA 3 has the following structure: ##STR16##
Dihydro-PGA 1 has the following structure: ##STR17##
PGB 1 has the following structure: ##STR18##
PGB 2 has the following structure: ##STR19##
PGB 3 has the following structure: ##STR20##
Dihydro-PGB 1 has the following structure: ##STR21##
In the above formulas, as well as in the formulas hereinafter given, broken line attachments to the cyclopentane ring indicate substituents in alpha configuration i.e., below the plane of the cyclopentane ring. Heavy solid line attachments to the cyclopentane ring indicate substituents in beta configuration, i.e., above the plane of the cyclopentane ring. The use of wavy lines (˜) herein will represent attachment of substituents in either the alpha or beta configuration or attachment in a mixture of alpha and beta configurations.
The side-chain hydroxy at C-15 in the above formulas is in S configuration. See, Nature 212, 38 (1966) for discussion of the stereochemistry of the prostaglandins. Expressions such as C-13, C-14, C-15, and the like, refer to the carbon atom in the prostaglandin analog which is in the position corresponding to the position of the same number in prostanoic acid.
Molecules of the known prostaglandins each have several centers of asymmetry, and can exist in racemic (optically inactive) form and in either of the two enantiomeric (optically active) forms, i.e. the dextrorotatory and leverotatory forms. As drawn, the above formulas each represent the particular optically active form of the prostaglandin as is obtained from mammalian tissues, for example, sheep vesicular glands, swine lung, or human seminal plasma, from carbonyl and/or double bond reduction of the prostaglandin so obtained. See, for example, Bergstrom et al., cited above. The mirror image of each of these formulas represents the other enantiomer of that prostaglandin. The racemic form of a prostaglandin contains equal numbers of both enantiomeric molecules, and one of the above formulas and the mirror image of that formula is needed to represent correctly the corresponding racemic prostaglandin. For convenience hereinafter, use of the term, prostaglandin or "PG" will mean the optically active form of that prostaglandin thereby referred to with the same absolute configuration as PGE 1 obtained from mammalian tissues. When reference to the racemic form of one of those prostaglandins is intended, the word "racemic" or "dl" will precede the prostaglandin name.
The term "prostaglandin-type" (PG-type) product, as used herein, refers to any cyclopentane derivative which is useful for at least one of the same pharmacological purposes as the prostaglandins, as indicated herein.
The term prostaglandin-type intermediate, as used herein, refers to any cyclopentane derivative useful in preparing a prostaglandin-type product.
The formulas, as drawn herein, which depict a prostaglandin-type product or an intermediate useful in preparating or prostaglandin-type product, each represent the particular stereoisomer of the prostaglandin-type product which is of the same relative stereochemical configuration as a corresponding prostaglandin obtained from mammalian tissues, or the particular stereoisomer of the intermediate which is useful in preparing the above stereoisomer of the prostaglandin-type product.
The term "prostaglandin analog", as used herein, represents that stereoisomer of a prostaglandin-type product which is of the same relative stereochemical configuration as a corresponding prostaglandin obtained from mammalian tissues or a mixture comprising that stereoisiomer and the enantiomer thereof. In particular, where a formula is used to depict a prostaglandin-type compound herein, the term prostaglandin analog refers to the compound and the enantiomer thereof.
The various PG's named above, their esters, acylates and pharmacologically acceptable salts, are extremely potent in causing various biological responses. For that reason, these compounds are useful for pharmacological purposes. See, for example, Bergstrom et al., Pharmacol. Rev. 20, 1 (1968) and references cited therein.
For the PGE compounds these biological responses include:
a. decreasing blood pressure (as measured, for example, in anesthetized, pentulinium-treated rats);
b. stimulating smooth muscle (as shown by tests, for example, on guinea pig ileum, rabbit duodenum, or gerbil colon);
c. effecting lipolytic activity (as shown by antagonism of epinephrine induced relase of glycerol from isolated rat fat pads);
d. inhibiting gastric secretion and reducing undesirable gastrointestinal effects from systematic administration of prostaglandin synthetase inhibitors;
e. controlling spasm and facilitating breathing in asthmatic conditions;
f. decongesting nasal passages;
g. decreasing blood adhesion (as shown by platelet to glass adhesiveness) and inhibiting blood platelet aggregation and thrombus formation induced by various physical stimuli (e.g., arterial injury) or chemical stimuli (e.g., ATP, ADP, serotinin, thrombin, and collagen);
h. affecting the reproductive organs of mammals as labor inducers, abortifacients, cervical dilators, regulators of the estrus, and regulators of the menstrual cycle; and
j. accelerating growth of epidermal cells and keratin in animals.
For the PGF.sub.α compound these biological responses include:
a. increasing blood pressure (as measured, for example, in anesthetized, pentolinium-treated rats);
b. stimulating smooth muscle (as shown by tests on guinea pig ileum, rabbit duodenum, or gerbil colon);
c. inhibiting gastric secretion and reducing undesirable gastrointestinal effects from systematic administration of prostaglandin synthetase inhibitors;
d. controlling spasm and facilitating breathing in asthmatic conditions;
e. decongesting nasal passages;
f. decreasing blood platelet adhesion (as shown by platelet to glass adhesiveness) and inhibiting blood platelet aggregation and thrombus formation induced by various physical stimuli (e.g., arterial injury) or chemical stimuli (e.g., ADP, ATP, serotinin, thrombin, and collagen); and
g. affecting the reproductive organs of mammals as labor inducers, abortifacients, cervical dilators, regulators of the estrus, and regulators of the menstral cycle.
For the PGF.sub.β compounds these biological responses include:
a. decreasing blood pressure (as measured, for example, in anesthetized, pentolinium-treated rats);
b. stimulating smooth muscle (as shown by tests on guinea pig ileum, rabbit duodenum, or gerbil colon); j
c. inhibiting gastric secretion and reducing undesirable gastrointestinal effects from systematic administration of prostaglandin synthetase inhibitors;
d. controlling spasm and facilitating breathing in asthmatic conditions;
e. decongesting nasal passages;
f. decreasing blood platelet adhesion (as shown by platelet to gas adhesiveness) and inhibiting blood platelet aggregation and thrombus formation induced by various physical stimuli (e.g., arterial injury) or chemical stimuli (e.g., ADP, ATP, serotinin, thrombin, and collagen); and
g. affecting the reproductive organs of mammals as labor inducers, abortifacients, cervical dilators, regulators of the estrus, and regulators of the menstrual cycle.
For the PGA compounds these biological responses include:
a. decreasing blood pressure (as measured, for example, in anesthetized, pentolinium-treated rats);
b. stimulating smooth muscle (as shown by tests on guinea pig ileum, rabbit duodenum, or gerbil colon);
c. inhibiting gastric secretion and reducing undesirable gastrointestinal effects from systematic adminstration of prostaglandin synthetase inhibitors;
d. controlling spasm and facilitating breathing in asthmatic conditions;
e. decongesting nasal passages; and
f. increasing kidney blood flow.
For the PGB compounds these biological responses include:
a. stimulating smooth muscle (as shown by tests on guinea pig ileum, rabbit duodenum, or gerbil colon); and
b. accelerating growth of epidermal cells and keratin in animals.
Because of these biological responses, these known prostaglandins are useful to study, prevent, control, or alleviate a wide variety of diseases and undesirable physiological conditions in birds and mammals, including humans, useful domestic animals, pets, and zoological specimens, and in laboratory animals, for example, mice, rats, rabbits, and monkeys.
The prostaglandins so cited above as hypotensive agents are useful to reduce blood pressure in mammals, including man. For this purpose, the compounds are administered by intravenous infusion at the rate about 0.01 to about 50 μg. per kg. of body weight per minute or in single or multiple doses of about 25 to 500 μg. per kg. of body weight total per day.
The PGF.sub.α compounds are useful in increasing blood pressure mammals, including man. Accordingly, these compounds are useful in the treatment of shock (hemorrhagic shock, endotoxin shock, cardiogenic shock, surgical shock, or toxic shock). Shock is marked by pallor and clamminess of the skin, decreased blood pressure, feeble and rapid pulse, decreased respiration, restlessness, anxiety, and sometimes unconsciousness. Shock usually follows cases of injury and trauma. Expert and fast emergency measures are required to successfully manage such shock conditions. Accordingly, prostaglandins, combined with a pharmaceutical carrier which adapts the prostaglandin for intramuscular, intravenous, or subcutaneous use, are useful, especially in the early stages of shock where the need to increase blood pressure is a critical problem for aiding and maintaining adequate blood flow, per fusing the vital organs, and exerting a pressor response by constricting veins and raising blood pressure to normal levels. Accordingly, these prostaglandins are useful in preventing irreversible shock which is characterized by a profound fall in blood pressure, dilation of veins, and venus blood pooling. In the treatment of shock, the prostaglandin is infused at a dose of 0.1-25 mcg/kg./min. The prostaglandin may advantageously be combined with known vasoconstrictors; such as phenoxy-benzamine, norepinephrine, and the like. Further, when used in the treatment of shock the prostaglandin is advantageously combined with steroids (such as, hydrocortisone or methylprednisolone), tranquilizers, and antibiotics (such as, lincomycin or clindamycin).
The compounds so cited above as extremely potent in causing stimulation of smooth muscle are also highly active in potentiating other known smooth muscle stimulators, for example, oxytocic agents, e.g., oxytocin, and the various ergot alkaloids including derivatives and analogs thereof. Therefore, these compounds for example, are useful in place of or in combination with less than usual amounts of these known smooth muscle stimulators, for example, to relieve the symptoms of paralytic ileus, or to control or prevent atonic uterine bleeding after abortion or delivery, to aid in expulsion of the placenta, and during the puerperium. For the latter purpose, the prostaglandin is administered by intravenous infusion immediately after abortion or delivery at a dose in the range about 0.01 to about 50 μg. per kg. of body weight per minute until the desired effect is obtained. Subsequent doses are given by intravenous, subcutaneous, or intramuscular injection or infusion during puerperium in the range 0.01 to 2 mg. per kg. of body weight per day, the exact dose depending on the age, weight, and condition of the patient or animal.
As mentioned above, the PGE compounds are potent antagonists of epinephrine-induced mobilization of free fatty acids. For this reason, this compound is useful in experimental medicine for both in vitro and in vivo studies in mammals, including man, rabbits, and rats, intended to lead to the understanding, prevention, symptom alleviation, and cure of diseases involving abnormal lipid mobilization and high free fatty acid levels, e.g., diabetes mellitus, vascular diseases, and hyperthyroidism.
The prostaglandins so cited above as useful in mammals, including man and certain useful animals, e.g., dogs and pigs, to reduce and control excessive gastric secretion, thereby reduce or avoid gastrointestinal ulcer formation, and accelerate the healing of such ulcers already present in the gastrointestinal tract. For this purpose, these compounds are injected or fused intravenously, subcutaneously, or intramuscularly in an infusion dose range about 0.1 μg. to about 500 μg. per kg. of body weight per minute, or in a total daily dose by injection or infusion in the range about 0.1 to about 20 mg. per kg. of body weight per day, the exact dose depending on the age, weight, and condition of the patient or animal, and on the frequency and route of administration.
These compounds are also useful in reducing the undesirable gastrointestinal effects resulting from systemic administration of anti-inflammatory prostaglandin synthetase inhibitors, and are used for that purpose by concomitant administration of the prostaglandin and the anti-inflammatory prostaglandin synthetase inhibitor. See Partridge et al., U.S. Pat. No. 3,781,429, for a disclosure that the ulcerogenic effect induced by certain non-steroidal anti-inflammatory agents in rats is inhibited by concomitant oral administration of certain prostaglandins of the E and A series, including PGE 1 , PGE 2 , PGE 3 , 13,14-dihydro-PGE 1 , and the corresponding 11-deoxy-PGE and PGA compounds. Prostaglandins are useful, for example, in reducing the undesirable gastrointestinal effects resulting from systemic administration of indomethacin, phenylbutazone, and aspirin. These are substances specifically mentioned in Partridge et al. as non-steroidal, anti-inflammatory agents. These are also known to be prostaglandin synthetase inhibitors.
The anti-inflammatory synthetase inhibitor, for example, indomethacin, aspirin, or phenylbutazone is administered in any of the ways known in the art to alleviate an inflammatory condition, for example, in any dosage regimen and by any of the known routes of systemic administration.
The prostaglandin is administered along with the anti-inflammatory prostaglandin synthetase inhibitor either by the same route of administration or by a different route. For example, if the anti-inflammatory substance is being administered orally, the prostaglandin is also administered orally or, alternatively, is administered rectally in the form of a suppository or, in the case of women, vaginally in the form of a suppository or a vaginal device for slow release, for example as described in U.S. Pat. No. 3,545,439. Alternatively, if the anti-inflammatory substance is being administered rectally, the prostaglandin is also administered rectally. Further, the prostaglandin can be conveniently administered orally or, in the case of women, vaginally. It is especially convenient when the administration route is to be the same for both anti-inflammatory substance and prostaglandin, to combine both into a single dosage orm.
The dosage regimen for the prostaglandin in accord with this treatment will depend upon a variety of factors, including the type, age, weight, sex and medical condition of the mammal, the nature and dosage regimen of the antiinflammatory synthetase inhibitor being administered to the mammal, the sensitivity of the particular individual mammal to the particular synthetase inhibitor with regard to gastrointestinal effects, and the particular prostaglandin to be administered. For example, not every human in need of an anti-inflammatory substance experiences the same adverse gastrointestinal effects when taking the substance. The gastrointestinal effects will frequently vary substantially in kind and degree. But it is within the skill of the attending physician or veterinarian to determine that administration of the anti-inflammatory substance is causing undesirable gastrointestinal effects in the human or animal subject and to prescribe an effective amount of the prostaglandin to reduce and then substantially to eliminate those undesirable effects.
The prostaglandins so cited above as useful in the treatment of asthma, are useful, for example, as bronchodilators or as inhibitors of mediators, such as SRS-A, and histamine which are released from cells activated by an antigen-antibody complex. Thus, these compounds control spasm and facilitate breathing in conditions such as bronchial asthma, bronchitis, bronchiectasis, pneumonia, and emphysema. For these purposes, the compounds are administered in a variety of dosage forms, e.g., orally in the form of tablets, capsules, or liquids; rectally in the form of suppositories; parenterally; subcutaneously; or intramuscularly; with intravenous administration being preferred in emergency situations; by inhalation in the form of aerosols or solutions for nebulizers; or by insufflation in the form of powder. Doses in the range of about 0.01 to 5 mg. per kg. of body weight are used 1 to 4 times a day, the exact dose depending on the age, weight, and condition of the patient and on the frequency and route of administration. For the above use these prostaglandins can be combined advantageously with other anti-asthmatic agents, such as sympathomimetics (isoproterenol, phenylephrine, epinephrine, etc.); xanthine derivatives (theophylline and aminophylline); and corticosteroids (ACTH and prednisolone). Regarding use of these compounds see M.E. Rosenthale, et al., U.S. Pat. No. 3,644,638.
The prostaglandins so cited above as useful in mammals, including man, as nasal decongestants are used for this purpose, in a dose range of about 10 μg. to about 10 mg. per ml. of a pharmacologically suitable liquid vehicle or as an aerosol spray, both for topical application.
The prostaglandins so cited above are useful whenever it is desired to inhibit platelet aggregation, reduce the adhesive character of platelets, and remove or prevent the formation of thrombi in mammals, including man, rabbits, and rats. For example, these compounds are useful in the treatment and prevention of myocardial infarcts, to treat and prevent post-operative thrombosis, to promote patency of vascular grafts following surgery, and to treat conditions such as atherosclerosis, arteriosclerosis, blood clotting defects due to lipemia, and other clinical conditions in which the underlying etiology is associated with lipid imbalance or hyperlipidemia. For these purposes, these compounds are administered systemically, e.g., intravenously, subcutaneously, intramuscularly, and in the form of sterile implants for prolonged action. For rapid response, especially in emergency situations, the intravenous route of administration is preferred. Doses in the range about 0.005 to about 20 mg. per kg. of body weight per day are used, the exact dose depending on the age, weight, and condition of the patient or animal, and on the frequency and route of administration.
These compounds are further useful as additives to blood, blood products, blood substitutes, or other fluids which are used in artificial extracorporeal circulation or perfusion of isolated body portions, e.g., limbs and organs, whether attached to the original body, detached and being preserved or prepared for transplant, or attached to a new body. During these circulations and perfusions, aggregated platelets tend to block the blood vessels and portions of the circulation apparatus. This blocking is avoided by the presence of these compounds. For this purpose, the compound is added gradually or in single or multiple portions to the circulating blood, to the blood of the donor animal, to the perfused body portion, attached or detached, to the recipient, or to two or all of those at a total steady state dose of about 0.001 to 10 mg. per liter of circulating fluid. It is especially useful to use these compounds in laboratory animals, e.g., cats, dogs, rabbits, monkeys, and rats, for these purposes in order to develop new methods and techniques for organ and limb transplants.
The prostaglandins so cited above as useful in place of oxytocin to include labor are used in pregnant female animals including man, cows, sheep, and pigs, at or near term, or in pregnant animals with intrauterine death of the fetus from about 20 weeks to term. For this purpose, the compound is infused intravenously at a dose of 0.01 to 50 μg. per kg. of body weight per minute until or near the termination of the second stage of labor, i.e., expulsion of the fetus. These compounds are especially useful when the female is one or more weeks post-mature and natural labor has not started, or 12 to 60 hours after the membranes have ruptured and natural labor has not yet started. An alternative route of administration is oral.
These compounds are further useful for controlling the reproductive cycle in menstruating female mammals, including humans. By the term menstruating female mammals is meant animals which are mature enough to menstruate, but not so old that regular menstruation has ceased. For that purpose the prostaglandin is administered systemically at a dose level in the range 0.01 mg. to about 20 mg. per kg. of body weight of the female mammal, advantageously during a span of time starting approximately at the time of ovulation and ending approximately at the time of menses or just prior to menses. Intravaginal and intrauterine routes are alternative methods of administration. Additionally, expulsion of an embryo or a fetus is accomplished by similar administration of the compound during the first or second trimester of the normal mammalian gestation period.
These compounds are further useful in causing cervical dilation in pregnant and nonpregnant female mammals for purposes of gynecology and obstetrics. In labor induction and in clinical abortion produced by these compounds, cervical dilation is also observed. In cases of infertility, cervical dilation produced by these compounds is useful in assisting sperm movement to the uterus. Cervical dilation by prostaglandins is also useful in operative gynecology such as D and C (Cervical Dilation and Uterine Curettage) where mechanical dilation may cause perforation of the uterus, cervical tears, or infections. It is also useful in diagnostic procedures where dilation is necessary for tissue examination. For these purposes, the prostaglandin is administered locally or systemically.
The prostaglandin, for example, is administered orally or vaginally at doses of about 5 to 50 mg. per treatment of an adult female human, with from one to five treatments per 24 hour period. Alternatively the prostaglandin is administered intramuscularly or subcutaneously at doses of about one to 25 mg. per treatment. The exact dosages for these purposes depend on the age, weight, and condition of the patient or animal.
These compounds are further useful in domestic animals as an abortifacient (especially for feedlot heifers), as an aid to estrus detection, and for regulation or synchronization of estrus. Domestic animals include horses, cattle, sheep, and swine. The regulation or synchronization of estrus allows for more efficient management of both conception and labor by enabling the herdsman to breed all his females in short pre-defined intervals. This synchronization results in a higher percentage of live births than the percentage achieved by natural control. The prostaglandin is injected or applied in a feed at doses of 0.1-100 mg. per animal and may be combined with other agents such as steroids. Dosing schedules will depend on the species treated. For example, mares are given the prostaglandin 5 to 8 days after ovulation and return to estrus. Cattle, are treated at regular intervals over a 3 week period to advantageously bring all into estrus at the same time.
The PGA compounds and derivatives and salts thereof increase the flow of blood in the mammalian kidney, thereby increasing volume and electrolyte content of the urine. For that reason, PGA compounds are useful in managing cases of renal dysfunction, especially those involving blockage of the renal vascular bed. Illustratively, the PGA compounds are useful to alleviate and correct cases of edema resulting, for example, from massive surface burns, and in the management of shock. For these purposes, the PGA compounds are preferably first administered by intravenous injection at a dose in the range 10 to 1000 82 g. per kg. of body weight or by intravenous infusion at a dose in the range 0.1 to 20 μg. per kg. of body weight per minute until the desired effect is obtained. Subsequent doses are given by intravenous, intramuscular, or subcutaneous injection or infusion in the range 0.05 to 2 mg. per kg. of body weight per day.
The compounds so cited above as promoters and acceleraters of growth of epidermal cells and keratin are useful in animals, including humans, useful domestic animals, pets, zoological specimens, and laboratory animals for this purpose. For this reason, these compounds are useful to promote and accelerate healing of skin which has been damaged, for example, by burns, wounds and abrasions, and after surgery. These compounds are also useful to promote and accelerate adherence and growth of skin autografts, especially small, deep (Davis) grafts which are intended to cover skinless areas by subsequent outward growth rather than initially, and to retard rejection of homografts.
For the above purposes, these compounds are preferably administered topically at or near the site where cell growth and keratin formation is desired, advantageously as an aerosol liquid or micronized powder spray, as an isotonic aqueous solution in the case of wet dressings, or as a lotion, cream, or ointment in combination with the usual pharmaceutically acceptable diluents. In some instances, for example, when there is substantial fluid loss as in the case of extensive burns or skin loss due to other causes, systemic administration is advantageous, for example, by intravenous injection or infusion, separately or in combination with the usual infusions of blood, plasma, or substitutes thereof. Alternative routes of administration are subcutaneous or intramuscular near the site, oral, sublingual, buccal, rectal, or vaginal. The exact dose depends on such factors as the route of administration, and the age, weight, and condition of the subject. To illustrate, a wet dressing for topical application to second and/or third degree burns of skin area 5 to 25 square centimeters would advantageously involve use of an isotonic aqueous solution containing 1 to 500 μg. per ml. of the prostaglandin. Especially for topical use, these prostaglandins are useful in combination with antibiotics, for example, gentamycin, neomycin, polymixin, bacitracin, spectinomycin, and oxytetracycline, with other antibacterials, for example, mafenide hydrochloride, sulfadiazine, furazolium chloride, and nitrofurazone, and with corticoid steroids, for example, hydrocortisone, prednisolone, methylprednisolone, and fluprednisolone, each of those being used in the combination at the usual concentration suitable for its use alone.
Certain PG 2 -type compounds wherein the C-13 to C-14 moiety is --C.tbd.C-- are known in the art. For example, see Gandolfi C., et al., Il Farmaco, 27, 1125, wherein 13,14-didehydro-PGF 2 .sub.α and 13,14-didehydro-PGE 2 and their 15-epimers are described. See further, South African Pat. No. 73-2329, Derwent Farmdoc CPI 54179U, wherein 13,14-didehydro-PGF 2 .sub.α -, PGF 2 .sub.β -, PGE 2 -, and PGA 2 -type compounds are disclosed with optional C-16 alkyl substitution and with optional oxa or thia substitution at the C-3 position. Further, the above South African Patent discloses the 8β,12α-stereoisomer of the above-described compounds. See also J. Fried, et al., Tetrahedron Letters, 3899 (1963), which discloses 13,14-dihydro-PGF 2 .sub.α.
Additionally certain 13-didehydro-PG 1 -type compounds are known in the prior art. See, for example, J. Fried, et al., Annals, of the New York Academy of Science 18, 38 (1971), which discloses 7-oxa-13,14-didehydro-PGF 1 .sub.α. See also R. Pappo, et al., Tetrahedron Letters, 2627, 2630 (1972), which discloses racemic 13,14-dihydro-11β-PGE 1 ; and R. Pappo, et al., Annals. of the New York Academy of Science 18, 64 (1971), which discloses 13,14-didehydro-11β-PGB 1 . Finally, see the following patents which disclose 13,14-dihydro-PGB 1 -type compounds: Belgian Pat. No. 777,022 (Derwent Farmdoc CPI 43791T) German Offenlegungsschrift No. 1,925,672 (Derwent Farmdoc CPI 41,084), and German Offenlegungsschrift No. 2,357,781 (Derwent Farmdoc 42046V).
SUMMARY OF THE INVENTION
This invention provides novel prostaglandin analogs, esters of these analogs, and pharmacologically acceptable salts of these analogs.
This invention further provides lower alkanoates of these analogs.
This invention further provides novel processes for preparing these analogs.
This invention further provides novel chemical intermediates useful in the preparation of these analogs.
The present invention discloses:
1. a prostaglandin analog of the formula ##STR22## wherein Y 1 is --C.tbd.C--; wherein g is one, 2, or 3;
wherein m is one to 5, inclusive;
wherein M 1 is ##STR23## wherein R 5 and R 6 are hydrogen or methyl, with the proviso that one of R 5 and R 6 is methyl only when the other is hydrogen; ##STR24## wherein R 3 and R 4 are hydrogen, methyl, or fluoro, being the same or different, with the proviso that one of R 3 and R 4 is fluoro only when the other is hydrogen or fluoro;
wherein R 1 is hydrogen, alkyl of one to 12 carbon atoms, inclusive, cycloalkyl of 3 to 10 carbon atoms, inclusive, aralkyl of 7 to 12 carbon atoms, inclusive, phenyl, phenyl substituted with one, two, or three chloro or alkyl of one to 3 carbon atoms, inclusive, or a pharmacologically acceptable cation;
2. a prostaglandin analog of the formula: ##STR25## wherein L 1 , R 1 , Y 1 , g, and m are as defined above; and wherein M 2 is ##STR26##
3. a prostaglandin analog of the formula: ##STR27## wherein L 1 , M 1 , R 1 , Y 1 , and g are as defined above;
4. a prostaglandin analog of the formula ##STR28## wherein L 1 , M 1 , R 1 , and Y 1 are as defined above; wherein Z 1 is
1. cis --CH=CH--CH 2 --(CH 2 ) g --CH 2 --,
2. cis--Ch=CH--CH 2 --(CH 2 ) g --CF 2 --,
3. cis--CH 2 --CH=CH--(CH 2 ) g --CH 2 --,
4. --(ch 2 ) 3 --(ch 2 ) g --CH 2 --,
5. --(ch 2 ) 3 --(ch 2 ) g --CF 2 --,
6. --ch 2 --o-ch 2 --(ch 2 ) g --CH 2 --, (7) --CH 2 ) 2 -O-(CH 2 ) g --CH 2 -,
8. --(ch 2 ) 3 --o--(ch 2 ) g --, ##STR29## wherein g is as defined above;
wherein R 7 is
(1) --(CH.sub.2).sub.m --CH.sub.3, ##STR30##
(4) cis--CH=CH--CH.sub.2 --CH.sub.3,
wherein m is one to 5, inclusive, T is chloro, fluoro, trifluoromethyl, alkyl of one to 3 carbon atoms, inclusive, or alkoxy of one to 3 carbon atoms, inclusive, and s is zero, one, 2, or 3, the various T's being the same or different, with the proviso that not more than two T's are other than alkyl, with the further proviso that R 7 is ##STR31## wherein T and s are as defined above, only when R 3 and R 4 are hydrogen or methyl, being the same or different; and
5. a prostaglandin analog of the formula ##STR32## wherein L 1 , M 1 , R 1 , R 7 , Y 1 , and Z 1 are as defined above; with the proviso that Z 1 is cis--CH=CH--CH 2 --(CH 2 ) g --CH 2 -- or --(CH 2 ) 3 --(CH 2 ) g --CH 2 --, only when R 7 is ##STR33## where T and s are as defined above.
Within the scope of the novel prostaglandin analogs of this invention, there are represented above:
a. PGE-type compounds when the cyclopentane moiety is: ##STR34##
b. PGF.sub.α-type compounds when the cyclopentane moiety is: ##STR35##
c. PGF.sub.β- type compounds when the cyclopentane moiety is: ##STR36##
d. PGA-type compounds when the cyclopentane moiety is: ##STR37##
e. PGB-type compounds when the cyclopentane moiety is: ##STR38##
f. 11-deoxy-PGE-type compounds when the cyclopentane moiety is: ##STR39##
g. 11-deoxy-PGF.sub.α-type compounds when the cyclopentane moiety is: ##STR40##
h. 11-deoxy-PGF.sub.β-type compounds when the cyclopentane moiety is: ##STR41##
i. 8β,12α -PGE-type compounds when the cyclopentane moiety is: ##STR42##
j. 8β,12α-PGF.sub.α-type compounds when the cyclopentane moiety is: ##STR43##
k. 8β,12α-PGF.sub.β-type compounds when the cyclopentane moiety is: ##STR44##
l. 8β,12α-PGA-type compounds when the cyclopentane moiety is: ##STR45##
m. 8β,12α-11-deoxy-PGF.sub.β-type compounds when the cyclopentane moiety is: ##STR46##
n. 8β,12α-11-deoxy-PGE-type compounds when the cyclopentane moiety is: ##STR47## and
o. 8β,12α-11-deoxy-PGF.sub.β-type compounds when the cyclopentane moiety is: ##STR48##
Those prostaglandin analogs herein wherein Z 1 is cis--CH=CH--CH 2 --(CH 2 ) g --CH 2 -- or cis--CH=CH--CH 2 --(CH 2 ) g --CF 2 -- are named "PG 2 " compounds. The latter compounds are further characterized as "2,2-difluoro" PG-type compounds. When g is 2 or 3, the prostaglandin analogs so described are "2a-homo" or "2a,2b-dihomo" compounds, since in this event the carboxy terminated side chain contains 8 or 9 carbon atoms, respectively, in place of the 7 carbon atoms contained in PGE 1 . These additional carbon atoms are considered as though they were inserted between the C-2 and C-3 positions. Accordingly, these additional carbon atoms are referred to as C-2a and C-2g, counting from the C-2 to the C-3 position.
Further when Z 1 is --(CH 2 ) 3 --(CH 2 ) g --CH 2 -- or --(CH 2 ) 3 --(CH 2 ) g --CF 2 , wherein g is as defined above, the compounds so described are "PG 1 " compounds. When g is 2 or 3, the "2a-homo" and "2a,2b-dihomo" compounds are described as is discussed in the preceding paragraph.
When Z 1 is --CH 2 --O--CH 2 --(CH 2 ) g --CH 2 -- the compounds so described are named as "5-oxa-PG 1 " compounds. When g is 2 or 3, the compounds so described are "2a-homo" or "2a,2b-dihomo" compounds, respectively, as discussed above.
When Z 1 is --(CH 2 ) 2 --O--(CH 2 ) g --CH 2 --, wherein g is as defined above, the compounds so described are named as "4-oxa-PG 1 " compounds. When g is 2 or 3, the compounds so described are additionally characterized as "2a-homo" or "2a,2b-dihomo" compounds, respectively, as is discussed above.
When Z 1 is --(CH 2 ) 3 --O--(CH 2 ) g --, wherein g is as defined above, the compounds so described are named as "3-oxa-PG 1 " compounds. When g is 2 or 3, the compounds so described are further characterized as "2a-homo" or "2a,2b-dihomo" compounds, respectively, as is discussed above.
When Z 1 is cis--CH 2 --CH=CH--(CH 2 ) g --CH 2 --, wherein g is as defined above, the compounds so described are named "cis-4,5-didehydro-PG 1 " compounds. When g is 2 or 3, the compounds so described are further characterized as "2a-homo" or "2a,2b-dihomo" compounds, respectively, as discussed above.
For the novel compounds of this invention wherein Z 1 is ##STR49## there are described, respectively, 3-oxa-3,7-inter-m-phenylene-4,5,6-trinor- or 3,7-inter-m-phenylene-4,5,6-trinor-PG-type compounds, when g is 1. When g is 2 or 3, the above compounds are additionally described as "2a-homo" or "2a,2b-dihomo" PG-type compounds, respectively.
The novel prostaglandin analogs of this invention contain a --C.tbd.C-- moiety at the C-13 to C-14 position, and are accordingly, referred to as "13,14-didehydro" compounds.
When R 7 is --(CH 2 ) m --CH 3 , wherein m is as defined above, the compounds so described are named as "19,20-dinor", "20-nor", "20-methyl", or "20-ethyl" compounds when m is one, 2, 4, or 5, respectively. ##STR50## wherein T and s are as defined above, the compounds so described are named as "17-phenyl-18,19,20-trinor" compounds, when s is 0. When s is one, 2, or 3, the corresponding compounds are named as "17-(substituted phenyl)-18,19,20-trinor" compounds.
When R 7 is ##STR51## wherein T and s are as defined above, and neither R 3 nor R 4 is methyl, the compounds so described are named as "16-phenoxy-17,18,19,20-tetranor" compounds, when s is zero. When s is one, 2, or 3, the corresponding compounds are named as "16-(substituted phenoxy)-17,18,19,20-tetranor" compounds. When one and only one of R 3 and R 4 is methyl or both R 3 and R 4 are methyl, then the corresponding compounds wherein R 7 is as defined in this paragraph are named as "16-phenoxy or 16-(substituted phenoxy)-18,19,20-trinor" compounds or "16-methyl-16-phenoxy- or 16-(substituted phenoxy)-18,19,20-trinor" compounds, respectively.
When R 7 is cis--CH=CH--CH 2 --CH 3 , the compounds so described are "PG 3 " or "17,18-didehydro-PG 1 " compounds depending on whether Z 1 is cis--CH=CH--(CH 2 ) g --C(R 2 ) 2 , wherein R 2 is hydrogen or fluoro; or another moiety, respectively.
When at least one of R 3 and R 4 is not hydrogen then (except for the 16-phenoxy compounds discussed above) there are described the "16-methyl" (one and only one of R 3 and R 4 is methyl), "16,16-dimethyl" (R 3 and R 4 are both methyl), "16-fluoro" (one and only one of R 3 and R 4 is fluoro), "16,16-difluoro" (R 3 and R 4 are both fluoro) compounds. For those compounds wherein R 3 and R 4 are different, the prostaglandin analogs so represented contain an asymmetric carbon atom at C-16. Accordingly, two epimeric configurations are possible: "(16S)" and "(16R)". Further, there is described by this invention the C-16 epimeric mixture: "(16RS)".
When R 5 is methyl, the compounds so described are named as "15-methyl" compounds. When R 6 is methyl, the compounds so described are named as "15-methyl ether" compounds.
There is further provided by this invention both epimeric configurations of the hydroxy or methoxy at C-15. As discussed herein, PGE 1 , as obtained from mammalian tissues, has the "S" configuration at C-15. Further, as drawn herein PGF 1 , as obtained from mammalian tissues, has the 15-hydroxy moiety in the "alpha" configuration.
For the 13,14-didehydro derivative of PGE 1 as obtained from mammalian tissues, the S configuration at C-15 represents the α-hydroxy configuration, using the convention by which the side chains of the novel prostaglandin analogs of this invention are drawn herein, as indicated above. Further, (15R)-PGE 1 , by the convention used for drawing the prostaglandins herein, has the 15-hydroxy substituent in the beta configuration. The corresponding (15R)-13,14-didehydro-PGE 1 compound, drawn using the convention herein for the representation of the novel prostaglandin analogs of this invention, likewise has the 15-hydroxy in the beta configuration. Thus, the novel prostaglandin analogs of this invention wherein the 15-hydroxy or 15-methoxy moiety has the same absolute configuration as (15R)-13,14-didehydro-PGE 1 at C-15 will be named "15-epi" compounds. When the designation "15-epi" is absent, those compounds wherein the configuration of the 15-hydroxy or 15-methoxy is the same as the absolute configuration of 15(S)-13,14-didehydro-PGE 1 are represented, i.e. the 15α-hydroxy configuration.
Accordingly, as indicated by the preceeding paragraphs, the novel PG analogs disclosed herein are named according to the system described in Nelson, N.A., J. Med. Chem. 17, 911 (1974).
Examples of alkyl of one to 12 carbon atoms, inclusive, are methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl, undecyl, dodecyl, and isomeric forms thereof.
Examples of cycloalkyl of 3 to 10 carbon atoms, inclusive, which includes alkyl-substituted cycloalkyl, are cyclopropyl, 2-methylcyclopropyl, 2,2-dimethylcyclopropyl, 2,3-diethylcyclopropyl, 2-butylcyclopropyl, cyclobutyl, 2-methylcyclobutyl, 3-propylcyclobutyl, 2,3,4-triethylcyclobutyl, cyclopentyl, 2,2-dimethylcyclopentyl, 2-pentylcyclopentyl, 3-tert-butylcyclopentyl, cyclohexyl, 4-tert-butylcyclohexyl, 3-isopropylcyclohexyl, 2,2-dimethylcyclohexyl, cycloheptyl, cyclooctyl, cyclononyl, and cyclodecyl.
Examples of aralkyl of 7 to 12 carbon atoms, inclusive, are benzyl, 2-phenethyl, 1-phenylethyl, 2-phenylpropyl, 4-phenylbutyl, 3-phenylbutyl, 2-(1-naphthylethyl), and 1-(2-naphthylmethyl).
Examples of phenyl substituted by one to 3 chloro or alkyl of one to 4 carbon atoms, inclusive, are p-chlorophenyl, m-chlorophenyl, 2,4-dichlorophenyl, 2,4,6-trichlorophenyl, p-tolyl, m-tolyl, o-tolyl, p-ethylphenyl, p-tert-butylphenyl, 2,5-dimethylphenyl, 4-chloro-2-methylphenyl, and 2,4-dichloro-3-methylphenyl.
Examples of ##STR52## wherein T is alkyl of one to 3 carbon atoms, inclusive, fluoro, chloro, trifluoromethyl, or alkoxy of one to 3 carbon atoms, inclusive; and s is zero, one, 2, or 3, with the proviso that not more than two T's are other than alkyl, are phenyl, (o-, m-, or p-)tolyl, (o-, m-, or p-)ethylphenyl, 2-ethyl-p-tolyl, 4-ethyl-o-tolyl, 5-ethyl-m-tolyl, (o-, m-, or p-)propylphenyl, 2-propyl-(o-, m-, or p-)tolyl, 4-isopropyl-2,6-xylyl, 3-propyl-4-ethylphenyl, (2,3,4-, 2,3,5-, 2,3,6-, or 2,4,5-)trimethylphenyl, (o-, m-, or p-)fluorophenyl, 2-fluoro-(o-, m-, or p-)tolyl, 4-fluoro-2,5-xylyl, (2,4-, 2,5-, 2,6-, 3,4-, or 3,5-)difluorophenyl, (o-, m-, p-)-chlorophenyl, 2-chloro-p-tolyl, (3-, 4-, 5-, or 6-)chloro-o-tolyl, 4-chloro-2-propylphenyl, 2-isopropyl-4-chlorophenyl, 4-chloro-3,5-xylyl, (2,3- 2,4-, 2,5- 2,6-, 3,4-, or 3,5-)dichlorophenyl, 4-chloro-3-fluorophenyl, (3 - or 4-)chloro-2-fluorophenyl, o-, m-, or p-trifluoromethylphenyl, (o-, m-, or p-)methoxyphenyl, (o-, m-, or p-)ethoxyphenyl, (4- or 5-)chloro-2-methoxyphenyl, and 2,4-dichloro(5- or 6-)methylphenyl.
The novel prostaglandin analogs of this invention correspond to the prostaglandins described above, in that the novel prostaglandin analogs exhibit prostaglandin-like activity.
Specifically, the 8β,12α-PGE-, 11-deoxy-8β,12α-PGE-, PGE-, and 11-deoxy-PGE-type compounds of this invention correspond to the PGE compounds described above, in that these novel PGE- and 11-deoxy-PGE-type compounds are useful for each of the above-described purposes for which the PGE compounds are used, and are used in the same manner as the PGE compounds, as described above.
The 8β,12α-PGF.sub.α-, 11-deoxy-8β,12α-PGF.sub.α-, PGF.sub.α- and 11-deoxy-PGF.sub.α-type compounds of this invention correspond to the PGF.sub.α compounds described above, in that these novel PGF.sub.α- and 11-deoxy-PGF.sub.α-type compounds are useful for each of the above-described purposes for which the PGF.sub.α compounds are used, and are used in the same manner as the PGF.sub.α compounds, as described above.
The 8β,12α-PGF.sub.β-, 11-deoxy-8β,12α-PGF.sub.β-, PGF.sub.β- and 11-deoxy-PGF.sub.β- type compounds of this invention correspond to the PGF.sub.β compounds described above, in that these novel PGF.sub.β- and 11-deoxy-PGF.sub.β-type compounds are useful for each of the above-described purposes for which the PGF.sub.β compounds are used, and are used in the same manner as the PGF.sub.β compounds, as described above.
The 8β,12α-PGA- and PGA-type compounds of this invention correspond to the PGA compounds described above, in that these novel PGA-type compounds are useful for each of the above described purposes for which the PGA compounds are used, and are used in the same manner as the PGA compounds, as described above.
The PGB-type compounds of this invention correspond to the PGB compounds described above, in that these PGB-type compounds are useful for each of the above described purposes for which the PGB compounds are used, and are used in the same manner as the PGB compounds, as described above.
The prostaglandins described above, are all potent in causing multiple biological responses evan at low doses. Moreover, for many applications, these prostaglandins have an inconveniently short duration of biological activity. In striking contrast, the novel prostaglandin analogs of this invention are substantially more selective with regard to potency in causing prostaglandin-like biological respones, and have a substantially longer duration of biological activity. Accordingly, each of these novel prostaglandin analogs is surprisingly and unexpectedly more useful than one of the corresponding prostaglandins described above for at least one of the pharmacological purposes indicated above for the latter, because it has a different and narrower spectrum of biological potency than the known prostaglandin, and therefore is more specific in its activity and causes smaller and fewer undesired side effects than when the prostaglandin is used for the same purpose. Moreover, because of its prolonged activity, fewer and smaller doses of the novel prostaglandin analog are frequently effective in attaining the desired result.
Another advantage of the novel prostaglandin analogs of this invention, especially the preferred PG analogs defined hereinbelow, compared with the corresponding prostaglandins, is that these novel PG analogs are administered effectively orally, sublingually, intravaginally, buccally, or rectally in those cases wherein the corresponding prostaglandin is effective only by the intravenous, intramuscular, or subcutaneous injection or infusion methods of administration indicated above as uses of these prostaglandins. These alternate routes of administration are advantageous because they facilitate maintaining uniform levels of these compounds in the body with fewer, shorter, or smaller doses, and make possible self-administration by the patient.
Accordingly, the novel prostaglandin analogs of this invention are administered in various ways for various purposes: e.g., intravenously, intramuscularly, subcutaneously, orally, intravaginally, rectally, buccally, sublingually, topically, and in the form of sterile implants for prolonged action. For intravenous injection or infusion, sterile aqueous isotonic solutions are preferred. For intravenous injection or infusion, sterile aqueous isotonic solutions are preferred. For that purpose, it is preferred because of increased water solubility that R 1 in the novel compounds of this invention be hydrogen or a pharmacologically acceptable cation. For subcutaneous or intramuscular injection, sterile solutions or suspensions of the acid, salt, or ester form in aqueous or non-aqueous media are used. Tablets, capsules, and liquid preparations such as syrups, elixirs, and simple solutions, with the usual pharmaceutical carriers are used for oral sublingual administration. For rectal or vaginal administration, suppositories prepared as known in the art are used. For tissue implants, a sterile tablet or silicone rubber capsule or other object containing or impregnated with the substance is used.
The chemical structure of the novel 11-deoxy-PGE-type compounds of this invention renders them less sensitive to dehydration and rearrangement than the corresponding prostaglandins, and these compounds accordingly exhibit a surprising and unexpected stability and duration of shelf life.
The novel PG analogs of this invention are used for the purposes described above in the free acid form, in ester form, in pharmacologically acceptable salt form. When the ester form is used, the ester is any of those within the above definition of R 1 . However, it is preferred that the ester be alkyl of one to 12 carbon atoms, inclusive. Of the alkyl esters, methyl and ethyl are especially preferred for optimum absorption of the compound by the body or experimental animal system; and straight-chain octyl, nonyl, decyl, undecyl, and dodecyl are especially preferred for prolonged activity in the body or experimental animal.
Pharmacologically acceptable salts of the novel prostaglandin analogs of this invention compounds useful for the purposes described above are those with pharmacologically acceptable metal cations, ammonium, amine cations, or quaternary ammonium cations.
Especially preferred metal cations are those derived from the alkali metals, e.g., lithium, sodium, and potassium, and from the alkaline earth metals, e.g., magnesium and calcium, although cationic forms of other metals, e.g., aluminum, zinc, and iron are within the scope of this invention.
Pharmacologically acceptable amine cations are those derived from primary, secondary, or tertiary amines. Examples of suitable amines are methylamine, dimethylamine, trimethylamine, ethylamine, dibutylamine, triisopropylamine, N-methylhexylamine, decylamine, dodecylamine, allylamine, crotylamine, cyclopentylamine, dicyclohexylamine, benzylamine, dibenzylamine, α-phenylethylamine, β-phenylethylamine, ethylenediamine, diethylenetriamine, and the like aliphatic, cycloaliphatic, araaliphatic amines containing up to and including about 18 carbon atoms, as well as heterocyclic amines, e.g., piperidine, morpholine, pyrrolidine, piperazine, and lower-alkyl derivatives thereof, e.g., 1-methylpiperidine, 4-ethylmorpholine, 1-isopropylpyrrolidine, 2-methylpyrrolidine, 1,4-dimethylpiperazine, 2-methylpiperidine, and the like, as well as amines containing water-solubilizing or hydrophilic groups, e.g., mono-, di-, and triethanolamine, ethyldiethanolamine, N-butylethanolamine, 2-amino-1-butanol, 2-amino-2-ethyl-1,3-butylethanolamine, 2-amino-1-butanol, 2-amino-2-ethyl-1,3-propanediol, 2-amino-2-methyl-1-propanol, tris(hydroxymethyl)aminomethane, N-phenylethanolamine, N-(p-tert-amylphenyl)-diethanolamine, galactamine, N-methylgycamine, N-methylglucosamine, ephedrine, phenylephrine, epinephrine, procaine, and the like. Further useful amine salts are the basic amino acid salts, e.g., lysine and arginine.
Examples of suitable pharmacologically acceptable quaternary ammonium cations are tetramethylammonium, tetraethylammonium, benzyltrimethylammonium, phenyltriethylammonium, and the like.
The novel PG analogs of this invention are used for the purposes described above in free hydroxy form or also in the form wherein the hydroxy moieties are transformed to lower alkanoate moieties such as acetoxy, propionyloxy, butyryloxy, valeryloxy, hexanoyloxy, heptanoyloxy, octanoyloxy, and branched chain alkanoyloxy isomers of those moieties. Especially preferred among these alkanoates for the above described purposes are the acetoxy compounds. These free hydroxy and alkanoyloxy compounds are used as free acids, as esters, and in salt form all as described above.
To obtain the optimum combination of biological response specificity, potency, and duration of activity, certain compounds within the scope of this invention are preferred.
It is preferred that the carboxy-terminated side chain contain either 7 or 9 carbon (or carbon and oxygen) atoms, especially preferred that it contain 7, i.e., the natural chain length of the prostaglandins. Further when the other side chain contains --(CH 2 ) m --CH 3 , it is preferred that m be 3. For those compounds wherein R 7 is ##STR53## it is preferred that s be zero or one and T be chloro, fluoro, or trifluoromethyl.
For those compounds wherein at least one of R 3 and R 4 is methyl or fluoro, it is preferred that R 5 and R 6 both be hydrogen. For those compounds wherein at least one of R 5 and R 6 is methyl, it is preferred that R 3 and R 4 both be hydrogen. For those compounds wherein R 7 is ##STR54## it is preferred that R 3 , R 4 , R 5 , and R 6 all be hydrogen.
For those compounds wherein an oxa is substituted for a methylene (i.e., --O-- for --CH 2 --), it is preferred that such substitution occur at C-5.
It is further preferred that the 15-hydroxy or 15-methoxy not be of the 15-epi configuration, i.e., that the hydroxy be in the alpha configuration when the formulas of the novel 13,14-didehydro-PG analogs are as drawn herein.
Especially preferred are those compounds which satisfy two or more of the above preferences. Further, the above preferences are expressly intended to describe the preferred compounds within the scope of any generic formula of novel prostaglandin analogs disclosed herein. Thus, for example the above preferences describe preferred compounds within the scope of each formula of a prostaglandin analog provided in the Tables hereinafter.
In another aspect of the interpretation of the preferences herein, the various prostaglandin cyclopentane ring structures as employed herein are each representative of a particular "parent structure" which is useful in naming and catagorizing the novel prostaglandin analogs disclosed herein. Further, where a formula depicts a genera of PG analogs disclosed herein evidencing a single cyclopentane ring structure, then each corresponding genus of PG analogs evidencing one of the remaining cyclopentane ring structures cited herein for novel prostaglandin analogs is intended to represent an equally preferred genus of compounds. Thus, for example, for each genus of PGF.sub.α-type products depicted by a formula herein, the corresponding genus of PGF.sub.β-, PGE-, and 11-deoxy-PGF.sub.α-type products are equally preferred embodiments of the invention as the genera of PGF.sub.α-type products.
Finally where subgeneric grouping of PG analogs of any cyclopentane ring structure are described herein, then the corresponding subgeneric groupings of PG analogs of each of the remaining cyclopentane ring structures are intended to represent equally preferred embodiments of the present invention.
The Charts herein describe methods whereby the novel prostaglandin analogs of this invention are prepared.
With respect to the Charts R 1 , Y 1 , R 7 , M 1 , L 1 , Z 1 , and g are as defined above; D is as variously defined above M 5 is ##STR55## when R 6 is hydrogen, wherein R 39 is hydrogen or methyl, being the same as R 5 .
R 2 is hydrogen or fluoro. R 8 is hydrogen or hydroxy. R 16 is hydrogen or --OR 9 , wherein R 9 is an acyl protecting group as defined below. R 18 is hydrogen or --OR 10 , wherein R 10 is as defined above. R 22 is methyl or ethyl. R 26 is hydrocarbyl, including alkyl, aralkyl, cycloalkyl, and the like. Examples of these hydrocarbyl groups include 2-methylbutyl, isopentyl, heptyl, octyl, nonyl, tridecyl, octadecyl, benzyl, phenethyl, p-methylphenethyl, 1-methyl-3-phenylpropyl, cyclohexyl, phenyl, and p-methylphenyl.
G 1 is alkyl of one to 4 carbon atoms, cycloalkyl of 3 to 10 carbon atoms, inclusive, aralkyl of 7 to 12 carbon atoms, phenyl, or phenyl substituted with one or 2 fluoro, chloro, or alkyl of one to 4 carbon atoms, with the proviso that in the --Si--(G 1 ) 3 moiety the various G 1 's are the same or different. R 38 is hydrogen or --O--Si--(G 1 ) 3 , wherein G 1 is as defined above.
R 9 is an acyl protecting group. Acyl protecting groups according to R 9 , include:
a. Benzoyl;
b. Benzoyl substituted with one to 5, inclusive, alkyl of one to 4 carbon atoms, inclusive, phenylalkyl of 7 to 12 carbon atoms, inclusive, or nitro, with the proviso that not more than 2 substituents are other than alkyl, and that the total number of carbon atoms in the substituents does not exceed 10 carbon atoms, with the further proviso that the substituents are the same or different;
c. Benzoyl substituted with alkoxycarbonyl of 2 to 5 carbon atoms, inclusive;
d. Naphthoyl;
Naphthoyl substituted with one to 9, inclusive, alkyl of one to 4 carbon atoms, inclusive, phenylalkyl of 7 to 10 carbon atoms, inclusive, or nitro, with the proviso that not more than 2 substituents on either of the fused aromatic rings are other than alkyl and that the total number of carbon atoms in the substituents on either of the fused aromatic rings does not exceed 10 carbon atoms, with the further proviso that the various substituents are the same or different; or
f. Alkanoyl of 2 to 12 carbon atoms, inclusive.
In preparing these acyl derivatives of a hydroxy-containing compound herein, methods generally known in the art are employed. Thus, for example, an aromatic acid of the formula R 9 OH, wherein R 9 is as defined above (e.g., benzoic acid), is reacted with the hydroxy-containing compound in the presence of a dehydrating agent, e.g. sulfuric acid, zinc chloride, or phosphoryl chloride; or alternatively an anhydride of the aromatic acid of the formula (R 9 ) 2 O (e.g., benzoic anhydride) is used.
Preferably, however, the process described in the above paragraph proceeds by use of the appropriate acyl halide, e.g., R 9 Hal, wherein Hal is chloro, bromo, or iodo. For example, benzoyl chloride is reacted with the hydroxy-containing compound in the presence of a hydrogen chloride scavenger, e.g. a tertiary amine such as pyridine, triethylamine or the like. The reaction is carried out under a variety of conditions, using procedures generally known in the art. Generally mild conditions are employed: 20-60° C., contacting the reactants in a liquid medium (e.g., excess pyridine or an inert solvent such as benzene. toluene, or chloroform). The acylating agent is used either in stoichiometric amount or in substantial stoichiometric excess.
As examples of R 9 , the following compounds are available as acids (R 9 OH), anhydrides ((R 9 ) 2 O), or acyl chlorides (R 9 Cl): benzoyl; substituted benzoyl, e.g., 2-, 3-, or 4-)-methylbenzoyl, (2-, 3-, or 4-)-ethyl benzoyl, (2-, 3-, or 4-)-isopropylbenzoyl, (2-, 3-, or 4-)-tert-butylbenzoyl, 2,4-dimethylbenzoyl, 3,5-dimethylbenzoyl, 2-isopropyltoluyl, 2,4,6-trimethylbenzoyl, pentamethylbenzoyl, alphaphenyl-(2-, 3-, or 4-)-toluyl, (2-, 3-, or 4-)-phenethylbenzoyl, (2-, 3-, or 4-)-nitrobenzoyl, (2,4-, 2,5-, or 2,3-)-dinitrobenzoyl, 2,3-dimethyl-2-nitrobenzoyl, 4,5-dimethyl-2-nitrobenzoyl, 2-nitro-6-phenethylbenzoyl, 3-nitro-2-phenethylbenzoyl, 2-nitro-6-n-phenethylbenzoyl, 3-nitro-2-phenethylbenzoyl; mono esterified phthaloyl, isophthaloyl, or terephthaloyl; 1- or 2-naphthoyl; substituted naphthoyl, e.g., (2-, 3-, 4-, 5-, 6-, or 7-)-methyl-1-naphthoyl, (2- or 4-)ethyl-1-naphthoyl, 2-isopropyl-1-naphthoyl, 4,5-dimethyl-1-naphthoyl, 6-isopropyl-4-methyl-1-naphthoyl, 8-benzyl-1-naphthoyl, (3-, 4-, 5-, or 8-)-nitro-1-naphthoyl, 4,5-dinitro-1-naphthoyl, (3-, 4-, 6-, 7-, or 8-)methyl-1-naphthoyl, 4-ethyl-2-naphthoyl, and (5- or 8-)nitro-2naphthoyl; and acetyl.
There may be employed, therefore, benzoyl chloride, 4-nitrobenzoyl chloride, 3,5-dinitrobenzoyl chloride, or the like, i.e. R 9 Cl compounds corresponding to the above R 9 groups. If the acyl chloride is not available, it is prepared from the corresponding acid and phosphorus pentachloride as is known in the art. It is preferred that the R 9 OH, (R 9 ) 2 O, or R 9 Cl reactant does not have bulky hindering substituents, e.g. tert-butyl on both of the ring carbon atoms adjacent to the carbonyl attaching cite.
The acyl protecting groups, according to R 9 , are removed by deacylation. Alkali metal carbonates are employed effectively at ambient temperature for this purpose. For example, potassium carbonate in methanol at about 25° C. is advantageously employed.
Those blocking groups within the scope of R 10 are any group which replaces a hydroxy hydrogen and is neither attacked nor as reactive to the reagents used in the transformations used herein as an hydroxy is and which is subsequently replaceable with hydrogen in the preparation of the prostaglandin-type compounds. Several blocking groups are known in the art, e.g. tetrahydropyranyl and substituted tetrahydropyranyl. See for reference E. J. Corey, Proceedings of the Robert A. Welch Foundation Conferences on Chemical Research, 12, Organic Synthesis, pgs. 51-79 (1969). Those blocking groups which have been found useful include
a. tetrahydropyranyl;
b. tetrahydrofuranyl; and
c. a group of the formula
--C(OR.sub.11)(R.sub.12)--CH(R.sub.13)(R.sub.14),
wherein R 11 is alkyl of one to 18 carbon atoms, inclusive, cycloalkyl of 3 to 10 carbon atoms, inclusive, aralkyl of 7 to 12 carbon atoms, inclusive, phenyl or phenyl substituted with one to 3 alkyl of one to 4 carbon atoms, inclusive, wherein R 12 and R 13 are alkyl of one to 4 carbon atoms, inclusive, phenyl, phenyl substituted with one, 2, or 3 alkyl of one to 4 carbon atoms, inclusive, or when R 12 and R 13 are taken together --(CH 2 ) a --or --(CH 2 ) b --O--(CH 2 ) c , wherein a is 3, 4, or 5, or b is one, 2, or 3, and c is one, 2, or 3, with the proviso that b plus c is 2, 3, or 4, with the further proviso that R 12 and R 13 may be the same or different, and wherein R 14 is hydrogen or phenyl.
When the blocking group R 10 is tetrahydropyranyl, the tetrahydropyranyl ether derivative of any hydroxy moieties of the PG-type intermediates herein is obtained by reaction of the hydroxy-containing compound with 2,3-dihydropyran in an inert solvent, e.g. dichloromethane, in the presence of an acid condensing agent such as p-toluenesulfonic acid or pyridine hydrochloride. The dihydropyran is used in large stoichiometric excess, preferably 4 to 10 times the stoichiometric amount. The reaction is normally complete in less than an hour at 20° to 50° C.
When the blocking group is tetrahydrofuranyl, 2,3-dihydrofuran is used, as described in the preceding paragraph, in place of the 2,3-dihydropyran.
When the blocking group is of the formula
--C(OR.sub.11)(R.sub.12)--CH(R.sub.13)(R.sub.14),
wherein R 11 , R 12 , R 13 , and R 14 are as defined above, the appropriate reagent is a vinyl ether, e.g. isobutyl vinyl ether or any vinyl ether of the formula
C(OR.sub.11)(R.sub.12)=C(R.sub.13)(R.sub.14),
wherein R 11 , R 12 , R 13 , and R 14 are as defined above; or an unsaturated cyclic or heterocyclic compound, e.g. 1-cyclohexen-1-yl methyl ether, or 5,6-dihydro-4-methoxy-2H-pyran. See C. B. Reese, et al., Journal of the Chemical Society 89, 3366 (1967). The reaction conditions for such vinyl ethers and unsaturated compounds are similar to those for dihydropyran above.
The blocking groups according to R 10 are removed by mild acidic hydrolysis. For example, by reaction with (1) hydrochloric acid in methanol; (2) a mixture of acetic acid, water, and tetrahydrofuran; or (3) aqueous citric acid or aqueous phosphoric acid in tetrahydrofuran, at temperatures below 55° C., hydrolysis of the blocking groups is achieved.
R 53 is hydrogen or alkyl of one to 4 carbon atoms, inclusive. R 55 and R 56 are alkyl of one to 4 carbon atoms, inclusive, being the same or different, or when taken together represent a group of the formula: ##STR56## wherein R 57 , R 58 , R 59 , R 60 , R 61 , and R 62 are hydrogen, alkyl of one to 4 carbon atoms, inclusive, or phenyl, being the same or different, with the proviso that not more than one of R 57 , R 58 , R 59 , R 60 , R 61 , and R 62 is phenyl and that the total number of carbon atoms in R 57 , R 58 , R 59 , R 60 , R 61 , and R 62 is from 2 to 10, inclusive, and h is zero or one.
R 63 is carboxyacyl of the formula ##STR57## wherein R 64 is hydrogen, alkyl of one to 19 carbon atoms, inclusive, or aralkyl of 7 to 12 carbon atoms, inclusive, wherein the above alkyl or aralkyl are substituted with zero to 3 fluoro, chloro, bromo, or iodo. R 66 is hydrogen or a blocking group, according to R 65 . Blocking groups according to R 65 useful for the purposes of this invention include all blocking groups according to R 10 , as enumerated herein, and additionally --Si(G 1 ) 3 , wherein G 1 is alkyl of one to 4 carbon atoms, inclusive, cycloalkyl of 3 to 10 carbon atoms, inclusive, aralkyl of 7 to 12 carbon atoms, inclusive, phenyl, or phenyl substituted with one or 2 fluoro, chloro, or alkyl of one to 4 carbon atoms, inclusive. In the use of these silyl blocking groups, according to R 65 , methods known in the art for the preparation of the necessary reagents and appropriate reaction conditions for replacing hydroxy hydrogens with these silyl blocking groups and subsequently hydrolyzing these silyl blocking groups, are employed.
R 68 is hydrogen, carboxyacyl according to R 63 , or an acyl protecting group according to R 9 . R 69 is hydrogen or alkyl of one to 4 carbon atoms, inclusive, R 70 is hydrogen, alkyl of one to 4 carbon atoms, inclusive, or silyl of the formula --Si(G 1 ) 3 , wherein G 1 is as defined above. R 66 is hydrogen or optionally R 65 , a blocking group.
Y 2 is trans-CH=C(Hal)-, wherein Hal is chloro, bromo, or iodo. Y 3 is trans-CH=CH, Z 2 is cis--CH=CH--CH 2 --(CH 2 ) g --C(R 2 ) 2 --, cis-CH 2 --CH=CH--(CH 2 ) g --CH 2 , --(CH 2 ) 3 --(CH 2 ) g --C(R 2 ) 2 --, --CH 2 --O--CH 2 --(CH 2 ) g --CH 2 --, --(CH 2 ) 2 --O--(CH 2 ) g --CH 2 --, or --(CH 2 ) 3 --O--(CH 2 ) g --, wherein R 2 and g are as defined above. Z 3 is oxa or methylene, e.g., --O-- or --CH 2 --, respectively.
With respect to Chart A the formula XXI compound is known in the art. This compound is available in either of two enantiomeric forms or as a mixture thereof. The formula XXI compound in racemic form may be transformed into corresponding optically active compound by methods known in the art.
The formula XXII compound is prepared from the formula XXI compound by a Wittig alkylation when R 7 is not 1-buten-yl. Reagents known in the art or prepared by methods known in the art are employed. The transenone lactone is obtained stereospecifically. See for reference D. H. Wadsworth, et al., Journal of Organic Chemistry 30, 680 (1965).
In the preparation of the formula XXII compound, certain phosphonates are employed in the Wittig reaction. These phosphonates are of the general formula ##STR58## wherein L 1 and R 7 are as defined above (but R 7 is not 1-butenyl) and R 15 is alkyl of one to 8 carbon atoms, inclusive.
Phosphonates of the above general formula are prepared by methods known in the art. See Wadsworth, et al. as cited above.
Conveniently the appropriate aliphatic acid ester is condensed with the anion of dimethyl methylphosphonate as produced using n-butyllithium. For this purpose, acids of the general formula ##STR59## are employed in the form of their lower alkyl esters, preferably methyl or ethyl. The methyl esters for example are readily obtained by reaction of the corresponding acids with diazomethane.
For example, when R 7 is ##STR60## wherein T and s are as defined above, and R 3 and R 4 of the L 1 moiety are both hydrogen, the corresponding phenoxy or substituted phenoxy acetic acids are known in the art or readily available in the art. Those known in the art include those wherein the R 7 moiety is: phenoxy,(o-, m-, or p-)tolyloxy-, (o-, m-, or p-)ethylphenoxy-, 4-ethyl-o-tolyloxy-, (o-, m-, or p-)propylphenoxy-, (o-, m-, or p-)-t-butylphenoxy-, (o-, m-, or p-)fluorophenoxy)-, 4-fluoro-2,5-xylyloxy-, (o-, m-, or p-)chlorophenoxy-, (2,3-, 2,4-, 2,5-, 2,6-, 3,4-, or 3,5-)dichlorophenoxy-, (o-, m-, or p-)trifluoromethylphenoxy-, or (o-, m-, or p-)methoxyphenoxy-.
Further, many 2-phenoxy- or substituted phenoxy propionic acids are readily available, and are accordingly useful for the preparation of the acids of the above formula wherein one and only one of R 3 and R 4 of the L 1 moiety is methyl and R 7 is phenoxy or substituted phenoxy. These 2-phenoxy or 2-substituted phenoxy propionic acids include those wherein the R 7 moiety is p-fluorophenoxy-, (o-, m-, or p-)chlorophenoxy-, (2,3-, 2,4-, 2,5-, 2,6-, 3,4-, or 3,5-)dichlorophenoxy-, (4- or 6-chloro-o-tolyloxy-, phenoxy-, (o-, m-, or p-)tolyloxy, 3,5-xylyloxy-, or m-trifluoromethylphenoxy-.
Finally there are available many 2-methyl- 2-phenoxy- or (2-substituted)phenoxypropionic acids, which are useful in the preparation of the above acids wherein R 3 and R 4 of the L 1 moiety are both methyl and R 7 is phenoxy or substituted phenoxy. These 2-methyl-2-phenoxy-, or (2-substituted)phenoxypropionic acids include those wherein R 7 is: phenoxy-, (o-, m-, or p-)chlorophenoxy-, (2,3-, 2,4-, 2,5-, 2,6-, 3,4-, or 3,5-)dichlorophenoxy-.
Other phenoxy substituted acids are readily available by methods known in the art, for example, by Williamson synthesis of ethers using an α-halo aliphatic acid or ester with sodium phenoxide or a substituted sodium phenoxide. Thus, the (T) s -substituted sodium phenoxide is reacted with, for example, the α-chloro aliphatic acid, or the alkyl ester derivative thereof, with heating to yield the acid of the above general formula, which is recovered from the reaction mixture by conventional purification techniques.
There are further available phenyl substituted acids of the above formula wherein R 7 is benzyl or substituted benzyl.
For example, when R 3 and R 4 of the L 1 moiety are both hydrogen there are available the following phenyl or substituted phenyl propionic acids: (o-, m-, or p-)-chlorophenyl-, p-fluorophenyl-, m-trifluoromethylphenyl-, (o-, m-, or p-)methylphenyl-, (o-, m-, or p-)methoxyphenyl-, (2,4-, 2,5-, or 3,4-)dichlorophenyl-, (2,3-, 2,4-, 2,5-, 2,6-, or 3,4-)dimethylphenyl-, or (2,3-, 2,4-, 2,5-, 2,6-, 3,4-, or 3,5-)dimethoxyphenyl-.
When one and only one of R 3 and R 4 of the L 1 moiety is methyl there are available, for example, the following 2-methyl-3-phenyl or substituted phenyl propionic acids: phenyl, o-chlorophenyl-, (o-, or p-)methylphenyl-, (o-, m-, or p-)methoxyphenyl-, (2,4- or 3,4-)difluorophenyl-, 2,3-dimethylphenyl-, and (2,3-, 3,4-, or 4,5-)dimethoxyphenyl-.
When both R 3 and R 4 are methyl there are available, for example, the following 2,2-dimethyl-3-phenyl or substituted phenyl propionic acids: phenyl- and p-methylphenyl.
When one and only one of R 3 and R 4 is fluoro, there is available, for example, 2-fluoro-3-phenyl propionic acid.
Phenyl substituted acids (as above wherein R 7 is benzyl) are available by methods known in the art, for example, by reacting a mixture of the appropriate methyl- or fluoro-substituted acetic acid, a secondary amine (e.g., diisopropylamine), n-butyllithium, and an organic diluent (e.g., tetrahydrofuran with the appropriately substituted benzyl chloride. Thus, the above acid is obtained by the following reaction: ##STR61## The above reaction proceeds smoothly, ordinarily at 0° C. The product acid is recovered using conventional methods.
For the acids of the above formula wherein R 7 is n-alkyl, many such acids are readily available.
For example, when R 3 and R 4 of the L 1 moiety are both hydrogen there are available butyric, pentanoic, hexanoic, heptanoic, and octanoic acids.
For example, when one and only one of R 3 and R 4 of the L 1 moiety is methyl, there are available the following 2-methyl alkanoic acids: butyric, pentanoic, hexanoic, heptanoic, and octanoic.
For example, when one of R 3 and R 4 of the L 1 moiety is fluoro there are available the following 2-fluoro alkanoic acids: butyric, pentanoic, hexanoic, heptanoic, and octanoic.
The acids of the above general formula wherein R 7 is alkyl and R 3 and R 4 of the L 1 moiety are fluoro are conveniently prepared from the corresponding 2-oxo-alkanoic acids, i.e. butyric, pentanoic, hexanoic, heptanoic, and octanoic. The transformation of these 2-oxo-alkanoic acids to the corresponding 2,2-difluoro alkanoic acids proceeds by methods known in the art, using known ketonic fluorinating reagents. For example, MoF 6 .BF 3 is advantageously employed in the fluorination.
When R 7 is 1-butenyl, the formula XXII compound is prepared from the formula XXI compound by transformation of the formula XXI 2β-carboxaldehyde to a corresponding 2β-(2-formyl-trans-1-ethenyl) compound followed by a Grignard reaction employing the reagent prepared from ##STR62## Thereupon the (3RS)-3-hydroxy compound corresponding to formula XXII is prepared, which is oxidized to the formula XXII compound with the Collins reagent. Accordingly, following the procedure of Japanese Application Number 0018-459, 3α-benzoyloxy-5α-hydroxy-2β-carboxaldehyde-1α-cyclopentaneacetic acid γ-lactone is transformed to benzoyl-oxy-5α-hydroxy-2β-(2-formyl-trans-1-ethenyl)-1α-cyclopentane acid γ-lactone. This product is then reacted with the Grignard reagent described above and oxidized as above.
The formula XXIII compound is prepared from the formula XXII compound by dihalogenation, followed by dehydrohalogenation. The halogenation proceeds by methods known in the art, conveniently by reaction of the formula XXII compound with a reagent such as N-halosuccinimide. The reaction proceeds slowly to completion, ordinarily within three to ten days. Alternatively the molecular form of the halide (Hal) 2 in a diluent (e.g., carbon tetrachloride or a mixture of acetic acid and sodium acetate) is employed in this dihalogenation. Thereafter dehydrohalogenation proceeds by addition of an organic base, preferably amine base, to the halide. For example pyridine, or a diazobicycloalkene, is an especially useful amine base, although non-amine bases such as methanolic sodium acetate are likewise employed.
Optionally the formula XXIII compound is prepared directly from the formula XXI compound using a Wittig reagent derived from a 1-halophosphonate corresponding to the phosphonate described above for the preparation of the formula XXII compound. These phosphonates are known in the art or are readily prepared by methods known in the art. For example, a phosphonate as described above is transformed to the corresponding 1-halophosphonate by dripping the molecular halogen into a solution of the phosphonate and a strong organic base, e.g. sodium methoxide. In any event, the 14-chloro intermediates are preferred formula XXIII products, in that they lead to PG intermediates which are more easily dehydrohalogenated at C-13 and C-14 according to the procedure of Chart R.
The 1-halophosphonate as prepared above is then reacted with the formula XXI compound in a manner described for the preparation of the formula XXII compound from the formula XXI compound to prepare the formula XXIII compound.
In each of the above described methods for the preparation of the formula XXIII compound the desired formula XXIII product is often contaminated with its corresponding cis isomer. In performing the below steps it is particularly desirable to obtain pure formula XXIII product in order to avoid creation of complicated mixtures of steroisomers. Accordingly, the formula XXIII compound is subjected to conventional separation techniques (e.g. silica gel chromatography) to obtain pure product.
The formula XXIV compound is prepared from the formula XXIII 3-oxo bicyclic lactone by transformation of the 3-oxo-moiety to the M 5 moiety.
The above 3-oxo bicyclic lactone is transformed to the corresponding 3α or 3β-hydroxy bicyclic lactone, wherein M 5 is ##STR63## by reduction of the 3-oxo moiety, followed by separation of the 3α- and 3β-hydroxy epimers. For this reduction the known ketonic carbonyl reducing agents which do not reduce ester or acid groups or carbon-carbon double bonds (when such reduction is undesirable) are employed. Examples of these agents are the metal borohydrides, especially sodium, potassium, and zinc borohydrides, lithium(tri-tert-butoxy)-aluminum hydride, metal trialkyl borohydrides, e.g. sodium trimethoxy borohydride, lithium borohydride, and the like. In those cases in which carbon-carbon double bond reduction need not be avoided, the boranes, e.g. disiamylborane (bis-3-methyl-2-butyl borane) are alternatively employed.
For the production of C-15 epimerically pure prostaglandins, the 15-epi compound is separated from the mixture by methods known in the art. For example, silica gel chromatography is advantageously employed.
For the transformation of the 3-oxo bicyclic lactone to the corresponding 3-methoxy bicyclic lactone, the 3-hydroxy moiety of the 3-hydroxy bicyclic lactone prepared above is alkylated, employing methods known in the art.
The alkylation described in the above paragraph proceeds, for example, by reaction of the 3-hydroxy bicyclic lactone with diazomethane, preferably in the presence of a Lewis acid (e.g., boron trifluoride etherate, aluminum chloride, or fluoboric acid). See for reference Fieser, et al., "Reagents for Organic Synthesis," John Wiley and Sons, New York, N. Y., (1967), especially page 191. The reaction is carried out by mixing a solution of the diazomethane in a suitable inert diluent, preferably diethyl ether, with the 3-hydroxy bicyclic lactone prepared above. This reaction proceeds at about 25° C.
An alternate method for the alkylation of the 3-hydroxy compound is by reaction with methanol in the presence of boron trifluoride etherate. Thus, the methanol and boron trifluoride etherate are reacted with the 3-hydroxy compound at 25° C., the reaction being monitored conveniently by thin layer chromatography (TLC).
The 3-oxo bicyclic lactone is transformed into the corresponding (3RS)-3-methyl bicyclic lactone wherein M 5 is a mixture of ##STR64## by reaction of the 3-oxo bicyclic lactone with a Grignard reagent, CH 3 MgHal, wherein Hal is chloro, bromo, or iodo. The Grignard complex is thereafter hydrolyzed, for example, using saturated aqueous ammonium chloride as is known in the art. An alternate method for transforming the 3-oxo compound to a 3(RS)-3-methyl compound is by reaction of the 3-oxo bicyclic lactone with trimethylaluminum.
The preferred method for separation of these (3RS)-3-methyl epimers is by separation of the corresponding C-15 epimers of the PG-type, methyl esters using silica gel chromatography or high pressure liquid chromatography (HPLC). The formula XXV compound is prepared from the formula XXIV compound by deacylation, as described above. The formula XXVI compound is then prepared from the formula XXV compound by replacing any free hydroxy moieties with blocking groups according to R 10 by the procedure described above. The formula XXVII compound is then prepared from the formula XXVI compound by reduction of the formula XXVI lactone to a lactol. Methods known in the art are employed. For example, diisobutylaluminum hydride is employed at -60° to -70° C.
Chart B provides a method whereby the formula XXXI lactol, prepared according to Chart A, is transformed into a corresponding formula XXXV 3-oxa-14-halo-PGF 1 .sub.α -type compound.
The formula XXXII compound is obtained from the formula XXXI lactol by the Wittig reaction, with an (alkoxymethylene)triphenyl phosphorane, R 22 OOC--CH=P(C 6 H 5 ) 3 , wherein R 22 is as defined above. The reaction is conveniently carried out at 25° C. using methods and reactants known in the art.
The formula XXXIII compound is then obtained by reduction of the ethylenic group in the carboxyl-containing side chain. For this purpose a reducing agent is used which does not reduce the Y group, for example hydrogen in the presence of a catalyst such as tris(triphenylphosphine)rhodium (I) chloride. Mild conditions are sufficient such as a pressure of 1-3 atmospheres and temperatures of 0° to 40° C.
The formula XXXIV alcohol is obtained from the formula XXXIII compound by reduction, for example with lithium aluminum hydride or lithium trimethoxy aluminum hydride. A solvent such as diethyl ether or tetrahydrofuran is conveniently used.
The formula XXXV compound is obtained by a Williamson synthesis, condensing the formula XXXIV alcohol with a haloalkanoate, Hal-(CH 2 ) g -COOR 1 , wherein Hal is chloro, bromo, or iodo and g and R 1 as above defined, in the presence of a base. For the base, there is used, for example, n-butyllithium, phenyllithium, triphenylmethyllithium, sodium hydride, or potassium t-butoxide. It is preferred that only one molecular equivalent of the base be used. The alkanoate is employed in about 100% stoichoimetric excess. Instead of a haloalkanoic acid ester, a salt, for example lithium chloroacetate is useful. After the condensation, the salt is transformed to the XXXV compound by methods known in the art. The condensation is conveniently run in a solvent such as dimethyl formamide, tetrahydrofuran, dimethyl sulfoxide, or hexamethylphosphoramide.
With respect to Chart C a method is provided whereby the formula XLI lactol is transformed into the corresponding formula XLIII 5-oxa-14-halo-PGF 1 .sub.α -type compound. The formula XLII alcohol is obtained upon reduction of the formula XLI lactol, for example, with aqueous methanolic or ethanolic sodium borohydride. Alternatively, and preferably, the formula XLII compound is obtained by a one step reduction of the formula XXVI lactone, for example, with lithium aluminum hydride or diisobutyl aluminum hydride at a temperature ranging from 0 to 35° C. For preparing the formula XLIII compound a Williamson synthesis is employed. For example, the formula XLII compound is condensed with a haloalkanoate within the scope of
Hal--(CH.sub.2).sub.g --CH.sub.2 --COOR.sub.1,
wherein Hal is chloro, bromo, or iodo and g is as defined above. Normally the reaction is done in the presence of a base such as n-butyllithium, phenyllithium, trimethyllithium, sodium hydride, or potassium t-butoxide.
Alternatively and preferably, an ortho-4-bromo-alkanoate is employed. Such reagents are available or are prepared by methods known in the art, for example, from the appropriate halonitrile by way of the corresponding imino ester hydrohalide as illustrated hereinafter.
The condensation is conveniently run in a solvent, such as tetrahydrofuran or dimethyl sulfoxide or especially if an organolithium compound is employed, preferably in dimethylformamide or hexamethylphosphoramide. The reaction proceeds smoothly at -20° to 50° C., but is preferably performed at ambient temperature. Following the condensation the formula XLIII compound is obtained by methods known in the art, for example, by hydrolysis in cold dilute mineral acid.
Chart D provides a method whereby the formula LI compound is transformed into the corresponding formula LVIII 4-oxa-14-halo-PGF 1 .sub.α -type compound or formula LIX cis-4,5-didehydro-14-halo-PGF 1 .sub.α -type compound.
The formula LI compound undergoes condensation to form the formula LII enol. For this purpose a hydrocarbyloxy, and preferably an alkoxymethylenetriphenylphosphorane is useful. See for reference, Levine, Journal of the American Chemical Society 80, 6150 (1958). The reagent is conveniently prepared from a corresponding quaternary phosphonium halide in a base, e.g. butyllithium or phenyllithium, at low temperature, e.g. preferably below -10° C. The formula LI lactol is mixed with the above reagent and the condensation proceeds smoothly within the temperature range of -30° C.-+30° C. At higher temperatures the reagent is unstable, whereas at low temperatures the rate of condensation is undesirably slow. Examples of alkoxymethylenetriphenylphosphoranes preferred for the above purposes are methoxy-, ethoxy-, propoxy-, isopropoxy-, butoxy-, isobutoxy-, s-butoxy-, and t-butoxy-methylenetriphenylphosphorane. Various hydrocarbyloxymethylenetriphenylphosphoranes which are optionally substituted for the alkoxymethylenetriphenylphosphoranes and are accordingly useful for preparing the formula LII intermediates wherein R 26 is hydrocarbyl, include alkoxy-, aralkoxy-, cycloalkoxy-, and aryloxymethylenetriphenylphosphoranes. Examples of these hydrocarbyloxytriphenylphosphoranes are 2-methyl butyloxy-, isopentyloxy-, heptyloxy-, octyloxy-, nonyloxy-, tridecyloxy-, octadecyloxy-, benzyloxy-, phenethyloxy-, p-methylphenethyloxy-, 1-methyl-3-phenylpropyloxy-, cyclohexyloxy-, phenoxy-, and p-methylphenoxy-, phenoxymethylenetriphenylphosphorane. See for reference, Organic Reactions, Vol. 14, pg. 346-348, John Wiley and Sons, New York, New York, (1965). The formula LII enol intermediates are then hydrolyzed to the formula LIII lactols. This hydrolysis is done under acidic conditions for example with perchloric acid or acetic acid. Tetrahydrofuran is a suitable diluent for this reaction mixture. Reaction temperatures of from 10° to 100° C. are employed. The length of time required for hydrolysis is determined in part by the hydrolysis temperature and using acetic acid-water-tetrahydrofuran at about 60° C. several hr. are sufficient to accomplish the hydrolysis.
The formula LIV compound is then prepared from the formula LIII compound by oxidation of the formula LIII lactol to a lactone. This transformation is carried out, using for example, silver oxide as an oxidizing reagent, followed by treatment with pyridine hydrochloride.
The formula LIV lactone may then be converted to the formula LV ether by transformation of any free hydroxy moieties to blocking groups, according to R 10 , following the procedures herein described for these transformations.
Thereafter the formula LVI compound is prepared from the formula LV compound by reduction of the formula LV lactone to a lactol. For example, diisobutylaluminum hydride is employed as is described above for the reduction of lactones to lactols. The formula LVI lactols so prepared are then used alternatively for the preparation of the formula LVIII or LIX compound.
In the preparation of the formula LVIII compound, the formula LVI lactol is first transformed into the formula LVII compound by reduction of the formula LVI lactol. The formula LVII compound is then transformed into the corresponding formula LVIII compound by a Williamson synthesis. Methods and corresponding reagents employed in the transformation of the formula LVI compound to the formula LVII and thereafter the transformation of the formula LVII compound to the formula LVIII compound are analogous to methods described hereinabove for the transformation of the formula XCI compound to the formula XCII compound and thereafter the transformation of the formula XCII compound to the formula XCIII compound.
Accordingly, the formula LVIII 4-oxa-PGF 1 .sub.α -type compound is prepared.
The formula LIX compound is prepared from the formula LVI compound by a Wittig alkylation, using the appropriate (ω-carboxyalkyl)triphenylphosphonium bromide, HOOC-CH 2 -(CH 2 ) h -CH 2 -P-(C 6 H 5 ) 3 , wherein h is as defined above. The reaction proceeds as is generally known in the art, by first mixing the appropriate (ω-carboxyalkyl)triphenylphosphonium bromide with sodio dimethyl sulfinylcarbanide, at ambient temperature, and adding the formula LVI lactol to this mixture. Thereafter the carboxy hydrogen of the compound so formed is transformed to an R 1 moiety by the methods and procedures hereinbelow described. Accordingly, there is prepared the formula LIX cis-4,5-didehydro-PGF 1 .sub.α -type compound.
Chart E provides a method whereby the formula LXI compound is transformed to the corresponding formula LXII 14-halo-PGF 2 .sub.α - or 11-deoxy-14-halo-PGF 2 .sub.α -type compound or formula LXIII 14-halo-PGF 1 .sub.α - or 11-deoxy-14-halo-PGF 1 .sub.α -type compound.
The formula LXII compound is prepared from the formula LXI compound using the appropriate (ω-carboxyalkyl)triphenylphosphonium bromide, HOOC-(CH 2 ) g -CH 2 -P-(C 6 H 5 ) 3 Br, as is described above followed by transformation of the carboxy hydrogen to an R 1 moiety as described below. The formula LXIII compound is then prepared from the formula LXII compound by catalytic hydrogenation of the cis-5,6-double bond. Hydrogenation methods known in the art are employed, e.g., the use of metal catalysts under a hydrogen atmosphere. The reaction here is terminated when one equivalent of hydrogen is absorbed per equivalent of prostaglandin-type compound. Mixtures of compounds thereby produced are conveniently separated by silica gel chromatography.
Chart F provides a method whereby the prostaglandin-type intermediates of Charts B, C, D, and E are transformed to the corresponding 14-halo-PGF, 11-deoxy-14-halo-PGF, 14-halo-PGE, 11-deoxy-14-halo-PGE, 14-halo-PGA, or 14-halo-PGB compounds.
The formula LXXI compound is as prepared above. The formula LXXII PGE-type compound is prepared from the formula LXXI compound by oxidation methods known in the art. For example, the Jones reagent is advantageously employed herein. The formula LXXIII compound is then prepared from the formula LXXI compound or the formula LXXII compound by hydrolysis of any blocking groups. Such hydrolysis proceeds by mixing the reactant with, for example, water, tetrahydrofuran, and acetic acid as described above.
The formula LXXIV compound is then prepared from the formula LXXIII compound by transformation of the R 1 moiety of the formula LXXXIII compound to its methyl ester. Methods hereinbelow described are employed. The C-15 epimers are then separated, thereby preparing the formula LXXV compound.
The formula LXXVI compound, which is represented by formula LXXIII when the M 5 moiety consists of separated C-15 epimers, is prepared optionally from the formula LXXV compound by transformation of the carboxy methyl ester of formula LXXV compound to an R 1 moiety as described above.
The formula LXXVII compound is prepared from the formula LXXVI compound wherein M 18 is =O by a ring carbonyl reduction. Methods hereinbelow described are employed. The formula LXXVIII and formula LXXIX compounds are prepared from the formula LXXVI wherein M 18 is O employing an acidic or basic dehydration respectively. Methods described below for these acidic or basic dehydrations are employed.
The formula LXXVIII compound is optionally prepared from the formula LXXVI compound wherein R 8 is hydroxy by acetylation with acetic anhydride, thereby preparing a highly unstable corresponding PGE-type 11,15-diacetate, followed by silica gel chromatography. The PGE-type 11,15-diacetate thereby spontaneously decomposes to the corresponding PGA-type 15-acetate, which is hydrolysed to yield the formula LXXVIII PGA-type product. Optionally, however, the 11,15-diacetate may be allowed to stand at room temperature whereby spontaneous decomposition will ordinarily be effected within one to five days.
The above acidic dehydrations are carried out by methods known in the art for acidic dehydrations of known prostanoic acid derivatives. See for reference Pike, et al., Proceedings of the Nobel Symposium II, Stockholm (1966), Interscience Publishers, New York, pg. 162-163 (1967); and British Spec. No. 1,097,533. Alkanoic acids of 2 to 6 carbon atoms, inclusive, preferentially acetic acid, are employed in this acidic dehydration. Dilute aqueous solutions of mineral acids e.g. hydrochloric acid, especially in the presence of a solubilizing diluent, e.g. tetrahydrofuran, are also useful as reagents for this acidic dehydration. Use however, of mineral acids as described above may cause partial hydrolysis of the carboxy ester of the formula LXXVI PGE reactant.
The above basic hydrations or double bond migrations (i.e., conversion of the PGA-type compound to the PGB-type compound are carried out by methods known in the art for dehydration or double bond migration of known prostanoic acid derivatives. See for reference Bergstrom, et al., Journal of Biological Chemistry 238, 3555 (1963). Bases employed are any of those whose aqueous solution has pH greater than 10. Preferred bases are the alkali metal hydroxides. A mixture of water and sufficient quantity of a water miscible alkanol to yield a homogeneous reaction mixture is suitable as a reaction medium. The reactant is then maintained in such reaction medium until the starting material is completely reacted, as shown by the characteristic ultraviolet absorption of the PGB-type compound at 278 mμ.
In the employment of the processes above when C-15 tertiary alcohols are to be prepared (R 5 is methyl) the use of blocking groups is not required. Accordingly, in the steps of the above charts the introduction and hydrolysis of blocking groups are thereby omitted by the preferred process.
Certain (3RS)-3-methyl lactones of chart A may be separated into their respective (3S) or (3R)- epimers by silica gel chromatographic separation techniques. Where such separation is possible, this route is preferred. Accordingly, in these cases the separation is effected and M 5 is ##STR65## wherein R 10 is a blocking group. Accordingly, the separation procedure described in Chart F (formula LXIII-LXXV) is omitted when the optional lactone separation is employed.
When a cis-4,5-didehydro-14-halo-PGF 1 .sub.α or cis-4,5-didehydro-11-deoxy-14-halo-PGF 1 .sub.α -type compound is to be prepared by the procedure of Chart D, the Wittig alkylation step LVI to LIX may be performed on the formula LIII lactol, instead of the formula LVI lactol, thereby eliminating the oxidation, etherification, and reduction steps of Chart D (LIII through LVI).
Charts G, H, I, and J provide methods whereby 3-oxa-3,7-inter-m-phenylene-4,5,6-trinor- or 3,7-inter-m-phenylene-4,5,6-trinor-PG-type intermediates are prepared. With respect to Charts G and H, R 7 is preferred to be --(CH 2 ) m --CH 3 , or ##STR66## wherein m, T, and s are as defined above. In Charts I or J a method is provided for preparing those novel compounds of this specification wherein R 7 is preferably cis---CH=CH--CH 2 --CH 3 , or ##STR67## wherein T and s are as defined above, respectively. Accordingly the Charts G-J provide methods whereby intermediates useful in producing all inter-m-phenylene-PG-type compounds are prepared.
In Chart G both endo and exo forms of bicylco hexene LXXXI are available or are made by methods known in the art, in either their racemic or enantiomerically pure forms. See U.S. Pat. No. 3,711,515. Either the endo or exo starting material will yield the ultimate intermediates of formuls XCIII compound by the process of Chart G.
Oxetane LXXXII is obtained by reaction of the formula LXXXI bicyclo hexene with an aldehyde of the formula ##STR68## wherein R 63 is carboxyacyl of the formula ##STR69## wherein R 64 is hydrogen, alkyl of one to 19 carbon atoms, inclusive, or aralkyl of 7 to 12 carbon atoms, inclusive, wherein alkyl or aralkyl are substituted with zero to 3 halo atoms.
The above benzyl aldehydes are available or readily prepared by methods known in the art. Examples of such compounds within this scope are: ##STR70##
The formation of oxetane LXXXII is accomplished by photolysis of a mixture of the bicyclo hexene and the aldehyde in a solvent. The bicyclo hexene is preferably used in excess over the molar equivalent, for example 2 to 4 times the stoichiometric equivalent amount. The solvent is a photochemically inert organic liquid, for example liquid hydrocarbons, including benzene or hexane, 1,4-dioxane, and diethyl ether. The reaction is conveniently run at ambient conditions, for example 25° C., but may be done over a wide range of temperature, from about -78° C. to the boiling point of the solvent. The irradiation is done with mercury vapor lamps of the low or medium pressure type, for example those peaking at 3500 A. Such sources are available from The Southern New England Ultraviolet Co., Middletown, Conn. Alternatively, those lamps which emit a broad spectrum of wavelengths and which may be filtered to transmit only light of λ ˜3000-3700 A may also be used. For a review of photoysis see D. R. Arnold in "Advances in Photochemistry", Vol. 6, W. A. Noyes et al., Wiley-interscience, New York, 1968, pp. 301-423.
The cleavage of the oxetane ring to yield the formula LXXXIII compound from the formula LXXXII compound is accomplished with an alkali metal in the presence of a primary amine or a alcohol. Preferred is lithium in ethylamine, or sodium in ethyl alcohol. See L. J. Altman et al., Synthesis 129 (1974). The cleavage transformation may also be accomplished by catalytic hydrogenation over an inert metal catalyst, e.g. Pd on carbon, in ethyl acetate or ethanol.
The formula LXXIV compound is prepared from the formula LXXXIII diol by preferably blocking the two hydroxyl groups with carboxyacyl groups according to R 63 , i.e. ##STR71## as defined above. For example, the diol is treated with an acid anhydride such as acetic anhydride, or with an acyl halide in a tertiary amine. Especially preferred is pivaloyl chloride in pyridine.
Other carboxyacylating agents useful for this transformation are known in the art or readily obtainable by methods known in the art, and include carboxyacyl halides, preferably chlorides, bromides, or fluorides, i.e. R 64 C(O)Cl, R 64 C(O)Br, or R 64 C(O)F, and carboxy acid anhydrides, (R 64 CO) 2 O, wherein R 64 is as defined above. The preferred reagent is an acid anhydride. Examples of acid anhydrides useful for this purpose are acetic anhydride, propionic anhydride, butyric anhydride, pentanoic anhydride, nonanoic anhydride, tridecanoic anhydride, steric anhydride, (mono, di, or tri)chloroacetic anhydride, 3-chlorovaleric anhydride, 3-(2-bromoethyl)-4,8-dimethylnonanoic anhydride, cyclopropaneacetic anhydride, 3-cycloheptanepropionic anhydride, 13-cyclopentanetridecanoic anhydride, phenylacetic anhydride, (2 or 3)-phenylpropionic anhydride, 13-phenyltridecanoic anhydride, phenoxyacetic anhydride, benzoic anhydride, (o, m, or p)-bromobenzoic anhydride, 2,4 (or 3,4)-dichlorobenzoic anhydride, p-trifluoromethylbenzoic anhydride, 2-chloro-3-nitrobenzoic anhydride, (o, m, or p)-nitrobenzoic anhydride, (o, m, or p)-toluic anhydride, 4-methyl-3-nitrobenzoic anhydride, 4-octylbenzoic anhydride, (2,3, or 5)-biphenylcarboxylic anhydride, 3-chloro-4-biphenylcarboxylic anhydride, 5-isopropyl-6-nitro-3-biphenylcarboxylic anhydride, and ( 1 or 2)-naphthoic anhydride. The choice of anhydride depends upon the identity of R 64 in the final acylated products, for example when R 64 is to be methyl, acetic anhydride is used; when R 64 is to be 2-chlorobutyl, 3-chlorovaleric anhydride is used.
When R 64 is hydrogen, ##STR72## is formyl. Formylation is carried out by procedures known in the art, for example, by reaction of the hydroxy compound with the mixed anhydride of acetic and formic acids or with formylimidazole, See, for example, Fieser et al., Reagents for Organic Synthesis, John Wiley and Sons, Inc., pp. 4 and 407 (1967) and references cited therein. Alternatively, the formula LXXXIII diol is reacted with two equivalents of sodium hydride and then with excess ethyl formate.
In formula LXXXIV, R 68 may also represent a blocking group including benzoyl, substituted benzoyl, monoesterified phthaloyl and substituted or unsubstituted naphthoyl. For introducing those blocking groups, methods known in the art are used. Thus, an aromatic acid of the formula R 63 OH, wherein R 63 is as defined above, for example benzoic acid, is reacted with the formula LXXXIII compound in the presence of a dehydrating agent, e.g. sulfuric acid, zinc chloride, or phosphoryl chloride; or an anhydride of the aromatic acid of the formula (R 64 CO) 2 O, for example benzoic anhydride, is used.
Preferably, however, an acyl halide, e.g. R 63 Cl, for example benzoyl chloride, is reacted with the formula LXXXIII compound in the presence of a tertiary amine such as pyridine, triethylamine, and the like. The reaction is carried out under a variety of conditions using procedures generally known in the art. Generally, mild conditions are employed, e.g. 20°-60° C., contacting the reactants in a liquid medium, e.g. excess pyridine or an inert solvent such as benzene, toluene, or chloroform. The acylating agent is used either in stoichiometric amount or in excess.
As examples of reagents providing R 63 for the purposes of this invention, see the discussion above pertaining to the use of acyl protecting groups.
The formula LXXXIV acetal is converted to aldehyde LXXXV by acid hydrolysis, known in the art, using dilute mineral acids, acetic or formic acids, and the like. Solvents such as acetone, dioxane, and tetrahydrofuran are used.
For the conversion of LXXXV to LXXXIX, it is optional whether R 66 be hydrogen or a "blocking group" as defined below. For efficient utilization of the Wittig reagent it is preferred that R 66 be a blocking group. If the formula LXXXIV compound is used wherein R 68 is hydrogen, the formula LXXXV intermediate will have hydrogen at R 66 . If R 66 is to be a blocking group, that may be readily provided prior to conversion of LXXXV to LXXXVI by reaction with suitable reagents as discussed below.
The blocking group, R 65 , is any group which replaces hydrogen of the hydroxyl groups, which is not attached by nor is reactive to the reagents used in the respective transformations to the extent that the hydroxyl group is, and which is subsequently replaceable by hydrogen at a later stage in the preparation of the prostaglandin-like products.
Several blocking groups are known in the art, e.g. tetrahydropyranyl, acetyl, and p-phenylbenzoyl (see Corey et al., J. Am. Chem. Soc. 93, 1491 (1971)).
Those which have been found useful include (a) carboxyacyl within the scope of R 63 above, i.e. acetyl, and also benzoyl, naphthoyl, and the like; (b) blocking groups according to R 10 ; and (c) -Si(G 1 ) 3 wherein G 1 is as defined above.
In replacing the hydrogen atoms of the hydroxyl groups with a carboxyacyl blocking group, methods known in the art are used. The reagents and conditions are discussed above for R 68 on the compound of formula LXXXIV.
When the blocking group is according to R 10 appropriate reagents and conditions are as defined above.
When the blocking group is silyl of the formula --Si(G 1 ) 3 , the formula LXXXIV compound is transformed to a silyl derivative of formula LXXXV by procedures known in the art. See, for example, Pierce, "Silylation of Organic Compounds," Pierce Chemical Co., Rockford, Illinois (1968). The necessary silylating agents for these transformations are known in the art or are prepared by methods known in the art. See, for example, Post "Silicones and Other Silicon Compounds," Reinhold Publishing Corp., New York, N.Y. (1949). These reagents are used in the presence of a tertiary base such as pyridine at temperatures in the range of about 0° to +50° C. Examples of trisubstituted monochlorosilanes suitable for this purpose include chlorotrimethylsilane, chlorotriisobutylsilane, chlorotriphenylsilane, chlorotris(p-chlorophenyl)silane, chlorotri-m-tolylsilane, and tribenzylchlorosilane. Alternatively, a chlorosilane is used with a corresponding disilazane. Examples of other silylating agents suitable for forming the formula LXXXV intermediates include pentamethylsilylamine, pentaethylsilylamine, N-trimethylsilyldiethylamine, 1,1,1-triethyl-N,N-dimethylsilylamine, N,N-diisopropyl-1,1,1-trimethylsilylamine, 1,1,1-tributyl-N,N-dimethylsilylamine N,N-dibutyl-1,1,1-trimethylsilylamine, 1-isobutyl-N,N,1,1-tetramethylsilylamine, N-benzyl-N-ethyl-1,1,1-trimethylsilylamine, N,N,1,1-tetramethyl-1-phenylsilylamine, N,N-diethyl-1,1-dimethyl-1-phenylsilylamine, N,N-diethyl-1-methyl-1,1-diphenylsilylamine, N,N-dibutyl-1,1,1-triphenylsilylamine, and 1-methyl-N,N,1,1-tetraphenylsilylamine.
In transforming the formula LXXXV compound to the formula LXXXVI compound the aldehyde group is transformed by the Wittig reaction to a moiety of the formula ##STR73## For this purpose a phosphonium salt prepared from an organic chloride or bromide of the formula ##STR74## is employed, wherein L 1 , R 7 , and R 53 are as defined above. These organic chlorides or bromides are known in the art or are readily prepared by methods known in the art. See for example the above-identified German Offenlegungsschrift No. 2,209,990. As to the Wittig reaction, see, for example, U.S. Pat. No. 3,776,941 and references cited therein.
The formula LXXXVII compound is obtained by deblocking if necessary. When R 66 is a hindered carboxyacyl, R 66 on the phenolic hydroxy is selectively replaced with hydrogen by hydrolysis with sodium or potassium hydroxide in ethanol-water. Instead of ethanol, other water-miscible solvents may be substituted, for example 1,4-dioxane, tetrahydrofuran, or 1,2-dimethoxyethane. The selective hydrolysis is preferably carried out at -15° to 25° C. Higher temperatures may be used but with some decrease in selectivity.
Total hydrolysis of R 66 blocking groups on the formula LXXXVI compound is accomplished, when R 66 is carboxyacyl, with an alkali alkoxide in an alcoholic solvent, preferably sodium methoxide in methanol at a temperature from 25° C. to 50° C. When R 66 is trialkylsilyl, either aqueous acid or base are used at 25° to 50° C.
Continuing with Chart G, a Williamson synthesis employed to obtain the formula LXXXVIII compound. The formula LXXXVII phenol is condensed with a haloalkanoate within the scope of Hal--(CH 2 ) g --COOR 1 wherein Hal is chloro, bromo, or iodo and g and R 1 are as defined above. Normally the reaction is done in the presence of a base such as n-butyllithium, phenyllithium, triphenylmethyllithium, sodium hydride, potassium t-butoxide, sodium hydroxide, or potassium hydroxide.
The transformation of the formula LXXXVIII compound to the formula LXXXIX is accomplished by any one of several routes known in the art. See U.S. Pat. No. 3,711,515. Thus, the alkene LXXXVIII is hydroxylated to glycol LXXXIX. For this purpose osmium tetroxide is a suitable reagent, for example in conjunction with N-methylmorpholine oxide-hydrogen peroxide complex (see Fieser et al., "Reagents for Organic Synthesis", p. 690, John Wiley and Sons, Inc., New York (1967)). Thereafter, several methods are available for obtaining the formula XC product. In one method the glycol is converted to a bis(alkanesulfonic acid) ester and subsequently hydrolyzed to the formula XC compound by methods known in the art (See, for example German Offenlegungsschrift No. 1,936,676, Derwent Farmdoc No. 6862R). Another method is by way of a diformate by formolysis of the glycol (see U.S. Pat. No. 3,711,515).
Still another method is by way of a cyclic ortho ester. For this purpose, glycol LXXXIX is reacted with an ortho ester of the formula ##STR75## wherein R 74 is hydrogen, alkyl of one to 19 carbon atoms, inclusive, or aralkyl of 7 to 12 carbon atoms, inclusive, substituted with zero to 3 halo atoms; and R 75 is methyl or ethyl. There is then formed a cyclic orthoester of the formula ##STR76## wherein g, R 1 , R 53 , R 66 , R 74 , R 75 , L 1 and R 7 are as defined above. The reaction goes smoothly in a temperature range of -50° C. to +100° C., although for convenience 0° C. to +50° C. is generally preferred. From 1.5 to 10 molar equivalents of the ortho ester are employed, together with an acid catalyst. The amount of the catalyst is usually a small fraction of the weight of the glycol, e.g., about 1%, and typical catalysts include pyridine hydrochloride, formic acid, hydrogen chloride, p-toluenesulfonic acid, trichloroacetic acid, or trifluoroacetic acid. The reaction is preferably run in a solvent, for example benzene, dichloromethane, ethylacetate, or diethyl ether. It is generally completed within a few minutes and is conveniently followed by TLC (thin layer chromatography on basic silica gel plates).
The ortho ester reagents are known in the art or readily available by methods known in the art. See for example S. M. McElvain et al., J. Am. Chem. Soc. 64, 1925 (1942), starting with an appropriate nitrile. Examples of useful ortho esters include:
trimethyl orthoformate,
triethyl orthoacetate,
triethyl orthopropionate,
trimethyl orthobutyrate,
trimethyl orthovalerate,
trimethyl orthooctanoate,
trimethyl orthophenylacetate, and
trimethyl ortho (2,4-dichlorophenyl)acetate.
Preferred are those ortho esters wherein R 74 is alkyl of one to 7 carbon atoms; especially preferred are those wherein R 74 is alkyl of one to 4 carbon atoms.
Next, the cyclic orthoester depicted above is reacted with anhydrous formic acid to yield a diol diester of the formula ##STR77## wherein g, R 1 , R 7 , R 53 , R 66 , and L 1 are as defined above.
Anhydrous formic acid refers to formic acid containing not more than 0.5% water. The reaction is run with an excess of formic acid, which may itself serve as the solvent for the reaction. Solvents may be present, for example dichloromethane, benzene, or diethyl ether, usually not over 20% by volume of the formic acid. There may also be present organic acid anhydrides, for example acetic anhydride, or alkyl orthoesters, for example trimethyl orthoformate, which are useful as drying agents for the formic acid. Although the reaction proceeds over a wide range of temperatures, it is conveniently run at about 20°-30° C. and is usually completed within about 10 minutes.
Finally, the diol diester above is converted to product XC by methods known in the art, for example by hydrolysis in the presence of a base in an alcoholic medium. Examples of the base are sodium or potassium carbonate or sodium or potassium alkoxides including methoxides or ethoxides. The reaction is conveniently run in an excess of the solvolysis reagent, for example methanol or ethanol. The temperature range is from -50° C. to 100° C. The time for completion of the reaction varies with the nature of R 74 and the base, proceeding in the case of alkali carbonates in a few minutes when R 74 is hydrogen but taking up to several hours when R 74 is ethyl, for example.
When the solvolysis proceeds too long or when conditions are too severe, an ester group (R 1 ) is often removed. They are, however, readily replaced by methods known in the art. See the discussion below.
The formula XCI compound is prepared from the formula XC compound by oxidation of the C-15 hydroxy to a 15-oxo. Accordingly, as is known in the art, 2,3-dichloro-5,6-dicyano-1,4-benzoquinone, activated manganese dioxide, or nickel peroxide (See Fieser, et al., "Reagents for Organic Synthesis", John Wiley and Sons, New York, N.Y., pgs. 215, 637 and 731) is advantageously employed. Thereafter, the formula XCI compound is prepared from the 15-oxo compound by transforming the C-9 and C-11 hydroxy hydrogens to R 65 blocking groups. Procedures known in the art are employed. See for reference Pierce, "Silylation of Organic Compounds," Pierce Chemical Company, Rockford, Ill. (1968) and the discussion above pertaining to the intorduction of blocking groups according to R 10 . The necessary silylating reagents for these transformations are known in the art or are prepared by methods known in the art. See for reference, Post, "Silicones and Other Silicone Compounds," Reinhold Publishing Corp., New York, N.Y. (1949).
The formula XCII compound is then prepared from the formula XCI compound by the procedure described in Chart A for transforming the formula XXII compound to the formula XXIV compound, followed by hydrolysis of the silyl groups, using, for example, dilute aqueous acetic acid in a water miscible solvent, such as ethanol (sufficient to yield a homogeneous reaction mixture). At 25° C., the hydrolysis is ordinarily complete in 2 to 12 hrs. Further, the hydrolysis preferably carried out in an inert atmosphere, e.g., nitrogen or argon.
The formula XCIII compound is prepared from the formula XCII compound by separation of the 15-methyl epimers when present. Such separation proceeds by methods discussed above for accomplishment of this purpose (e.g., thin layer chromatography or high pressure liquid chromatography).
Referring to Chart H, there are shown process steps by which the formula XCVI bicyclo hexene is transformed first to an oxetane (formula XCVII) with a fully developed side chain, e.g., ##STR78## wherein Z 3 is oxa or methylene, and ultimately to the formula CIV compound.
In transforming XCVI to XCVII in Chart H, there is employed an aldehyde of the formula ##STR79## wherein Z 3 and R 69 are as defined above. Such aldehydes are available or are readily prepared by methods known in the art, e.g., ##STR80##
The conditions for this transformation are essentially the same as for the corresponding step of Chart G (i.e., LXXXI to LXXXII). Thereafter, the preparation of the formula CI compound proceeds by methods analogous and by employing the same conditions as the corresponding steps of Chart G (i.e., LXXXII to LXXXVI).
The steps transforming CI to CIV then proceed in similar fashion, employing the same or similar reagents and conditions as the corresponding steps of Chart G discussed above.
Referring next to Chart I the process steps are shown whereby aldehyde CVI prepared in Chart H is transformed to a 17,18-tetradehydro-PG intermediate (formula CIX) and 17,18-didehydro-PG intermediate (formula CX).
In Chart I, A Wittig reagent is employed which is prepared from a phosphonium salt of a haloalkyne of the formula ##STR81## wherein R 53 and L 1 are as defined above, (See, for example, U. Axen et al., Chem. Comm. 1969, 303, and ibid, 1970, 602) in transforming CVI to CVII.
Thereafter, in subsequent transformations yielding the 17,18-tetradehydro compound CIX, the reagents and conditions are similar to those employed for the corresponding reactions shown in Chart H.
Transformation of the formula CIX compound to the formula CX compound is accomplished by hydrogenation of CIX using a catalyst which catalyzes hydrogenation of --C.tbd.C-- only to cis-CH=CH-, as known in the art. See, for example, Fieser et al., "Reagents for Organic Syntheses", pp. 566-567, John Wiley and Sons, Inc., New York (1967). Preferred is Lindlar catalyst in the presence of quinoline. See Axen, references cited above.
As discussed above, Chart J provides a method whereby the formula CXI PG-type intermediate, prepared according to Chart G or Chart H is transformed to the corresponding formula CXIV 16-phenoxy-PG-type intermediates.
The formula CXII compound is prepared from the formula CXI compound by cleavage of the 13,14-trans double bond, conveniently by ozonolysis. Ozonolysis proceeds by bubbling dry oxygen, containing about 3 percent ozone, through a mixture of a formula CXI compound in a suitable nonreactive diluent. For example, n-hexane is advantageously employed. The ozone may be generated using methods known in the art. See, for example Fieser, et al., "Reagents for Organic Synthesis," John Wiley and Sons, Inc. (1967), pages 773-777. Reaction conditions are maintained until the reaction is shown to be complete, for example, by silica gel thin layer chromatography or when the reaction mixture no longer rapidly decolorizes a dilute solution of bromine in acetic acid.
The formula CXIII compound is then prepared from the formula CXII compund employing a phosphonate of the formula: ##STR82## wherein R 15 , L 1 , T, and s are as defined above. Phosphonates of this general formula are prepared by methods known in the art. See the text hereinabove accompanying Chart A for discussion of the preparation and the appropriate reaction conditions by which the Wittig reaction proceeds. The formula CXIV compound is prepared from the formula CXIII compound by transformation of the 15-oxo moiety to an M 1 moiety. Methods hereinabove, particularly those discussed in Charts G and H above, are employed.
Optionally the methods of Chart J is used to introduce the various other R 7 moieties to the formula CXII compound using the appropriate phosphonate.
Chart K provides a method whereby the formula CXXI bicyclic lactone aldehyde is transformed to the corresponding formula CXXIV PGF 2 .sub.α -type intermediate which is useful according to the procedures of Chart L in preparing the novel 13,14-didehydro-PGF 2 .sub.α -type compounds disclosed in this specification.
The formula CXXI compound is known in the art. This compound is available in either of its two pure enantiomeric forms or as a mixture comprising both of these enantiomers. The formula CXXII compound is prepared from the formula CXXI compound using reagents and conditions analogous to the preparation of the formula XXIII compound of Chart A from the formula XXI compound. Thus, methods generally known to the art are employed. The formula CXXIII compound is then prepared from the formula CXXII compound using reaction conditions and reagents analogous to the preparation of the formula XXXV compound from the formula XXXI compound (Chart B), the preparation of the formula XLIII compound from the formula XLI compound (Chart C), -- the preparation of the formula LVIII or LIX compound from the formula LI compound (Chart D), or the preparation of the formula LXIII compound from the formula LXI compound (Chart E). Thereafter the formula CXXIV compound is prepared from the formula CXXIII compound by first hydrolyzing any blocking groups according to R 10 , (using procedures and methods hereinabove described), and second separating the C-15 epimers when R 5 is methyl. Methods herein described (e.g., silica gel chromatography or high pressure liquid chromatography) are employed.
Further by the procedure of Chart F, the various PGF.sub.α- or 11-deoxy-PGF.sub.α-type compounds prepared according to Charts G, H, I, J or K are transformed to corresponding PGE or 11-deoxy-PGE-, PGF.sub.β - or 11-deoxy-PGF.sub.β-, PGA-, or PGB-type compounds.
Chart L provides a method whereby the formula CXXXI compound (as shown in the art, or as prepared herein) is transformed to the corresponding formula CXXXVI 14-halo-PGF- or 11-deoxy-PGF-type product.
The formula CXXXII compound is prepared from the formula CXXXI compound by selective oxidation of the C-15 alcohol. The oxidation is accomplished employing conventional methods known in the art, for example, the use of 2,3-dichloro-5,6-dicyanobenzoquinone, activated manganese dioxide, or nickel peroxide. See Fieser, et al. "Reagents for Organic Synthesis" John Wiley and Sons, New York, N.Y. pages 215, 637, and 731.
The formula CXXXIII compound is prepared from the formula CXXXII compound by protection of free hydroxy moieties with acyl protecting groups according to R 9 . Methods described hereinabove for preparing these acyl derivatives are employed. Optionally, however, silyl groups within the scope of --Si(G 1 ) 3 , wherein G 1 is defined above, are employed in place of the acyl protecting groups. Finally, the acyl protection or silylation described herein is optionally omitted, particularly, where R 5 and R 6 of the M 1 moiety of the formula CXXXVI compound are both hydrogen.
The formula CXXXIV compound is prepared from the formula CXXXIII compound by 14-halogenation. This 14-halogenation is achieved by one of several general methods known in the art. For example, following the procedure of Chart A wherein the formula XXIII compound is prepared from the formula XXII compound, formula CXXXIV compound herein is prepared. As especially useful reagent for the instant transformation is sulfuryl chloride, as described above. Mixtures of products produced are separated, using conventional techniques. The formula CXXXV compound is then prepared from the formula CXXXIV compound by transformation of the 15-oxo to an M 1 moiety. Techniques as described hereinabove are employed. Thereafter, the formula CXXXVI compound is prepared from the formula CXXXV compound by removal of the optionally present acyl or silyl protecting groups, following the procedures described hereinabove.
Chart M provides a method whereby the 14-halo-8β,12α-PG-type compounds of formula CXLVI and CXLVII are prepared from the formula CXXXVIIa of formula CXXXVIIb enantiomeric starting material, which compounds are known in the art or readily prepared by methods known in the art. With respect to Chart M, R 51 is R 30 -SO 2 --, wherein R 30 is alkyl, cycloalkyl, aralkyl, phenyl, or phenyl substituted with alkyl or halogen, but preferably methyl or p-tolyl.
By the procedure of Chart M the formula CXXXVIIa compound is transformed to the formula CXXXVIII compound by the procedure described in Chart A for the preparation of the formula XXIV compound from the formula XXI compound. Thereafter, the formula CXXIX compound is prepared from the formula CXXXVIII compound by the method described in Chart A for the preparation of the formula XXVI compound from the formula XXV compound. Thereafter the formula CXXXIX compound is deacylated following the procedure described in Chart A for the preparation of the formula XXV compound from the formula XXIV compound. Following deacylation the formula CXLI compound prepared from the formula CXL compound by sulfonation. Thereby, the alkyl, aralkyl, cycloalkyl, phenyl or substituted phenyl sulfonyl derivative of the formula CXL compound is prepared. This sulfonation proceeds by a method analogous to the acylation, employing protecting groups according to R 9 , described hereinabove. Thus, for example, the sulfonyl chloride, e.g., mesyl chloride (methane sulfonyl chloride) or tosyl chloride (p-toluenesulfonyl chloride) is reacted with the hydroxy containing compound in the presence of a catalytic amount of an amine base (e.g. pyridine).
Thereafter the 11β-sulfonyl moiety is transformed to an 11α-acyl moiety employing the sodium, potassium or lithium salt of the corresponding carboxylicacid. Thus, for example when R 9 is benzoyl the formula CXLI sulfonyl derivative is reacted with sodium, potassium or lithium benzoate in an inert diluent (preferably, in a polar aprotic solvent) to yield the formula CXLII compound. As described above the carboxylic acids of the formula R 9 OH are known in the art or are readily prepared by methods known in the art. Further, these acids are transformed into the sodium, potassium or lithium salts employing conventional methods.
Thereafter, the formula CXLII compound is transformed to the formula CXLIII compound by selective deacylation of the R 9 protecting group. Methods described hereinabove for deacylation are employed (see the transformation of the formula CXXXIX compound to the formula CXL compound).
Thereafter the formula CXLIV compound is prepared from the formula CXLIII compound by transforming the 11-hydroxy hydrogen to a blocking group by methods hereinabove described or by transformation of the formula CXXXVIIb compound employing the methods and procedures described hereinabove for the preparation of the formula XXVI compound from the formula XXI compound.
Finally following the procedure of Chart A the formula CXLIV compound is transformed to the formula CXLV compound and thereafter the formula CXLV compound (following the procedure of Charts A-F) is transformed to the formula CXVI and formula CXLVII compounds.
Chart N provides a method whereby PGA-type compounds are transformed into corresponding 11-deoxy PGE-type compounds, according to formula CLII or CLVI.
The formula CLII compound is prepared from the formula CLI compound by selective catalytic hydrogenation of the cyclopentene ring olefin unsaturation. This transformation is selectively effected without affecting sidechain unsaturation. For this purpose a 5 to 10 percent palladium or rhodium catalyst on carbon, alumina or other suitable support is employed. The reaction is carried out in any suitable organic solvent, e.g. ethyl acetate, methanol, ethanol, or diethyl ether at temperatures of -30° to +50° C. and pressures greater than or equal to the atmospheric pressure, but less than several atmospheres.
The formula CLIII compound is prepared from the formula CLI compound by replacing any free hydroxy hydrogen with a blocking group, according to R 31 .
This blocking group function prevents attack on the hydroxy by subsequent reagents, especially the reagent employed herein for the transformation of the C-9 hydroxy to a C-9 oxo group. This blocking group further functions so as to be replaceable by hydrogen or a later stage in the preparation of the prostaglandin-type products. Blocking groups, according to R 31 , which are useful for these purposes include alkanoyl of 2 to 12 carbon atoms, inclusive, tetrahydropyranyl, tetrahydrofuranyl, a group of the formula
--C(R.sub.11) (OR.sub.12)--CH(R.sub.13) (R.sub.14),
wherein R 11 , R 12 , R 13 , and R 14 are as defined above, and a silyl group of the formula --Si(G 1 ) 3 , wherein G is alkyl of one to 4 carbon atoms, inclusive, phenyl, phenyl substituted with one or 2 fluoro, chloro, or alkyl of one to 4 carbon atoms, inclusive, or aralkyl of 7 to 12 carbon atoms, inclusive.
The transformations of Chart N which involve replacing any hydroxy hydrogen with a blocking group according to R 31 employ methods known in the art. Further subsequent hydrolysis of these blocking groups according to R 31 proceeds by methods known in the art.
When the blocking group is of the formula
--C(R.sub.11) (OR.sub.12)----CH(R.sub.13)(R.sub.14),
wherein R 11 , R 12 , R 13 , and R 14 are as defined above, the appropriate reagent is a vinyl ether, e.g. isobutyl vinyl ether or any vinyl ether of the formula
C(R.sub.11) (OR.sub.12) =C(R.sub.13) (R.sub.14),
wherein R 11 , R 12 , R 13 , and R 14 are as defined above; or an unsaturated cyclic or heterocyclic compound, e.g. 1-cyclohexen-1-yl methyl ether or 5,6-dihydro-4-methoxy-2H-pyran. See C. B. Reese, et al., Journal of the American Chemical Society 89, 3366 (1967). The reaction conditions for such vinyl ethers and unsaturates are similar to those for dihydropyran above.
The subsequent hydrolysis of these blocking groups according to R 31 proceeds by methods known in the art. Silyl groups are readily removed by prior art procedures known to be useful for transforming silyl ethers and silyl esters to alcohols and carboxylic acids, respectively. For reference see Pierce, cited above, especially page 447 thereof. A mixture of water and a sufficient quantity of a water miscible organic diluent to yield the homogeneous reaction mixture represents a suitable reaction medium. Addition of a catalytic amount of an organic or inorganic acid hastens the hydrolysis. The length of time required for hydrolysis is determined in part by temperature. With a mixture of water and methanol at 25° C. several hours is usually sufficient for hydrolysis. At 0° C., several days are required.
For the hydrolysis of the various other blocking groups according to R 31 mild acidic conditions are employed.
The formula CLIV compound is prepared from the formula CLIII compound by reduction of the formula CLIII compound with reducing agent which selectively effects reduction of the ring unsaturation and reduction of the C-9 oxo group to a C-9 hydroxy group, without reducing side chain unsaturation. For this purpose an alkali metal borohydride, e.g. sodium, potassium, or lithium borohydride is effectively employed in aqueous solution. The reaction is carried at about -20° C. and is complete within a few minutes.
The formula CLV compound is prepared by oxidation of the formula CLIV compound using an oxidizing reagent, such as the Jones reagent (acidified chromic acid). See for reference Journal of the Chemical Society 39 (1946). A slight stoichiometric excess beyond the amount necessary to oxidize a single hydroxy group is employed. Acetone is a useful diluent for this purpose. Reaction temperatures at least as low as about 0° C. should be used. Preferred reaction temperatures are in the range of -10° to -50° C. An especially useful reagent for this purpose is the Collins reagent (chromium trioxide in pyridine). See for reference J. C. Collins, et al., Tetrahedron Letters 3363, (1968). Dichloromethane is a suitable diluent for this purpose. Reaction temperatures below 30° C. are preferred. Reaction temperatures in the range of -10° to +10° C. are especially preferred. This oxidation proceeds rapidly and is complete within several minutes. The formula CLV compound may then be isolated by conventional methods, e.g. silica gel chromatography.
Examples of other oxidation reagents useful for this transformation are silver carbonate on celite (Chemical Communications 1102 (1969)), mixtures of chromium trioxide in pyridine (Journal of the American Chemical Society 75, 422 (1953)), and Tetrahedron Letters, 18, 1351 (1962)), tert-butyl chromate in pyridine (Biological Chemical Journal, 84, 195 (1962)), mixtures of sulfur trioxide in pyridine and dimethyl sulfoxide (Journal of the American Chemical Society 89, 5505 (1967)), and mixtures of dicyclohexylcarbodiimide and dimethyl sulfoxide (Journal of the American Chemical Society 87, 5661 (1965)).
The formula CLVI compound is then prepared from the formula CLV compound by hydrolysis of the blocking groups, according to R 31 , as described above.
From the formula CLVI 11-deoxy-PGE-type compound, there is prepared the corresponding 11-deoxy-PGF.sub.α- or PGF.sub.β-type compound. Further, employing the 8β,12α-PGA-type compound corresponding to the formula CXLVI PGA-type compound, there are prepared the corresponding 8β,12α-11-deoxy-PGE-, PGF.sub.α-, or PGF.sub.β-type products.
Chart O provides a method whereby the formula CLXI, 8β,12α-PGA-type compound is transformed to the formula CLXVII 8β,12α-PGF.sub.α-, PGF.sub.β-, or PGE-type compounds.
The formula CLXI compound is prepared hereinabove. The formula CLXII compound is then prepared from the formula CLXI compound by the procedure described hereinabove for the preparation of the formula CLIII compound from the formula CLI compound. Thereafter the formula CLXIII compound, the formula CLXIV compound, formula CLXV compound, and formula CLXVI compound are successively prepared from the formula CLXII compound employing methods known in the art. See for reference Belgian Pat. No. 804,873, Derwent Farmdoc CPI No. 22865V/13, and G. L. Bundy et al., J. Am. Chem. Soc. 94, 2123 (1972). There are first formed the formula CXLIII 10,11-epoxides, using any agent known to epoxidize an α,β-unsaturated ketone without reacting with isolated carbon-carbon double bonds, for example see Steroid Reactions, Carl Djerassi, ed., Holden-Day Inc., 1963, p. 593. Especially preferred are aqueous hydrogen peroxide or an organic tertiary hydroperoxide. See, for example, Organic Peroxides, A. V. Tobolsky et al., Interscience Publishers, N. Y., 1954. For this purpose, the peroxide or hydroperoxide is employed in an amount of at least one equivalent per mole of formula CLXII reactant in the presence of a strong base, e.g., an alkali metal hydroxide, a metal alkoxide, or a quaternary ammonium hydroxide. For example, there is employed lithium hydroxide, sodium hydroxide, potassium hydroxide, lithium ethoxide, lithium octyloxide, magnesium methoxide, megnesium isopropoxide, benzyltrimethylammonium hydroxide, and the like.
It is advantageous to use an inert liquid diluent in the epoxidation step to produce a mobile homogeneous reaction mixture, for example, a lower alkanol, dioxane, tetrahydrofuran, dimethoxyethane, dimethylsulfoxide, or dimethylsulfone. A reaction temperature in the range -60° to 0° C. is generally preferred, especially below -10° C. At a temperature of -20° C., the epoxidation is usually complete in 3 to 6 hours. It is also preferred that the reaction be carried out in an atmosphere of an inert gas, e.g., nitrogen, helium, or argon. When the reaction is complete as shown by the absence of starting material on TLC plates (5% acetone in dichloromethane), the reaction mixture is neutralized, and the epoxy product is isolated by procedures known in the art, for example, evaporation of the diluent and extraction of the residue with an appropriate waterimmiscible solvent, e.g., ethyl acetate.
This transformation of CLXII to CLXIII usually produces a mixture of formula CLXIII alpha and beta epoxides. Although these mixtures are separable into the individual alpha and beta isomers, for example, by chromatography by procedures known to be useful for separating alpha and beta epoxide mixtures, it is usually advantageous to transform the formula CLXIII mixture of alpha and beta epoxides to the corresponding mixture of formula CLXIV IIα- and IIβ- hydroxy compounds. The latter mixture is then readily separated into the IIα and IIβ compounds, for example, by chromatography on silica gel.
Referring again to Chart O, the transformation of epoxide CLXIII to hydroxy compound CLXIV is accomplished by reduction with chromium (II) salts, e.g., chromium (II) chloride or chromium (II) acetate. Those salts are prepared by methods known in the art. This reduction is carried out by procedures known in the art for using chromium (II) salts to reduce epoxides of α,β-unsaturated ketones to β-hydroxy ketones. See, for example, Cole et al., J. Org. Chem. 19, 131 (1954), and Neher et al., Helv. Chem. Acta 42, 132 (1959). In these reactions, the absence of air and strong acids is desirable.
Amalgamated aluminum metal has also been found to be useful as a reducing agent in place of chromium (II) salts for the above purpose. Amalgamated aluminum is prepared by procedures known in the art, for example, by contacting aluminum metal in the form of foil, thin sheet, turnings, or granules with a mercury (II) salt, for example, mercuric chloride, advantageously in the presence of sufficient water to dissolve the mercury (II) salt. Preferably, the surface of the aluminum metal is free of oxide. That is readily accomplished by physical removal of the usual oxide layer, e.g., by abrasion or scraping, or chemically, e.g., by etching with aqueous sodium hydroxide solution. It is only necessary that the aluminum surface be amalgamated. The amalgamated aluminum should be freshly prepared, and maintained in the absence of air and moisture until used.
The reductive opening of the formula CLXIII epoxide ring is accomplished by contacting said epoxide with the amalgamated aluminum in the presence of a hydroxylic solvent and sufficient inert organic liquid diluent to give a mobile and homogeneous reaction mixture with respect to the hydroxylic solvent and said epoxide. Among hydroxylic solvents, water is especially preferred although lower alkanols, e.g., methanol and ethanols are also operable.
Examples of inert organic liquid diluents are normally liquid ethers such as diethyl ether, tetrahydrofuran, dimethoxyethane, diglyme (dimethyl ether of diethylene glycol), and the like. Especially preferred is tetrahydrofuran. When a water-immiscible liquid diluent is used, a mixture of water and methanol or ethanol is especially useful in this reaction since the latter two solvents also aid in forming the desired homogeneous reaction mixture. For example, a mixture of diethyl ether and water is used with sufficient methanol to give a homogeneous reaction mixture. Thereafter the formula CLXV compound is prepared from the formula CLXIV compound by separating the 11α-hydroxy epimer from the 11- epimeric mixture. Thereafter, the formula CLXVI compound is prepared from the formula CLXV compound by removal of the blocking groups, using methods described in Chart N wherein the formula CLV compound is transformed to the formula CLV compound. Thereafter, the formula CLXVII compound is prepared from the formula CLXVI compound using the procedures described herein in Chart F, i.e. the preparation of the formula LXXIII compound from the formula LXXII compound.
Optionally, the procedure of Chart O is followed, except that 13,14 -didehydro-8β, 12α-PGA-type starting material is used in place of 14-halo-8β,12α-PGA-type starting material and according 13,14-dihydro-PG-type products are prepared. Thus the procedure of Chart O is followed except that in place of the Y 2 moiety in the formulas of Chart O, the Y 1 moiety is present.
Chart P provides a method whereby the formula CLXXl PGF.sub.α or 11-deoxy-PGF.sub.α -type starting material, as prepared herein, is transformed into the corresponding PGE -type compound by selective silylation of all hydroxy hydrogens of the formula CLXXl compound, other than the C-9 hydroxy.
The formula CLXXll compound is prepared from the formula CLXXl compound by selective silylation of the various hydroxy groups of the formula CLXXl compound over the C-9 hydroxy. Silyl groups with the scope --Si(G 1 ) 3 , wherein G is alkyl of 1 to 4 carbon atoms, inclusive, aralkyl of 7 to 12 carbon atoms, inclusive, phenyl, phenyl substituted with one or 2 chloro, fluoro, or alkyl of one to 4 carbon atoms, inclusive, with the proviso that the various G's of the --Si(G) 3 moiety are the same or different, are employed. These reagents are known in the art and their use is known in the art.
For the selective silylation procedure of Chart P procedures known in the art for selective silylation of known prostanoic acid derivatives are employed. See for reference U.S. Pat. No. 3,822,303 (issued July 2, 1974), German Offenlegungschrift 2,259,195 (Derwent Farmdoc CPl 36457U-B), and Netherlands Pat. No. 7,214,142 (Derwent Farmdoc CPl 26221U-B).
Examples of the --Si(G 1 ) 3 moiety are trimethylsilyl, dimethyl(tert-butyl)silyl, dimethyl phenyl silyl, and methylphenylsilyl. Examples of alkyl of one to 4 carbon atoms, inclusive, aralkyl of 7 to 12 carbon atoms, inclusive, and phenyl or substituted phenyl moieties are provided hereinabove.
The formula CLXXlll compound is prepared from the formula CLXXll compound by oxidation of the C-9 hydroxy to a C-9 oxo. Oxidation reagents and methods known in the art are employed. For example, the Jones reagent is advantageously employed as discussed above.
The formula CLXXIV compound is prepared from the formula CLXXIII compound by hydrolysis of the silyl groups. Hydrolysis proceeds by methods known in the art, e.g. the use of water or dilute aqueous acetic acid in a diluent of water and a quantity of a water miscible solvent sufficient to yield a homogeneous reaction mixture. This hydrolysis is ordinarily complete within 2 to 12 hours at 25° C., and is preferably carried in an atmosphere of an inert gas such as nitrogen or argon.
Optionally the procedure of Chart P is used to transform 13,14-didehydro-PGF.sup.θ-type products to corresponding 13,14-didehydro-PGE-type products. Accordingly, in this alternate process Y 2 in this Chart is defined to be --C.tbd.C-- instead of trans-CH=C(Hal)-.
Chart R provides a method whereby the 14-halo compounds described herein are transformed corresponding 13,14-dihydro-PG-type products.
The transformation of Chart R (the formula CLXXXI compound to the formula CLXXII compound) proceeds by dehydrohalogenation. By the preferred method the reaction proceeds using as a reaction diluent a mixture of dimethylsulfoxide, or similar aprotic solvent, and methanol in ratio by volumn between 5:1 and 10:1. Thereafter a strong organic base, for example potassium t-butoxide or sodium methoxide is added and the reaction is allowed to proceed to completion, ordinarily within about 24 hours. Reaction temperatures between 0°-25° C. are employed for convenience.
When this dehydrohalogenation procedure is employed using PGE- or PGA-type compounds or 8β,12α-PGE- or PGA-type compounds undesired dehydration and/or double bond migration occurs. Accordingly, it is preferred that these dehydrations be performed on PGF-type reactants and thereafter the corresponding 13,14-didehydro-PGF-type compounds be transformed respectively to 13,14-didehydro-PGE- or PGA-type products, by procedures described hereinabove. Accordingly, by this preferred method the 14-halo-PGF compound is successively transformed to a 13,14-didehydro-PGF-type compound and thereafter to 13,14-didehydro-PGE- or PGA-type compounds.
Optically active PG-type products are obtained from optically active intermediates, according to the process steps of the above charts. Likewise optically active PG-type compounds are obtained from corresponding optically active PG-type compounds following the procedures in the above charts. When racemic intermediates are used in the reactions above, racemic products are obtained. These products may be used in their racemic form or if preferred they may be resolved as optically active enantiomers following procedures known in the art. For example when a PG-type free acid is obtained, the racemic form thereof is resolved into d and 1 forms by reacting said free acid by known procedures with an optically active base (e.g., brucine or strychnine) thereby yielding a mixture of 2 diastereomers which are separable by procedures known in the art (fractional crystallization to yield the separate diastereomeric salts). The optically active acid may then be prepared from the salt by general procedures known to the art.
In all of the above described reactions, the products are separated by conventional means from starting material and impurities. For example, by use of silica gel chromatography monitored by thin layer chromatography the products of the various steps of the above charts are separated from the corresponding starting materials and impurities.
As discussed above, the processes herein described lead variously to acids (R 1 is hydrogen) or to esters.
When the alkyl ester has been obtained and an acid is desired, saponification procedures, as known in the art for PGF-type compounds are employed.
For alkyl esters of PGE-type compounds enzymatic processes for transformation of esters to their acid forms may be used by methods known in the art when saponification procedures would cause dehydration of the prostaglandin analog. See for reference E. G. Daniels, Process For Producing An Esterase, U.S. Pat. No. 3,761,356.
When an acid has been prepared and alkyl, cycloalkyl, or aralkyl ester is desired, esterification is advantageously accomplished by interaction of the acid with the appropriate diazohydrocarbon. For example, when diazomethane is used, the methyl esters are produced. Similar use of diazoethane, diazobutane, and 1-diazo-2-ethylhexane, and diazodecane, for example, gives the ethyl, butyl, and 2-ethylhexyl and decyl esters, respectively. Similarly, diazocyclohexane and phenyldiazomethane yield cyclohexyl and benzyl esters, respectively.
Esterification with diazohydrocarbons is carried out by mixing a solution of the diazohydrocarbon in a suitable inert solvent, preferably diethyl ether, with the acid reactant, advantageously in the same or a different inert diluent. After the esterification reaction is complete the solvent is removed by evaporation, and the ester purified if desired by conventional methods, preferably by chromatography. It is preferred that contact of the acid reactants with the diazohydrocarbon be no longer than necessary to effect the desired esterification, preferably about one to about ten minutes, to avoid undesired molecular changes. Diazohydrocarbons are known in the art or can be prepared by methods known in the art. See, for example, Organic Reactions, John Wiley and Sons, Inc., New York, N. Y., Vol. 8, pp. 389-394 (1954).
An alternative method for alkyl, cycloalkyl or aralkyl esterification of the carboxy moiety of the acid compounds comprises transformation of the free acid to the corresponding silver salt, followed by interaction of that salt with an alkyl iodide. Examples of suitable iodides are methyl iodide, ethyl iodide, ethyl iodide, butyl iodide, isobutyl iodide, tert-butyl iodide cyclopropyl iodide, cyclopentyl iodide, benzyl iodide, phenethyl iodide, and the like. The silver salts are prepared by conventional methods, for example, by dissolving the acid in cold dilute aqueous ammonia, evaporating the excess ammonia at reduced pressure, and then adding the stoichiometric amount of silver nitrate.
Various methods are available for preparing phenyl or substituted phenyl esters within the scope of the invention from corresponding aromatic alcohols and the free acid PG-type compounds, differing as to yield and purity of product.
Thus by one method, the PG-type compound is converted to a tertiary amine salt, reacted with pivaloyl halide to give the mixed acid anhydride and then reacted with the aromatic alcohol. Alternatively, instead of pivaloyl halide, an alkyl or arylsulfonyl halide is used, such as p-toluenesulfonyl chloride. See for example Belgian Pat. Nos. 775,106 and 776,294, Derwent Farmdoc Nos. 33705T and 39011T.
Still another method is by the use of the coupling reagent, dicyclohexylcarbodiimide. See Fieser et al., "Reagents for Organic Synthesis", pp. 231-236, John Wiley and Sons, Inc., New York, (1967). The PG-type compound is contacted with one to ten molar equivalents of the aromatic alcohol in the presence of 2-10 molar equivalents of dicyclohexylcarbodiimide in pyridine as a solvent.
One preferred novel process for the preparation of theses esters, however, comprises the steps:
a. forming a mixed anhydride with the PG-type compound and isobutylchloroformate in the presence of a tertiary amine and
b. reacting the anhydride with an appropriate aromatic alcohol.
The mixed anhydride described above is formed readily at temperatures in the range -40° to +60° C., preferably at -10° to +10° C. so that the rate is reasonably fast and yet side reactions are minimized. The isobutylchloroformate reagent is preferably used in excess, for example 1.2 molar equivalents up to 4.0 per mole of the PG-type compound. The reaction is preferably done in a solvent and for this purpose acetone is preferred, although other relatively nonpolar solvents are used such as acetonitrile, dichloromethane, and chloroform. The reaction is run in the presence of a tertiary amine, for example triethylamine, and the co-formed amine hydrochloride usually crystallizes out, but need not be removed for the next step.
The aromatic alcohol is preferably used in equivalent amounts or in substantial stoichiometric excess to insure that all of the mixed anhydride is converted to ester. Excess aromatic alcohol is separated from the product by methods described herein or known in the art, for example by crystallization. The tertiary amine is not only a basic catalyst for the esterification but also a convenient solvent. Other examples of tertiary amines useful for this purpose include N-methylmorpholine, triethylamine, diisopropylethylamine, and dimethylaniline. Although they are effectively used, 2-methylpyridine and quinoline result in a slow reaction. A highly hindered amine such as 2,6-dimethyllutidine is, for example, not useful because of the slowness of the reaction.
The reaction with the anhydride proceeds smoothly at room temperature (about 20° to 30° C.) and can be followed in the conventional manner with thin layer chromatography (TLC).
The reaction mixture is worked up to yield the ester following methods known in the art, and the product is purified, for example by silica gel chromatography.
Solid esters are converted to a free-flowing crystalline form on crystallization from a variety of solvents, including ethyl acetate, tetrahydrofuran, methanol and acetone, by cooling or evaporating a saturated solution of the ester in the solvent or by adding a miscible nonsolvent such as diethyl ether, hexane, or water. The crystals are then collected by conventional techniques, e.g. filtration or centrifugation, washed with a small amount of solvent, and dried under reduced pressure. They may also be dried in a current of warm nitrogen or argon, or by warming to about 75° C. Although the crystals are normally pure enough for many applications, they may be recrystallized by the same general techniques to achieve improved purity after each recrystallization.
The compounds of this invention prepared by the processes of this invention, in free acid form, are transformed to pharmacologically acceptable salts by neutralization with appropriate amounts of the corresponding inorganic or organic base, examples, of which correspond to the cations and amines listed hereinabove. These transformations are carried out by a variety of procedures known in the art to be generally useful for the preparation of inorganic, i.e., metal or ammonium salts. The choice of procedure depends in part upon the solubility characteristics of the particular salt to be prepared. In the case of the inorganic salts, it is usually suitable to dissolve an acid of this invention in water containing the stoichiometric amount of a hydroxide, carbonate, or bicarbonate corresponding to the inorganic salt desired. For example, such use of sodium hydroxide, sodium carbonate, or sodium bicarbonate gives a solution of the sodium salt. Evaporation of the water or addition of a water-miscible solvent of moderate polarity, for example, a lower alkanol or a lower alkanone, gives the solid inorganic salt if that form is desired.
To produce an amine salt, an acid of this invention is dissolved in a suitable solvent of either moderate or low polarity. Examples of the former are ethanol, acetone, and ethyl acetate. Examples of the latter are diethyl ether and benzene. At least a stoichiometric amount of the amine corresponding to the desired cation is then added to that solution. If the resulting salt does not precipitate, it is usually obtained in solid form by addition of a miscible diluent of low polarity or by evaporation. If the amine is relatively volatile, any excess can easily be removed by evaporation. It is preferred to use stoichiometric amounts of the less volatile amines.
Salts wherein the cation is quaternary ammonium are produced by mixing an acid of this invention with the stoichiometric amount of the corresponding quaternary ammonium hydroxide in water solution, followed by evaporation of the water.
The acids or esters of this invention prepared by the processes of this invention are transformed to lower alkanoates by interaction of a free hydroxy compound with a carboxyacylating agent, preferably the anhydride of a lower alkanoic acid, i.e., an alkanoic acid of two to 8 carbon atoms, inclusive. For example, use of acetic anhydride gives the corresponding acetate. Similar use of propionic anhydride, isobutyric anhydride, or hexanoic anhydride gives the corresponding carboxyacylate.
The carboxyacylation is advantageously carried out by mixing the hydroxy compound and the acid anhydride, preferably in the presence of a tertiary amine such as pyridine or triethylamine. A substantial excess of the anhydride is used, preferably about 10 to about 10,000 moles of anhydride per mole of the hydroxy compound reactant. The excess anhydride serves as a reaction diluent and solvent.
An inert organic diluent (e.g., dioxane) can also be added. It is preferred to use enough of the tertiary amine to neutralize the carboxylic acid produced by the reaction, as well as any free carboxyl groups present in the hydroxy compound reactant.
The carboxyacylation reaction is preferably carried out in the range about 0° to about 100° C. The necessary reaction time will depend on such factors as the reaction temperature, and the nature of the anhydride and tertiary amine reactants. With acetic anhydride, pyridine, and a 25° C. reaction temperature, a 12 to 24 hour reaction time is used.
The carboxyacylated product is isolated from the reaction mixture by conventional methods. For example, the excess anhydride is decomposed with water, and the resulting mixture acidified and then extracted with a solvent such as diethyl ether. The desired carboxyacylate is recovered from the diethyl ether extract by evaporation. The carboxyacylate is then purified by conventional methods, advantageously by chromatography or crystallization.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The invention can be more fully understood by the following examples and preparations.
All temperatures are in degrees centigrade.
IR (infrared) absorption spectra are recorded on a Perkin-Elmer Model 421 infrared spectrophotometer. Except when specified otherwise, undiluted (neat) samples are used.
UV (Ultraviolet) spectra are recorded on a Cary Model 15 spectrophotometer.
NMR (Nuclear Magnetic Resonance) spectra are recorded on a Varian A-60, A-60D, and T-60 spectrophotometer on deuterochloroform solutions with tetramethylsilane as an internal standard (downfield).
Mass spectra are recorded on an CEC model 21-110B Double Focusing High Resolution Mass Spectrometer on an LKB Model 9000 Gas-Chromatograph-Mass Spectrometer. Trimethylsilyl derivatives are used, except where otherwise indicated.
The collection of chromatographic eluate fractions starts when the eluant front reaches the bottom of the column.
"Brine", herein, refers to an aqueous saturated sodium chloride solution.
The A-IX solvent system used in thin layer chromatography is made from ethyl acetate-acetic acid-cyclohexane-water (90:20:50:100) as modified from M. Hamberg and B. Samuelsson, J. Biol. Chem. 241, 257 (1966).
Skellysolve-B (SSB) refers to mixed isomeric hexanes.
Silica gel chromatography, as used herein, is understood to include elution, collection of fractions, and combination of those fractions shown by TLC (thin layer chromatography) to contain the pure product (i.e., free of starting material and impurities).
Melting points (MP) are determined on a Fisher-Johns or Thomas-Hoover melting point apparatus.
DDQ refers to 2,3-dichloro-5,6-dicyano -1,4-benzoquinone. THF refers to tetrahydrofuran. Specific Rotations, [α], are determined for solutions of a compound in the specified solvent at ambient temperature with a Perkin-Elmer Model 141 Automatic Polarimeter.
EXAMPLE 1
Dimethyl 3,3-dimethyl-2-oxo-4-phenylbutylphosphonate, ##STR83##
A. To a solution of 101.2 g. of diisopropylamine in 125 ml. of tetrahydrofuran under nitrogen at 0° C. is added dropwise with cooling (using an ice-methanol bath) 625 ml. of 1.6M n-butyllithium in hexane. To the resulting solution is added dropwise with cooling 46.5 ml. of isobutyric acid. This mixture is then stirred at 0° C. for 90 min. and thereafter cooled to -15° C. Benzyl chloride (60 ml.) is added with stirring at such a rate as to maintain the reaction temperature below -5° C. The resulting mixture is thereafter stirred at ambient temperature for 4 hours. This stirred mixture is then diluted with diethyl ether and excess cold dilute hydrochloric acid. The organic layer is washed with saline and thereafter dried, concentrated, and the residue distilled under vacuum. Accordingly, there is prepared 2,2-dimethyl-3-phenyl propionic acid.
B. A mixture of 48 g. of the product of part A of this example and 82 g. of thionyl chloride are heated with stirring on a steam bath for 2 hours. The mixture is then concentrated under vacuum. Thereafter dry benzene is added and the resulting mixture is concentrated again, removing all traces of thionyl chloride. Distillation of this residue yields 48.2 g. of 2,2-dimethyl-3-phenyl-propionyl chloride.
C. To a solution of 63 g. of dimethylmethylphosphonate in 600 ml. of tetrahydrofuran under nitrogen at -75° C. is added with stirring 312 ml. of 1.6 molar n-butyllithium in hexane. The addition rate is adjusted so that the reaction temperature remains below 55° C. Ten minutes after the addition is complete, 48.2 g. of the reaction product of part B of this example and 50 ml. of tetrahydrofuran are added dropwise at such rate as to maintain the reaction temperature below -60° C. The resulting mixture is then stirred at -75° C. for 2 hours and then ambient temperature overnight. Acetic acid (20 ml.) is thereafter added and the resulting mixture distilled under vacuum, thereby removing most of the tetrahydrofuran. The residue is then shaken with diethyl ether in methylene chloride (3:1 by volume) and a cold dilute sodium bicarbonate solution. The organic layer is then washed with brine, dried, and concentrated. The residue was crystallized from diethyl ether, yielding 54 g. of dimethyl 3,3-dimethyl-2-oxo-4-phenylbutylphosphonate the title compound. The melting point is 48°-50° C.
Following the procedure of Example 1, but using in place of benzyl chloride substituted benzyl chlorides of the formula ##STR84## wherein T is fluoro, chloro, trifluoromethyl, alkyl of one to 3 carbon atoms, inclusive, or alkoxy of one to 3 carbon atoms, inclusive, and wherein s is zero, one, 2, or 3, with the proviso that not more than two T's are other than alkyl, and with the further proviso that the various T's may be the same or different, there are prepared the corresponding dimethyl-3,3-dimethyl-2-oxo-4-(substituted phenyl)butylphosphonates. For example, there is prepared by this procedure dimethyl 3,3-dimethyl-2-oxo-4-(p-fluorophenyl)butylphosphonate.
Further, following the procedure of Example 1, but using in place of the isobutyric acid of Example 1, part A, propionic acid, there is prepared dimethyl 3-methyl-2-oxo-4-phenylbutylphosphonate. Following the procedure of Example 1, but using the substituted benzyl chlorides described above in place of benzyl chloride and propionic acid in place of isobutyric acid there are prepared the various diemthyl 3-methyl-2-oxo-4-(substituted phenyl)butylphosphonates wherein the phenyl substitution is as described above.
Further, following the procedure of Example 1, but using acetic acid in place of isobutyric acid as used in Example 1, part A, there is prepared dimethyl-2-oxo-4-phenylbutylphosphonate. Using acetic acid in combination with the various substituted benzyl chlorides described above according to the procedure of Example 1, there are prepared the various dimethyl 2-oxo-4-(substitutedphenyl)butyl phosphonates, wherein the phenyl substitution is as described above.
Following the procedure of Example 1, but using 2,2-difluoroacetic acid in place of isobutyric acid as used in part A of Example 1, there is prepared dimethyl 3,3-difluoro2-oxo-4-phenylbutylphosphonate. Further, following the procedure of Example 1, but using 2,2-difluoro acetic acid in combination with substituted benzyl chlorides described above, there are prepared the corresponding dimethyl 3,3-difluoro-2-oxo-4-(substituted) phenylbutylphosphonate, wherein the phenyl substitution is as described above.
Further, following the procedure of Example 1, but using 2-fluoro acetic acid in place of isobutyric acid there is prepared dimethyl 3-fluoro-2-oxo-4-phenylbutylphosphonate.
Using 2-fluoro acetic acid and the various substituted benzyl chlorides described above according to the procedure of Example 1, there are prepared the various dimethyl 3-fluoro-2-oxo-4-(substituted)phenylbutyl phosphonates, wherein the phenyl substitution is as described above.
EXAMPLE 2
Triphenylphosphonium salt of 2,2-difluoro-5-bromopentanoic acid, Br(C 6 H 5 ) 3 P--(CH 2 ) 3 --CF 2 --COOH.
A. Methyl furoate (50.4 g.) is dissolved in 180 ml. of methanol. Thereafter 1 g. of 5 percent palladium-on-charcoal is added. This mixture is then hydrogenated at 1 to 3 atmospheres. After 45 hours 0.79 moles of hydrogen are consumed. The black mixture is then filtered through Celite using 50 ml. of methanol to wash the reaction flask and filter. Evaporation of the filtrate under reduced pressure at 40°-45° C. bath temperature yields 51 g. of a yellow oil which is thereafter distilled, collecting that fraction boiling at 32°-35° C. Thereby, methyl tetrahydrofuroate (46.7 g.) is prepared.
B. Anhydrous hydrobromic acid is bubbled through 50 ml. of acetic anhydride with cooling until a specific gravity of 1.3 is obtained. This reagent is then added to 25 g. of the reaction product of step A of this example, with exclusion of moisture while cooling and stirring. Stirring in the ice water bath is continued for 15 min.; thereafter, the mixture is allowed to stand at room temperature ture overnight. The reaction mixture is then poured into 600 g. of crushed ice and water with stirring and extracted with diethyl ether. The ether extract is washed with aqueous sodium hydroxide, dried over sodium sulfate, filtered, and thereafter evaporated under reduced pressure to yield 38 g. of a pale yellow oil, which is thereafter distilled under high vacuum, yielding 31.6 g. of methyl 2-acetoxy-5-bromopentanoate.
C. To a solution of 60 g. of the reaction product of part B of this example in 200 ml. of methanol is added 100 ml. of methanol, which is saturated with hydrobromic acid at 0° C. and 1.3 specific gravity before the addition. The reaction mixture is then allowed to stand at room temperature overnight. The solvent is thereafter evaporated under reduced pressure at 35° C. bath temperature and 400 ml. of toluene is thereafter added. The solvent is again evaporated. This residue is then dissolved in 2 1. of ethyl acetate, washed with 5 percent aqueous sodium hydroxide solution and sodium chloride solution before being dried over sodium sulfate. Filtration and evaporation of the solvent under reduced pressure at 45° C. yields 42 g. of oil which is distilled under high vacuum, yielding 28.8 g. of methyl 2-hydroxy-5-bromopentanoate.
D. To a solution of 34.4 g. of the reaction product of part C of this example and 400 ml. of acetone is added with stirring and cooling 75 ml. of Jones reagent (26.73 g. of CrO 3 in 23 ml. of concentrated sulfuric acid, diluted to 100 ml. with water) at such a rate that the reaction temperature is maintained between 30° and 40° C. The reaction is complete in approximately 20 min. Thereafter the reaction mixture is stirred for 1.5 hr. Thereafter 150 ml. of isopropyl alcohol are slowly added with stirring during 30 min. The reaction mixture is then diluted with 1.8 l. of water and extracted with 2.4 l. of methylene chloride. These extracts are washed with brine and dried with sodium sulfate. Filtration and evaporation of the solvent under reduced pressure yields 30.8 g. of a pale yellow oil, containing methyl 2-oxo-5-bromopentanoate. This oil is used in the following steps of this example without further purification.
E. With the exclusion of moisture under a nitrogen atmosphere 195 ml. of MoF 6 .sup.. BF 3 is cooled in a dry-ice acetone bath. A solution of 30.8 g. of the reaction product of step D of this example and 40 ml. of methylene chloride is added dropwise with stirring over a period of 15 min. The reaction temperature is maintained between -35° and -45° C. Stirring the dry ice acetone bath is continued for one hour, the cooling bath thereafter is removed, and the reaction mixture thereafter diluted with 200 ml. of methylene chloride and 400 ml. of water. The organic and aqueous layers are separated, the aqueous layer being extracted with methylene chloride and the combined methylene chloride extracts washed with 250 ml. of water, 250 ml. of 5 percent aqueous potassium bicarbonate, 250 ml. of brine, and thereafter dried over sodium sulfate. Filtration and evaporation of the solvent yields 31.1 g. of a dark brown oil, which when distilled under high vacuum yields methyl 2,2-difluoro-5-bromopentanoate (14 g.).
F. The reaction product of part E of this example (28 g.) is stirred in 175 ml. of aqueous hydrobromic acid (specific gravity 1.71) for 3 hours at room temperature. The reaction mixture is then cooled in an ice bath, and diluted with 1300 ml. of diethyl ether. The organic and aqueous layers are separated and the aqueous layer is extracted with diethyl ether. The combined etheral solutions are washed with water and the ethereal loss solutions are backwashed with 400 ml. of ether and the combined ethereal solutions is then dried over sodium sulfate. Filtration and evaporation of the solvent yields 27.7 g. of a pale yellow oil, 2,2-difluoro-5-bromopentanoic acid, which is used in the following step of this example without further purification.
G. A mixture of 15.2 g. of the reaction product of part F of this example, 80 ml. of acetonitrile and 22 g. of triphenylphosphine are heated to reflux with stirring for 30 hours. The reaction mixture is then heated to 110° C., diluted with 160 ml. of toluene, and the mixture is allowed to cool slowly at room temperature for 12 hours with stirring. The reaction mixture is then stored at 5° C. for 24 hours. A precipitate is collected, washed with 50 ml. of toluene, and dried under vacuum at room temperature. 20.9 g. of the title compound of this example is thereby obtained.
EXAMPLE 3
(6-Carboxyhexyl)triphenylphosphonium bromide.
A mixture of 63.6 g. of 7-bromoheptanoic acid, 80 g. of triphenylphosphine, and 30 ml. of acetonitrile, is refluxed for 68 hours. Thereafter 200 ml. of acetonitrile is removed by distillation. After the remaining solution is cooled to room temperature, 30 ml. of benzene is added with stirring. The mixture is then allowed to stand for 12 hours. A solid separates which is collected by filtration, yielding 134.1 g. of product, melting point 185°-187° C.
Following the procedure of Example 3, but using 3-bromopropionic acid, 4-bromobutanoic acid, 5-bromopentanoic acid, or 6-bromohexanoic acid, in place of 7-bromoheptanoic acid, there are prepared the corresponding (ω-carboxyalkyl)triphenylphosphonium bromides.
EXAMPLE 4
3α-Benzoyloxy-5α-hydroxy-2β-(2-chloro-3-oxo-4,4-dimethyl-trans-1-octenyl)-1α-cyclopentaneacetic acid, γ lactone (Formula XXIII: R 7 is n-butyl, R 16 is benzoyloxy, R 3 and R 4 of the L 1 moiety are methyl, and Y 2 is trans-CH=C(Cl)-).
Refer to Chart A.
A. A solution of 24.3 g. of thallous ethoxide in 125 ml. of dry benzene is cooled in an ice bath, and thereafter a solution of 25.3 g. of methyl 3,3-dimethyl-2-oxo-heptylphosphonate in 75 ml. of benzene is added and thereafter rinsed with 50 ml. of benzene. The solution is stirred for 30 min. at 5° C. and thereafter 22.1 g. of crystalline 3α-benzoyloxy-5α-hydroxy-2β-carboxaldehyde-1α-cyclopentaneacetic acid, γ lactone is added rapidly. This reaction mixture is then stirred for 13 hours at ambient temperature yielding a brown solution of pH 9-10. Acetic acid (6 ml.) is added and the mixture is transferred to a beaker with 600 ml. of diethyl ether. Celite and 500 ml. of water is added, followed by the addition of 30 ml. (about 33 g.) of saturated potassium iodide. The mixture (containing a bright yellow precipitate of thallous iodide) is stirred for about 45 min., and thereafter filtered through a bed of Celite. The organic layer is then washed with water, aqueous potassium bicarbonate, and brine. Thereafter the resulting mixture is dried over magnesium sulfate and evaporated at reduced pressure, yielding 33.6 g. of an oil, which is then chromatographed on 600 g. of silica gel packed in 20 percent ethyl acetate in cyclohexane. Elution, collecting 500 ml. fractions, with 2 l. of 20 percent, 2 l. of 20 percent, 2 l. of 25 percent and 4 1. of 30 percent ethyl acetate in cyclohexane yields 20.3 g. of crude product, which upon recrystallization from 240 ml. of diethyl ether in pentane (2:1) yields 3α-benzoyloxy-5α-hydroxy-2β-(3-oxio-4,4-dimethyl-trans-1-octenyl)-1α-cyclopentaneacetic acid, γ lactone.
Alternatively this product is prepared by adding 3α-benzoyloxy-2β-carboxaldehyde-5α-hydroxy-1α-cyclopentaneacetic acid γ lactone (3 g.) in 30 ml. of dichloromethane to a solution of dimethyl 2-oxo-3,3-dimethylheptylphosphonate (6.69 g.) and sodium hydride (1.35 g.) in 15 ml. of tetrahydrofuran. The resulting reaction mixture is then stirred for 2 hours at about 25° C., acidified with acetic acid, and concentrated under reduced pressure. The residue is partitioned between dichloromethane and water, and the organic phase is concentrated. The residue is chromatographed on silica gel, eluting with ethyl acetate in Skellysolve B (1:1).
B. A solution of the reaction product of part A of this example (1.15 g.) in dioxane (35 ml.) is treated with N-chlorosuccinimide (9.7 g.) and stirred for 6 days. The resulting solution is then diluted with methylene chloride, washed with saline and a sodium sulfate solution, dried, and evaporated to yield a viscous residue. The residue in benzene is subjected to silica gel chromatography, eluting with hexane and ethyl acetate (9:1 ) whereupon pure 3α-benzoyloxy-5α-hydroxy-2β-(1,2-dichloro-3-oxo-4,4-dimethyloctyl)-1α-cyclopentaneacetic acid γ lactone is recovered (as a mixture of isomers). Thereafter the dichlorides so obtained are diluted with pyridine (20 ml.) and heated at 100° C. for 4.5 hours. The resulting solution is then diluted with diethyl ether and washed with ice cold dilute hydrochloric acid and brine. The resulting mixture is then dried and subject to silica gel chromatography, eluting with hexane and ethyl acetate (9:1), yielding 0.765 g. of pure product. NMR absorptions are observed at 0.85, 1.22, 1.0-1.9, 1.9-3.5, 4.8-5.1, 5.35, 6.28, 7.2-7.6, and 7.8-8.1 δ. The mass spectrum shows peaks at 432, 396, 376, 378, 254, and 256.
Alternatively, the reaction product of part A above (0.190 g.) in dry pyridine (5 ml.) at 0° C. is treated with freshly distilled sulfuryl chloride (0.386 g.) and the reaction is maintained for 5 hours. Thereafter additional sulfuryl chloride (0.667 g.) and pyridine (5 ml.) is added and the reaction continued for 12 hours for ambient temperature. A resulting dark solution is then diluted with methylene chloride, washed with ice cold phosphoric acid, sodium bicarbonate, dried, and evaporated. The residue is chromatographed on silica gel eluting with hexane and ethyl acetate (9:1). Pure product identical with that recovered in the preceding paragraph is obtained.
Following the procedure of Example 4, but using in place of 3α-benzoyloxy-5α-hydroxy-2β-carboxaldehyde-1α-cyclopentaneacetic acid γ lactone; 5α-hydroxy-2β-carboxaldehyde-1α-cyclopentaneacetic acid γ lactone, there is obtained 5α-hydroxy-2β-(2-chloro-3-oxo-4,4-dimethyl-trans-1-octenyl)-1.alpha.-cyclopentaneacetic acid γ lactone.
Further, following the procedure of Example 4, but using in place of dimethyl 2-oxo-3,3-dimethylheptylphosphonate, any of the various dimethyl phosphonates described hereinabove there are prepared the corresponding 3α-benzoyloxy-5α-hydroxy-1α-cyclopentaneacetic acid γ lactones or 5α-hydroxy-1α-cyclopentane-acetic acid γ lactones with a 2β-(2-chloro-3-oxo-trans-1-alkenyl)-substituent, optionally substituted, as follows:
4,4-difluorohexenyl; 4,4-difluoroheptenyl; 4,4-difluorooctenyl; 4,4-difluorononenyl; 4,4-difluorodecenyl; 4-fluorohexenyl; 4 -fluoroheptenyl; 4-fluorooctenyl, 4-fluorononenyl; 4-fluorodecenyl; 4,4-dimethylhexenyl; 4,4-dimethylheptenyl 4,4-dimethylnonenyl; 4,4-dimethyldecenyl; 4-methylhexenyl; 4-methylheptenyl; 4 -methyloctenyl; 4-methylnonenyl; 4-methyldecenyl; hexenyl; heptenyl; octenyl; nonenyl; decenyl; 5-phenylpentenyl; 5-(m-trifluoromethylphenyl)-pentenyl; 5-(m-fluorophenyl)-pentenyl; 5-(m-chlorophenyl)-pentenyl; 5-(p-trifluoromethylphenyl)-pentenyl; 5-(p-fluorophenyl)-pentenyl; 5-(p-chlorophenyl)-pentenyl; 4-methyl-5-phenylpentenyl; 4-methyl-5-(m-trifluoromethylphenyl)pentenyl; 4-methyl-5-(m-fluorophenyl)-pentenyl; 4-methyl-5-(p-trifluoromethylphenyl)-pentenyl; 4-methyl-5-(p-fluorophenyl)-pentenyl; 4-methyl-5-(p-chlorophenyl)-pentenyl; 4,4-dimethyl-5-(m-trifluoromethylphenyl)-pentenyl; 4,4-dimethyl-5-(m-fluorophenyl)-pentenyl; 4,4-difluoro-5-(m-chlorophenyl)-pentenyl; 4,4-dimethyl-5-(p-trifluoromethylphenyl)-pentenyl; 4,4-dimethyl-5-(p-fluorophenyl)-pentenyl; 4,4-dimethyl-5-(p-chlorophenyl)-pentenyl; 4-fluoro-5-phenylpentenyl; 4-fluoro-5-(m-trifluoromethylphenyl)-pentenyl; 4-fluoro-5-(m-fluorophenyl)-pentenyl; 4-fluoro-5-(m-chlorophenyl)-pentenyl; 4-fluoro-5-(p-trifluoromethylphenyl)-pentenyl; 4-fluoro-5-(p-fluorophenyl)-pentenyl; 4-fluoro-5-(p-chlorophenyl)-pentenyl; 4,4-difluoro-5-phenylpentenyl; 4,4-difluoro-5-(m-trifluoromethylphenyl)-pentenyl; 4,4-difluoro-5-(m-fluorophenyl)-pentenyl; 4,4-difluoro-5-(m-chlorophenyl)-pentenyl; 4,4-difluoro-5-(p-trifluoromethylphenyl)-pentenyl; 4,4-difluoro-5-(p-fluorophenyl)-pentenyl; 4,4-difluoro-5-(p-chlorophenyl)-pentenyl; 4-phenoxybutenyl; 4-(m-trifluoromethylphenoxy)-butenyl; 4-(p-fluorophenoxy)-butenyl; 4-(m-chlorophenoxy)-butenyl; 4-(m-trifluoromethylphenoxy)-butenyl; 4-(p-fluorophenoxy)-butenyl; 4-(p-chlorophenoxy)-butenyl; 4-methyl-4-phenoxy-butenyl; 4-methyl-4-(m-trifluoromethylphenoxy)-butenyl; 4-methyl-4-(m-fluorophenoxy)-butenyl; 4-methyl-4-(m-chlorophenoxy)-butenyl; 4 -methyl-4-(p-trifluoromethylphenoxy)-butenyl; 4-methyl-4-(p-fluorophenoxy)-butenyl; 4-methyl-4-(p-chlorophenoxy)-butenyl; 4,4-dimethyl-4-phenoxybutenyl; 4,4-dimethyl-4-(trifluoromethylphenoxy)-butenyl; 4,4-dimethyl-4-(m-fluorophenoxy)-butenyl; 4,4-dimethyl-4-(m-chlorophenoxy)-butenyl; 4,4-dimethyl-4-(p-trifluoromethylphenoxy)-butenyl; 4,4-dimethyl-4-(p-fluorophenoxy)-butenyl; 4,4-dimethyl-4-(p-chlorophenoxy)-butenyl; and the like.
PGF.sub.α, PGE, PGF.sub.β, PGA, and PGB analogs described herein are prepared from the formula XXIII compound wherein the C-3 position of the cyclopentane ring is substituted by a benzoyloxy moiety at C-3, as described above (Example 4).
Likewise, intermediates useful in preparing 11-deoxy-PGF.sub.α, 11-deoxy-PGE, and 11-deoxy-PGF.sub.β-type compounds of these disclosed are prepared as described above in and following Example 4 except the starting material employed is a 3-unsubstituted lactone; that is 5-hydroxy-2β-carboxaldehyde-1 α -cyclopentaneacetic acid γ lactone. Accordingly there are prepared 5α hydroxy-1α-cyclopentaneacetic acid γ lactones with the various 2β-side chains described following Example 4 which are useful in the same manner as the 3α-benzoyloxy compounds in the procedures of succeeding examples for preparing the 11-deoxy-PGF.sub..sub.α -, PGE-, or PGF.sub..sub.β -type compounds corresponding to the PGF.sub.α-, PGE-, and PGF.sub.β -type compounds therein prepared.
EXAMPLE 5
3α-Benzoyloxy-5α-hydroxy-2β-[2-chloro-(3R)-3-hydroxy-4,4-dimethyl-trans-1-octenyl]-1α-cyclopentaneacetic acid γ lactone (Formula XXIV: R 3 and R 4 of the L 1 moiety are methyl, R 5 and R 6 of the M 5 moiety are hydrogen, R 7 is n-pentyl, R 16 is benzoyloxy, and Y 2 is trans-CH=C(Cl) or its (3S)-hydroxy epimer.
Sodium borohydride (0.92 g.) is slowly added to a stirred suspension of 2.1 g. of anhydrous zinc chloride in 45 ml. of dimethyl ether in ethylene glycol (glyme) with ice bath cooling. The mixture is stirred for 20 hours at ambient temperature and thereafter cooled to -18° C. A solution of 0.76 g. of 3α-benzoyloxy-5α-hydroxy-2β-(2-chloro-3-oxo-4,4-dimethyl-trans-1-octenyl)-1α-cyclopentaneacetic acid γ (prepared according to Example 4) in 12 ml. of glyme is added over a period of 20 minutes. Stirring is continued for 24 hours at -20° C. and thereafter 40 ml. of water is cautiously added. The reaction mixture is warmed to room temperature, diluted with ethyl acetate, and washed twice with brine. The aqueous layers are extracted with ethyl acetate. The combined organic extracts are dried over sodium sulfate and evaporated to yield crude product, which when chromatographed on 12 g. of silica gel eluting with hexane and in ethyl acetate (3:1) yields the epimerically pure title product.
The 3R epimer exhibits ultraviolet absorptions at λ max .sup.. equals 229.5 nm. (ε 13,550). The mass spectrum shows absorption at 337, 336, 335, 217, 216, 215, 214, and 213. NMR absorptions in CDCl 3 are observed at 0.85, 0.90, 0.80-1.0, 1.0-1.5, 1.9-3.0, 3.0-3.6, 4.0, 4.7-5.5, 5.65, 7.2-7.7, and 7.8-8.2 δ.
The 3S epimer exhibits NMR absorptions in CDCl 3 at 0.86, 0.90, 0.8-1.0, 1.0-1.5, 2.1-3.0, 3.0-3.8, 4.0, 7.1-7.7, and 7.8-8.2 δ.
Following the procedure of Example 5, but using in place of the 3α-benzoyloxy-5α-hydroxy-2β-(2-chloro-3-oxo-4,4-dimethyl-trans-1-octenyl)-1α-cyclopentaneacetic acid γ lactone starting material employed therein, the various 3α-benzoyloxy-5α-hydroxy-2β(2-chloro-3-oxo-trans-1-alkenyl, trans-1-cis-5-alkadienyl, or substituted alkenyl or alkadienyl)-1α-cyclopentaneacetic acid γ lactones there are prepared the corresponding 3R or 3S hydroxy products.
Following the procedure of Example 5, but using in place of the 3α-benzoyloxy-5α-hydroxy-2-(2-chloro-3-oxo-4,4-dimethyl-trans-1-octenyl)-1α-cyclopentaneacetic acid γ lactone used therein, 5α-hydroxy-2β-(2-chloro-3-oxo-trans-1-alkenyl, trans-1-cis-5-alkadienyl, or substituted alkenyl or alkadienyl)-1α-cyclopentaneacetic acid γ lactones described following Example 4, there are prepared the corresponding 3R or 3S-hydroxy products. For example, there are obtained the above 3α-benzoyloxy-5α-hydroxy- or 5α-hydroxy- 1α-cyclopentaneacetic acid γ lactones wherein the 2β-side chain in either the 3R or 3S form consists of
2-chloro-3-hydroxy-trans-1-hexenyl;
2-chloro-3-hydroxy-trans-1-heptenyl;
2-chloro-3-hydroxy-trans-1-octenyl;
2-chloro-3-hydroxy-trans-1-nonenyl;
2-chloro-3-hydroxy-trans-1-decenyl;
2-chloro-3-hydroxy-4-methyl-trans-1-octenyl;
2-chloro-3-hydroxy-4-fluoro-trans-1-octenyl;
2-chloro-3-hydroxy-4,4-difluoro-trans-1-octenyl;
2-chloro-3-hydroxy-5-phenyl-trans-1-pentenyl;
2-chloro-3-hydroxy-5(p-fluorophenoxy)-trans-1-pentenyl;
2-chloro-3-hydroxy-5-(m-chlorophenyl)-trans-1-pentenyl;
2-chloro-3-hydroxy-5-(m-trifluoromethylphenyl)-trans-1-pentenyl;
2-chloro-3-hydroxy-4,4-dimethyl-5-phenyl-trans-1-pentenyl;
2-chloro-3-hydroxy-4,4-dimethyl-5-(p-fluorophenyl)-trans-1-pentenyl;
2-chloro-3-hydroxy-4,4-dimethyl-5-(m-chlorophenyl)-trans-1-pentenyl;
2-chloro-3-hydroxy-4,4-dimethyl-5-(m-trifluoromethylphenyl)-trans-1-pentenyl;
2-chloro-3-hydroxy-4,4-difluoro-5-phenyl-trans-1-pentenyl;
2-chloro-3-hydroxy-4,4-difluoro-5-(p-fluorophenyl)-trans-1-pentenyl;
2-chloro-3-hydroxy-4,4-difluoro-5-(m-chlorophenyl)-trans-1-pentenyl;
2-chloro-3-hydroxy-4,4-difluoro-5-(m-trifluoromethylphenyl)-trans-1-pentenyl;
2-chloro-3-hydroxy-4-phenoxy-trans-1-butenyl;
2-chloro-3-hydroxy-4-(p-fluorophenoxy)-trans-1-butenyl;
2-chloro-3-hydroxy-4-(m-chlorophenoxy)-trans-1-butenyl;
2-chloro-3-hydroxy-4-(m-trifluoromethylphenoxy)-trans-1-butenyl;
2-chloro-3-hydroxy-4,4-phenoxy-trans-1-butenyl;
2-chloro-3-hydroxy-4,4-dimethyl-4-(p-fluorophenoxy)-trans-1-butenyl;
2-chloro-3-hydroxy-4,4-dimethyl-4-(m-chlorophenoxy)-trans-1-butenyl;
2-chloro-3-hydroxy-4,4-dimethyl-4-(m-trifluoromethylphenoxy)-trans-1-butenyl; and the like.
EXAMPLE 6
3α-Benzoyloxy-5α-hydroxy-2β-[2-chloro-(3R)-3-methoxy-4,4-dimethyl-trans-1-octenyl]-1α-cyclopentaneacetic acid γ lactone (Formula XXIV: R 3 and R 4 of the L 1 moiety are methyl, M 5 is ##STR85##
R 7 is n-pentyl; R 16 is benzoyloxy, and Y is trans-CH=CH=C(Cl)-) or its (3S) epimer.
Refer to Chart A. A mixture of the (3R) or (3S) reaction product of Example 5 (3.6 g.), silver oxide (4.0 g.) in 50 ml. of methyl iodide and 150 ml. of benzene is stirred and heated at reflux for 18 hours. The resulting mixture is then cooled and filtered and the filtrate concentrated. The resulting concentrate is then subjected to silica gel chromatography, and those fractions as shown by thin layer chromatography to contain pure title compound are combined, yielding respectively the 3R or 3S epimer.
For 3R epimer NMR absorptions are observed at 3.21, 3.8-4.2, 4.9-5.6, 7.25-7.7, and 7.9-8.2 δ.
Following the procedure of Example 6, but using in place of the lactone starting material therein, the various 3-hydroxy lactones described following Example 5, there are prepared the corresponding 3-methoxy products. ##STR86##
Refer to Chart A.
A solution of 18 g. of 3α-benzoyloxy-5α-hydroxy-2β-(2-chloro-3-oxo-trans-1-octenyl)-1α-cyclopentaneacetic acid γ lactone in 890 ml. of dry benzene is cooled to 9° C. under a nitrogen atmosphere. A toluene solution of trimethylaluminum (60 ml.) is added over a period of 4 min. to the resulting mixture. This mixture is then stirred for 1.5 hours at 20°-25° C. then cooled to 10° C. Thereupon 370 ml. of saturated ammonium chloride is slowly added at such a rate so as to maintain the reaction mixture at ambient temperature. After 0.5 hours the reaction mixture is diluted with ethyl acetate and water and filtered, the filter cake being washed with the ethyl acetate-water solvent. The aqueous layer is extracted with ethyl acetate and the combined organic extracts are washed with brine, dried over magnesium sulfate, and evaporated to yield crude product, which is chromatographed on one kg. of silica gel packed in 10 percent ethyl acetate and Skellysolve B. Elution with 10 to 16 percent ethyl acetate in Skellysolve B (18 l.), 28 percent ethyl acetate in Skellysolve B (8 l.) yields pure title compound or pure (3R)-epimer.
Omitting the chromatographic separation described above, the (3RS)-epimeric mixture obtained on trimethylaluminum alkylation are separated in high yield as prostaglandin-type products.
Following the procedure of Example 7, but using in place of the 2-chloro-3-oxo lactone starting material therein, the various lactones described following Example 4, there are obtained 2-chloro-3-hydroxy-3-methyl products corresponding to each of the 2-chloro-3-hydroxy products of Example 5.
EXAMPLE 8
3α-dihydroxy-2β-[2-chloro-(3R)-3-hydroxy-4,4-dimethyl-trans-1-octenyl]-1α-cyclopentaneacetaldehyde, γ lactol, bis-tetrahydropyranyl ether (Formula XXVII: R 3 and R 4 of the L 1 moiety are methyl, M 6 is ##STR87##
R 7 is n-butyl, R 18 is tetrahydropyran-2-yloxy, and Y 2 is trans-CH=C(Cl)-) and its (3S)-epimer.
Refer to Chart A.
A. A solution of 100 mg. of the reaction product of Example 5 in 20 ml. of methanol is purged with nitrogen. Thereafter, potassium carbonate (30 mg.) is added and the resulting mixture is stired at ambient temperature until thin layer chromatographic analysis shows the solvolysis to be complete (about 12 hours). The solution is then diluted with ice water and neutralized with cold, dilute phosphoric acid. The resulting mixture is then dried and evaporated under reduced pressure. The residue is then chromatographed using silica gel eluting with hexane and ethylacetate (3:2). Accordingly, 40 mg. of the deacylated lactone are prepared. NMR absorptions are observed at 0.92, 0.95, 1.1-1.6, 2.0-3.3, 4.02, 4.8-5.2, 5.57, and 5.66 δ.
B. A solution of 0.39 g. of the reaction product of part A above, in 25 ml. of methylene chloride (containing 1.2 ml. of dihydropyran and 1.2 mg. of a saturated solution of pyridine in methylene chloride) is allowed to stand for one hour at ambient temperature. Additional dihydropyran (1.2 ml.) is added and the reaction continued for 36 hours. The reaction mixture is then washed with water, aqueous sodium bicarbonate, dried, and evaporated, yielding an oil (0.371 g.), the bis-tetrahydropyranyl lactone coresponding to the lactone reaction product of part A above. NMR absorptions are observed at 0.6-1.05, 1.05-1.4, 1.4-1.9, 1.9-3.0, 3.0-4.3, 4.0, 4.3-5.2, and 5.48 δ.
C. A solution of the reaction product of part B above (0.39 g.) in 10 ml. of toluene is cooled to -70° C. and thereafter 10 ml. of 10 percent diisobutylaluminum hydride (1.64 mmoles) in toluene (10 ml.) is slowly added. The reaction mixture is then stirred at -70° C. until thin layer chromatographic analysis indicates that the reduction is complete (about 10 min.). Thereafter the cooling bath is removed and 9 ml. of a mixture of tetrhydrofuran and water (3:1) is added slowly. The reaction mixture is then stirred and allowed to warm to room temperature, and is then filtered through a cellulose bed. The filter cake is rinsed with benzene, combined organic extracts are then dried and evaporated to yield 0.40 g. of the title compound. NMR absorptions are observed at 0.7-1.05, 1.05-1.35, 1.35-1.9, 1.9-2.8, 2.8-4.2, 4.00, and 5.60 δ.
Following the procedure of Example 8, the 3α-benzoyloxy-5-hydroxy or 5-hydroxy lactones described in and following Examples 5, 6, and 7 are transformed into corresponding γ-lactols.
Following the procedure of Example 8 there is prepared from (3S) starting material, respectively:
1. 3α,5α-Dihydroxy-2β-[2-chloro-(3S)-3-hydroxy-4,4-dimethyl-trans-1-octenyl]-1α-cyclopentaneacetic γ lactone. NMR absorptions are observed at 0.92, 1.1-1.7, 1.8-3.2, 3.2-3.5, 4.0, 4.8-5.2, and 5.66 δ. The mass spectrum shows peaks at 312, 233, 232, 231, 216, and 215.
2. 3α,5α-Dihydroxy-2β-[2-chloro-(3s)-3-hydroxy-4,4-dimethyl-trans-1-octenyl]-1α-cyclopentaneacetic acid γ lactone bis-tetrahydropyranyl ether. NMR absorptions are observed at 0.6-1.05, 1.05-1.4, 1.4-2.0, 2.0-3.0, 3.0-4.4, 4.00, 4.4-5.7, and 5.48 δ.
3. 3α,5α-Dihydroxy-2β[2-chloro-(3s)-3-hydroxy-4,4-dimethyl-trans-1-octenyl]-1α-cyclopentane acetaldehyde γ lactol bis-tetrahydropyranyl ether. NMR absorptions are observed at 0.6-1.1, 1.35-1.85, 1.85-3.0, 3.2-4.3, 4.00, 4.3-5.1, and 5.58 δ.
Further following the procedure of Example 8, but using the various lactones described following Examples 5 and 7 wherein R 16 is hydrogen, there are prepared the corresponding 5α-hydroxy-1α-cyclopentaneacetaldehyde γ lactol bis-tetrahydropyranyl ethers. Further following the procedure of Example 8, parts A and B, but using as starting material the various lactones described following Example 6, wherein R 16 is hydrogen, there are prepared the corresponding 5α-hydroxy-1α-cyclopentaneacetaldehyde γ lactols.
Further following the procedure of Example 8, but using as starting material the various lactols described following Example 5 and in and following Example 7, wherein R 16 is benzoyloxy, there are prepared the corresponding 3α,5α-dihydroxy-1α-cyclopentaneacetaldehyde γ lactol bis-tetrahydropyranyl ethers. Finally, following the procedure of Example 8, but using as starting material the various lactones described in and following Example 6, wherein R 16 is benzoyloxy, there are prepared the corresponding 3α,5α-dihydroxy-1α-cyclopentaneacetaldehyde γ lactol bis-tetrahydropyranyl ethers.
EXAMPLE 9
3-Oxa-14-chloro-PGF 1 .sub.α, 11,15-bis-(tetrahydropyranyl ether), methyl ester (Formula XXXV: g is one, R 3 and R 4 of the L 1 moiety are hydrogen, M 6 is ##STR88##
R 7 is n-butyl, R 18 is tetrahydropyranyloxy, and Y 2 is trans-CH=C(Cl)-) or its 15-epimer.
Refer to Chart B.
A. 3α,5α-Dihydroxy-2β-[2-chloro-(3s)-3-hydroxy-trans-1-octenyl]-1α-cyclopentaneacetaldehyde γ-lactol, bis-tetrahydropyranyl ether, (10.0 g.) is dissolved in 150 ml. of absolute ethanol (containing 3 drops of acetic acid). To this solution is added carbethoxymethylene-triphenylphosphorane (10 g.) and the mixture is stirred at ambient temperature for 72 hours. The resulting mixture is concentrated under reduced pressure to a volume of about 35 ml., mixed with ice, and dilute sodium bicarbonate solution, and shaken with ethyl acetate. The organic phase is washed with brine, dried over magnesium sulfate, and concentrated to yield a residue. The residue is slurried in 100 ml. of diethyl ether and filtered. The filtrate is concentrated to a residue which is subjected to silica gel chromatography, eluting with 20 to 40 percent ethyl acetate in Skellysolve B. There is obtained 2,3,4-trinor-14-chloro-PGF 2 .sub.α, ethyl ester, bis(tetrahydropyranyl)ether.
B. The reaction product of step A above is mixed with the 5 percent palladium-on-charcoal catalyst (0.3 g.) in 30 ml. of ethyl acetate and hydrogenated at atmospheric pressure. When about one equivalent of hydrogen is consumed, the catalyst is filtered off and the filtrate concentrated under reduced pressure to yield 2,3,4-trino-14-chloro-PGF 1 .sub.α, ethyl ester, bis(tetrahydropyranyl)ether.
C. The reaction product of step B above (1.1 g.) in 30 ml. of diethyl ether is added with stirring to a mixture of lithium aluminum hydride (0.3 g.) in 60 ml. of diethyl ether. The addition continues over a 10 min. period. The mixture is heated at reflux for 2 hours then cooled, and treated with 0.35 ml. of water cautiously added. Thereafter 0.35 ml. of 15 percent aqueous sodium hydroxide solution is added, and thereafter one ml. of water. The solids are removed by filtration and filtrate is concentrated under reduced pressure to yield 2-decarboxy-2-hydroxymethyl-2,3,4-trinor-14-chloro-PGF 1 .sub.α, bis-tetrahydropyranyl ether.
D. The reaction product of part C above (1.7 g.) together with 15 ml. of dimethyl sulfoxide and 5 ml. of tetrahydrofuran is treated with 2.28 ml. of 1.6 molar n-butyllithium in hexane, with stirring and cooling. After 5 min. there is added 5 ml. of dimethylformamide. The resulting solution is then stirred and cooled to 0° C. Thereafter lithium chloroacetate (0.7 g.) is added. The mixture is then stirred at 0° C. for 2 hours and at about 25° C. for 22 hours. Thereafter the resulting solution is diluted with 200 ml. of ice-water, acidified with a cold solution of 3 ml. of concentrated hydrochloric acid in 50 ml. of water, and immediately extracted with dichloromethane. The organic phase is washed with cold water and brine and dried over magnesium sulfate. Accordingly, there is prepared 3-oxa-14-chloro-PGF 1 .sub.α, 11,15-bis-tetrahydropyranyl ether.
E. To the above solution is added excess ethereal diazomethane and after a few minutes the excess reagent is destroyed with acetic acid. The mixture is then washed with a mixture of sodium bicaronbate solution and brine and thereafter with brine. The resulting solution is then dried and concentrated under reduced pressure. The residue so obtained is subjected to silica gel chromatography eluting with ethyl acetate and Skellysolve B to yield the title compounds.
Following the procedure of Example 9, but using the (3R) starting material there is obtained the corresponding 15-epi product.
Following the procedure of Example 9, but using the various lactols described following Example 8, there are obtained the corresponding products. For those lactols described following Example 8, wherein the C-3 position of the cyclopentane ring is unsubstituted (R 18 is hydrogen), there are obtained the corresponding 11-deoxy products wherein the C-11 position is not etherified. When the 3-methoxy lactones described following Example 8 are employed there are obtained the corresponding 14-chloro-prostaglandin-type compounds wherein the C-15 position is methoxy-substituted.
Following the procedure of Example 9, but omitting the etherification step (part E) there are obtained the above compounds in free acid form.
Following the procedure of Example 9, but replacing lithium chloroacetate used in part D of Example 9 with lithium chloropropionate or lithium chlorobutyrate, there are obtained the corresponding 3-oxa-14-chloro-PGF 1 .sub.α -type compounds wherein g is 2 or 3. Further, using the various lactols described following Example 8, there are obtained the corresponding 3-oxa-14-chloro-PGF 1 .sub.α -type compounds wherein g is 2 or 3 when the above chloroalkanoates are substituted for lithium chloroacetate.
EXAMPLE 10
5-Oxa-14-chloro-PGF 1 .sub.α, methyl ester, 11,15-bis-(tetrahydropyranyl) ether (Formula XLIII: g is one, R 3 and R 4 of the L 1 moiety are hydrogen, M 6 is ##STR89##
R 1 is methyl, R 7 is n-butyl, R 18 is tetrahydropyranyloxy, and Y 2 is trans-CH=C(Cl)-) or its 15-epimer.
Refer to Chart C.
A. A mixture of lactol starting material of Example 9 (6.3 g.) and 50 ml. of 95 percent ethanol is treated at 0° C. with stirring with a solution of sodium borohydride in 10 ml. of water (added over a period of 1 minute). The resulting mixture is then stirred at 0° C. for 10 minutes and then shaken with 10 ml. of water, 250 ml. of ethyl acetate, and 150 ml. of brine. The organic phase is then washed with brine, dried, and concentrated under reduced pressure to yield 2-decarboxy-2-hydroxymethyl-2,3,4,5,6-pentanor -14-chloro-PGF 1 .sub.α, 11,15-bis-tetrahydropyranyl ether.
B. A solution of potassium tert-butoxide (1.77 g.) in 30 ml. of tetrahydrofuran is mixed at 0° C., with stirring, with a solution of the reaction product of part A (5.8 g.) in 30 ml. of tetrahydrofuran. The resulting mixture is then stirred at 0° C. for 5 minutes and thereafter 5 ml. of trimethyl ortho-4-bromobutyrate is added. Stirring is continued at 0° C. for 2 hours and at about 25° C. for 16 hours. To this mixture is added 30 ml. of dimethylformamide and 0.5 g. of potassium-t-butoxide. The resulting mixture is then stirred for 20 hours. Some of the solvent is then removed under reduced pressure and the residue is then shaken with water and diethyl ether and dichloro methane (3:1). The organic phase is then washed with water and brine, dried, and concentrated. The residue, containing the ortho ester, is dissolved in 6 ml. of methanol at 0° C. and treated with 15 ml. of cold water containing 2 drops of concentrated hydrochloric acid. The resulting mixture is then stirred at 0° C. for 5 minutes, shaken with 200 ml. of diethyl ether, 50 ml. of dichloromethane, and 200 ml. of brine. The organic phase is then washed with brine, dried, and concentrated under reduced pressure. The residue is subjected to silica gel chromatography, yielding the title compounds.
C. Trimethylortho-4-butyrate is prepared as follows:
Refer to S. M. McEldian, et al., Journal of the American Chemical Society 64, 1825 (1942). A mixture of 4-bromobutyronitrile (74 g.), 21 ml. of methanol, and 150 ml. of diethyl ether is treated at 0° C. with stirring, with hydrogen bromide (40 g.). The mixture is then stirred for an additional 4 hours at 0° C. and 100 ml. of hexane is added. The precipitated imino ester hydrobromide is separated from the liquid by filtration and washed with 400 ml. of diethyl ether in hexane (1:1). The imino ester salt is treated in 250 ml. of diethyl ether with 150 ml. of methanol and 25 ml. of methyl orthoformate, with stirring, at about 25° C. for 24 hours. The resulting mixture is then cooled to about 10° C. and the organic solution is separated from the ammonium bromide thereby formed. Diethyl ether (100 ml.). is then added. The resulting solution is then immediately and quickly washed wth an ice cold solution prepared from potassium carbonate (20 g.) and 300 ml. of brine. The organic phase is washed with brine, treated with 3 drops of pyridine, and dried over anhydrous magnesium sulfate. The solution is then concentrated under reduced pressure, diluted with 150 ml. of benzene, and again concentrated. The residue is then distilled to yield the title ortho-4-bromobutyrate.
Following the procedure of part C of Example 10, but using 5-bromo pentanonitrile or 6-bromo hexanonitrile there is prepared trimethylortho-5-bromo pentanoate or trimethylortho-6-bromo hexanoate.
Following the procedure of Example 10, but using the corresponding (3R) lactone, there is obtained the corresponding 15-epi-PGF 1 .sub.α -type product.
Following the procedure of Example 10, but using any of the various lactols described following Example 8, there is prepared the corresponding 5-oxa-14-chloro-PGF 1 .sub.α -type product. For those lactols wherein the C-3 position of the cyclopetane ring is unsubstituted (R 18 is hydrogen), the corresponding 11-deoxy-PGF 1 .sub.α -type product produced is not etherified at the C-11 position. For those lactols described following Example 8, wherein the C-3 position of the side chain contains a methoxy group, the corresponding 3-oxa-14-chloro-13-PGF 1 .sub.α -type product contains no tetrahydropyranyl ether at the C-15 position.
Further, following the procedure of Example 10, but using trimethylortho-5-bromopentanoate or trimethylortho-6-bromohexanoate there is prepared the corresponding 5-oxa-14-chloro-PGF 1 .sub.α -type product wherein g is 3 or 4. Likewise using the various lactosl described following Example 8, corresponding 2a-homo or 2a,2b-dihomo products are obtained.
EXAMPLE 11
4-Oxa-14-chloro-PGF 1 .sub.α 11,15-bis(tetrahydropyranyl)ether (Formula LVIII: g is one, R 3 and R 4 of the L 1 moiety are hydrogen, M 6 is ##STR90##
R 1 is hydrogen, R 7 is n-butyl, R 18 is tetrahydropyranyloxy, and Y 2 is trans-CH=C(Cl)-).
Refer to Chart D.
A. A suspension of methoxymethyltriphenylphosphonium chloride (32.4 g.) in 150 ml. of tetrahydrofuran is cooled to -15° C. To the suspension is added 69.4 ml. of n-butyllithium in hexane (1.6 molar) in 45 ml. of tetrahydrofuran. After 30 minutes there is added a solution of 3α,5α-dihydroxy-2β-[2-chloro-(3S)-3-hydroxy-trans-1-octenyl]-1α-cyclopentaneacetaldehyde γ lactol bis-(tetrahydropyranyl)-ether, (10 g.), in 90 ml. of tetrahydrofuran. The mixture is stirred for 1.5 hours while warming to 25° C. The resulting solution is thereafter concentrated under reduced pressure. The residue is partitioned between dichloromethane and water, the organic phase being dried and concentrated. This dry residue is then subjected to chromatography over silica gel eluting with cyclohexane and ethyl acetate (2:1). Those fractions as shown by thin layer chromatography to contain pure formula LII product are combined.
B. The reaction product of part A above in 20 ml. of tetrahydrofuran is hydrolyzed with 50 ml. of 66 percent aqueous acetic acid at about 57° C. for 2.5 hours. The resulting mixture is then concentrated under reduced pressure. Toluene is added to the residue and the solution is again concentrated. Finally the residue is subjected to chromatography on silica gel, eluting with chloroform and methanol (6:1). The title compound is thereby obtained by combining and concentrating fractions as shown by thin layer chromatography to contain pure product. Accordingly, there is obtained the corresponding formula LIII δ-lactol.
C. Silver oxide is prepared by the addition of silver nitrate (1.14 g.) in water (3 ml.) dropwise to a 2 normal sodium hydroxide solution (6.8 ml.). A precipitate is formed. Added to the precipitate in ice water bath is the δ lactol of part B above (1 g.) in tetrahydrofuran (4 ml). When the addition is complete, the ice bath is removed and the reaction mixture allowed to warm to ambient temperature. When the reaction is complete, as shown by thin layer chromoatography (chloroform and methanol), (9:1), impurities are removed by filtration. The filtrate is then extracted with diethyl ether. The aqueous layer is then chilled in an ice bath and acidified with 10 percent potassium bisulfate solution to pH less than 2. This aqueous mixture is then extracted with diethyl ether. The ethereal extracts are then combined, washed with brine, dried over magnesium sulfate, filtered, and evaporated under reduced pressure to yield the formula LIV lactone.
D. The formula LIV lactone prepared in part C above is then transformed to its bis-tetrahydropyranyl ether derivative following the procedure described in Example 8, part B.
E. The formula LV compound prepared in part D above is then reduced to the corresponding δ lactol bis-tetrahydropyranyl ether by the procedure described in Example 8, part C.
F. The formula LVI lactol prepared in part E above is then transformed to the corresponding formula LVII primary alcohol by the procedure described in Example 10, part A.
G. The formula LVIII compound is prepared from the formula LVII compound by etherification of the primary alcohol moiety following the procedure described in Example 10, part B, but by substituting trimethylortho-3-bromopropionate in place of trimethylortho-4-bromobutyrate.
Following the procedure of Example 11, but using the corresponding (3R) starting material in place of the (3S) starting material there is obtained the corresponding 15-epi-PGF 1 .sub.α -type product.
Following the procedure of Example 11, but using in step G, trimethyl ortho-4-bromobutyrate or ortho-5-bromopentanoate in place of trimethyl ortho-3-bromopropionate, there are obtained the corresponding formula LVIII compound wherein g is 2 or 3.
Following the procedure of Example 11, but using in place of the formula LVI lactol, the various formula XXVII lactols described following Example 8, there are obtained the corresponding 4-oxa-14-chloro-PGF 1 .sub.α -type products. Finally using the above ortho-ω-alkanoates there are prepared corresponding 2a-homo or 2a,2b-dihomo compounds.
EXAMPLE 12
cis-4,5-Didehydro-14-chloro-PGF 1 .sub.α, 11,15-bis(tetrahydropyranyl) ether (Formula LIX: g is one, R 3 and R 4 of the L 1 moiety are hydrogen, M 6 is ##STR91##
R 1 is hydrogen, R 7 is n-butyl, R 18 is tetrahydropyranyloxy, and Y 2 is trans-CH=C(Cl)-) and its 15-epimer.
Refer to Chart D.
A. Following the procedure of Example 11, parts A, B, C, D, and E there is prepared the formula LVI lactol wherein L 1 , M 6 , R 7 , R 18 , and Y 2 are as defined for the title compound.
B. 3-Carboxypropyltriphenylphosphonium bromide (prepared by heating 4-bromobutyric acid and triphenylphosphine in benzene at reflux for 18 hours, and thereafter purifying), 106 g., is added to sodiomethylsulfinylcarbanide prepared from sodium hydride (2.08 g., 57 percent) and 30 ml. of dimethylsulfoxide. The resulting Wittig reagent is combined with the formula LVI lactol of part A above and 20 ml. of dimethylsulfoxide. The mixture is stirred overnight, diluted with about 200 ml. of benzene, and washed with potassium hydrogen sulfate solution. The two lower layers are washed with dichloromethane, the organic phases are combined, washed with brine, dried, and concentrated under reduced pressure. The residue is subjected to chromatography over acid washed silica gel, eluting with ethyl acetate and isomeric hexanes (3:1). Those fractions as shown to contain the desired compound by thin layer chromatography are combined to yield pure product.
Following the procedure of Example 12, but using in place of the (3S) starting material the corresponding (3R) starting material there is obtained the corresponding 15-epi-14-chloro-PGF 1 .sub.α -type compound.
Following the procedure of Example 12, but using in place of the 3-carboxypropyltriphenylphosphonium bromide, 4-carboxybutyltriphenylphosphonium bromide, or 5-carboxypentyltriphenylphosphonium broimde, there are prepared the corresponding formula LIX compounds wherein g is 2 or 3.
Further, following the procedure of Example 12, but using in place of the formula LI starting material the various formula XXVII lactols described following Example 8, there are prepared the corresponding cis- 4,5-didehydro-14-chloro-PGF 1 .sub.α or 11-deoxy-PGF 1 .sub.α -type products.
EXAMPLE 13
14-Chloro-16,16-dimethyl-PGF 2 .sub.α, methyl ester, 11,15-bis-tetrahydropyranyl ether (Formula LXII: g is 1, R 3 and R 4 of the L 1 moiety are methyl, M 6 is ##STR92##
R 1 is methyl, R 2 is hydrogen, R 7 is n-butyl, R 18 is tetrahydropyranyloxy, and Y 2 is trans-CH=C(Cl)-) or its 15 -epimer.
Refer to Chart E.
A. Sodium hydride (0.40 g., 57 percent in mineral oil) in 20 ml. of dimethylsulfoxide, is added to 1.82 g. of 4-carboxybutyltriphenylphosphonium bromide. The reaction mixture is maintained at 20° C. with stirring for 25 min. A solution of the title compound of Example 8 (0.39 g.) in 10 ml. of toluene is added. The reaction mixture is stirred at ambient temperature for 2 hours and diluted with benzene. Potassium bisulfate (2.7 g. in 30 ml. of water) is slowly added, maintaining the reaction temperature at less than or equal to 10° C. The aqueous layer is extracted with 50 ml. of benzene and the organic extracts are washed successfully with 50 ml. of water and 50 ml. of brine before combining, drying, and evaporating. Evaporation yields semi-crystalline residue which is chromatographed on 100 g. of acid washed silica gel eluting 20 percent ethyl acetate m-hexane. Thereby 0.241 g. of the pure free acid of the title product is obtained. NMR absorptions are observed at 0.65-1.1, 1.1-1.4, 1.4-1.8, 1.8-2.6, 2.8-4.4, 4.05, 4.4-4.8, 5.2-5.75, and 6.0-6.9 δ.
B. A solution of the reaction product of part A above and 15 ml. of diethyl ether is esterified with diazomethane, used in stoichiometric excess. The crude methyl ester is chromatographed on 100 g. of silica gel packed in 2 percent acetone methylene chloride. Elution with 2-12 percent acetone in methylene chloride yields the title compound.
Following the procedure of Example 13, but using the (3R) lactol there is obtained the corresponding 15-epi-14-chloro-PGF 2 .sub.α, methyl ester, 11,15-bis-tetrahydropyranyl ether. NMR absorptions are observed at 0.7-1.1, 1.1-1.4, 1.4-1.8, 1.8-2.55, 3.15-4.2, 3.66, 4.05, 4.5-4.8, 5.2-5.8, and 5.6 δ.
Following the procedure of Example 13, but using 5-carboxypentyltriphenylphosphonium bromide or 6-carboxyhexyltriphenylphosphonium bromide in place of 4-carboxybutyltriphenylphosphonium bromide there is obtained the corresponding 2a-homo or 2a,2b-dihomo-14-chloro-PGF 2 .sub.α -type compound or its 15-epimer.
Further, following the procedure of Example 13, but using in place of 4-carboxybutyltriphenylphosphonium bromide, 4,4-difluoro-4-carboxybutyltriphenylphosphonium bromide there is obtained the corresponding 2,2-difluoro-14-chloro-PGF 2 .sub.α -type tetrahydropyranyl ether or its 15-epimer.
Further, following the procedure of Example 13, but using in place of the formula LXI lactol starting material therein one of the various lactols described following Example 8, and optional by any of the Wittig reagents described above, there are prepared the corresponding 14 -chloro or 11-deoxy-14-chloro-PGF 2 .sub.α -type products.
EXAMPLE 14
15-Methyl-14-chloro-PGF 2 .sub.α, methyl ester (Formula LXXVI: R 3 and R 4 of the L 1 moiety are hydrogen, M 1 is ##STR93##
R 1 is methyl, R 7 is n-butyl, R 8 is hydroxy, Y 2 is trans-CH=C(Cl)-), and Z 2 is cis-CG=CH(CH 2 ) 3 -) or its 15-epimer.
A. A solution of 5.7 g. of the reaction product of Example 7, 3α-benzoyloxy-5α-hydroxy-2β-[(3s)-hydroxy-3-methyl-cis-1-octenyl]-1α-cyclopentaneacetic acid γ lactone in 150 ml. of methanol is deacylated according to the rocedure of Example 8, part A, yielding of 3α,5α-dihydroxy2β-[2-chloro-(3S)-3-hydroxy-3-methyl-trans- 1-octenyl]-1αcyclopentaneacetic acid γ lactone.
A sample of the corresponding (3R) starting material is decaylated in a similar fashion, yielding the corresponding (3R) product.
B. A solution of 3.65 g. of the reaction product of part A in 150 m. of tetrahydrofuran is cooled to -60° C. Diisobutylaluminum hydride and toluene (85 ml.) is added over a period of 23 minutes at a temperature of -70° C. The reaction mixture is stirred for an additional 24 minutes. Thereafter 100 ml. of saturated aqueous ammonium chloride solution is slowly added at a temperature of -60° C. The resulting mixture is then stirred and allowed to warm to room temperature, yielding a gelatin as precipitate. This mixture is then diluted with 70 ml. of water and 150 ml. of ethyl acetate, mixed thoroughly and filtered. The filter cake is washed with water and ethyl acetate. The aqueous layer is extracted with ethyl acetate. The combined organic extracts are washed with brine, dried over sodium sulfate, and evaporated to yield the lactol corresponding to lactone starting material.
C. Following the procedure of Example 13, sodium hydride in dimethylsulfoxide is combined with 4-carboxybutyltriphenylphosphonium bromide to yield the title compound in free acid form.
The reaction product of part C above is esterified with diazomethane following the procedure described above, yielding the title compound.
Following the procedure of steps B-D above, but using the deacylated (3R)-lactone there is obtained 1. 15-epi-15-methyl-14-chloro-PGF 2 .sub.α, methyl ester.
The preparation of the above title compound or its 15-epimer is optionally accomplished following the procedure of Chart F. Accordingly, the 3(RS)-3-methyl lactone corresponding to Example 7 is prepared by omitting the chromatographic separation step therein. Thereafter, by the procedure of Example 8 the corresponding 3(RS)-3-methyl lactol is prepared. Thereafter, following the procedure of Example 13, the (15RS)-15-methyl-14-chloro-PGF 2 .sub.α -bis-tetrahydropyranyl ether, methyl ester is prepared by methyl esterification of the free acid so formed. The tetrahydropyranyl ether moieties may then be hydrolyzed and the C-15 epimers separated by chromatographic techniques.
Following the procedure of Example 14, or the optional procedure discussed above, there are prepared 15-epi-15-methyl or 15-methyl-PGF 2 .sub.α -type compounds from the corresponding lactols described following Example 8.
Further, using the compounds described in or following Examples 9, 10, 11, 12, or 13 there are prepared the corresponding 3-oxa-, 4-oxa-, 5-oxa-, or cis-4,5-didehydro-15-methyl- or 15-epi-15-methyl-14-chloro-PGF 2 .sub.α -type products.
EXAMPLE 15
15-Methyl-14-chloro-PGF 2 .sub.α (Formula LXXVI: R 3 and R 4 of the L 1 moiety are hydrogen, M 1 is ##STR94##
R 1 is hydrogen, R 7 is n-butyl, R 8 is hydroxy, Y 1 is trans-CH=C(Cl)-, and Z 2 is cis-CH=CH-(CH 2 ) 3 -) or its 15-epimer.
A solution of 2.0 g. of the reaction product of Example 14, or its 15-epimer, in 20 ml. of methanol is cooled to 0° C. The resulting mixture is thereafter treated dropwise under a nitrogen atmosphere with 12 ml. of 10 percent aqueous sodium hydroxide solution. The mixture is then allowed to warm to room temperature and stirred for 2 hours. After removal of the methanol by evaporation under reduced pressure the residue is diluted wih water and extracted with methylene chloride. The aqueous layer is then cooled with ice, treated with 24 ml. of 2 molar aqueous sodium bisulfate solution and extracted immediately with ethyl acetate. The combined organic extracts are washed with brine, dried over anhydrous sodium sulfate, and concentrated. Crude product may then be chromatographed on 150 g. of silica gel, yielding the title compound or its 15-epimer.
Following the procedure of Example 15, but using any of the 15-methyl-14-chloro-PGF.sub.α or 11-deoxy-15-methyl-14-chloro-PGF.sub.α-type methyl esters, there are prepared the corresponding free acid products.
EXAMPLE 16
14-Chloro-16,16-dimethyl-PGF 2 .sub.α methyl ester (Formula LXXVI: R 3 and R 4 of the L 1 moiety are methyl, M 1 is ##STR95##
R 1 is methyl, R 7 is n-butyl, R 8 is hydroxy, Y 1 is trans-CH=C(Cl)-, and Z 2 is cis-CH=CH-(CH 2 ) 3 -) or its 15-epimer.
Refer to Chart F.
14-Chloro-16,16-dimethyl-PGF 2 .sub.α -bis-tetrahydropyranyl ether (0.241 g.) is reacted with 20 ml. of tetrahydrofuran, water, and acetic acid (1:3:6) at 40° C. for 4 hours. Thereafter, the resulting mixture is diluted with 60 ml. of water and lyophylized. The residue is then esterified with diazomethane, quenching with ethereal acetic acid, and thereafter washing with sodium bicarbonate and brine, drying and evaporating to a residue. The chromatographed (eluting with methylene chloride and acetone, 3:1) residue yields 0.056 g. of pure product. NMR absorptions ar observed at 0.44, 0.98, 1.1-1.42, 1.42-2.6, 2.7-3.4, 3.7, 3.8-4.5, 4.04, 5.25-5.8, and 5.65 δ. The mass spectrum shows peaks at 395, 340, 331, 296, and 281. Characteristic ester IR absorptions are observed at 1550, 1577, 1760, and 3450 cm - 1 .
Using corresponding 15-epimeric starting material the corresponding 15-epimeric product is prepared.
Following the procedure of Example 16, but using as starting material any of the 11,15-bis-tetrahydropyranyl ethers, 11-tetrahydropyranyl ethers, or 15-tetrahydropyranyl esters described in and following Examples 9, 10, 11, 12, or 13, there are prepared respectively the corresponding 14-chloro-PGF 2 .sub.α -15-methyl ether, 14-chloro-PGF 2 .sub.α -, or 11-deoxy-14-chloro-PGF 2 .sub.α, 15-methyl ether or 11-deoxy-14-chloro-PGF 2 .sub.α -type compounds.
EXAMPLE 17
15-Methyl-14-chloro-PGE 2 , methyl ester, (formula LXXVI: R 3 and R 4 of the L 1 moiety and R 6 of the M 1 moiety are hydrogen, M 18 is O, R 1 and R 5 are methyl, R 7 is n-butyl, R 8 is hydroxy, Y 2 is trans-CH=C(Cl), and Z 2 is cis-CH=CH-(CH 2 ) 3 -) or its 15-epimer.
A. A solution of 15-methyl-14-chloro-PGF 2 .sub.α, methyl ester, 11,15-bis-tetrahydropyranyl ether, prepared above, in 60 ml. of acetone is cooled to -25° C. Thereupon 1.9 ml. of Jones reagent is added. The reaction mixture is then stirred for 25 minutes at -25° C. and isopropyl alcohol (1.9 ml.) is added after an additional 15 minutes at -25° C. the reaction mixture is diluted with 200 ml. of water (0° C.) and extracted with diethyl ether. Ethereal extracts are washed with 75 ml. of cold 0.1 normal potassium bicarbonate, 150 ml. of brine, dried over magnesium sulfate, and evaporated, thereby yielding 15-methyl-14-chloro-PGE 2 , methyl ester, 11,15-bis-tetrahydropyranyl ether.
B. A solution of the crude product of part A above is reacted with 16 ml. of tetrahydrofuran, water, and acetic acid (1:3:6) and allowed to stand at 40° C. for 4 hours. The resulting mixture is thereafter diluted with 120 ml. of water and freeze dried. The residue is dissolved in diethyl ether and washed with potassium bicarbonate, brine, and thereafter dried and evaporated to yield crude product. The crude product is chromatographed on 25 g. of silica gel packed in 5 percent acetone in methylene chloride. Elution with 5 to 40 percent acetone in methylene chloride yields the pure product.
Following the above procedure but using 15-epimeric starting material, the corresponding 15-epimer is prepared.
Following the procedure of Example 17, but using the various 15-methyl-14-chloro-PGF.sub.α or 11-deoxy-PGF.sub.α methyl ester, 11,15-bis-tetrahydropyranyl ethers, or 15-tetrahydropyranyl ethers, as prepared in or following Examples 9, 10, 11, 12, and 13 there are prepared the corresponding 15-methyl-14-chloro-PGE or 11-deoxy-14-chloro-PGE-type products.
EXAMPLE 18
15-Methyl-14-chloro-PGE 2 or its 15-epimer.
The title compound is prepared by enzymatic hydrolysis of the methyl ester of the reaction product of Example 17 or its 15-epimer.
The enzyme is prepared as follows:
Freshly harvested colony pieces of Plexaura homomalla (Esper), 1792, forma S (10 kg.), are chopped into pieces less than 3 cm. in their longest dimension and then covered with about 3 volumes (20 l.) of acetone. The mixture is stirred at about 25° C. for one hour. The solids are separated by filtration, washed with a quantity of acetone, air dried, and finally stored at about 20° C. as a coarse enzymatic powder.
The esterase hydrolysis then proceeds as follows:
The suspension of the esterase composition prepared above in 25 ml. of water is combined with the solution of the above indicated starting material. 8 ml. of methanol is added, and the resulting mixture is stirred at about 25° C. for 24 hours. 50 ml. of acetone is then added and the mixture is stirred briefly, filtered, and the filtrate is then concentrated under reduced pressure. The aqueous residue is then acidified to pH 3.5 with citric acid and extracted with dichloromethane. The combined extracts are concentrated under reduced pressure to yield the title acid.
Following the procedure of Example 18, but using the various methyl esters described following Example 17, the corresponding products are prepared.
EXAMPLE 19
14-Chloro-PGF 1 .sub.α, methyl ester, or its 15-epimer.
A solution of 4.8 g. of 14-chloro-PGF 2 .sub.α, methyl ester in 90 ml. of acetone and 60 ml. of benzene containing 0.75 g. of tris(triphenylphosphine)rhodium (l) chloride is shaken under hydroen atmosphere at ambient temperature at 1 to 3 atmospheres pressure for 3.5 hours. Thereafter the solvent is evaporated and the residue chromatographed on 400 g. of silica gel packed in methylene chloride eluting with one to 6 percent methanol in methylene chloride. There is recovered 0.90 g. of impure product. The above product is purified using silica gel chromatograhpy, thereby preparing pure product.
Following the above procedure, but using 15-epi-14-chloro-PGF 2 .sub.α, methyl ester, there is prepared the corresponding 15-epi-14-chloro-PGF 1 .sub.α methyl ester.
Following the procedure of Example 20, but using in place of the indicated starting material any of the PGF 2 .sub.α or 11-deoxy-PGF 2 .sub.α -type compounds described in or following Example 13, there are prepared the corresponding PGF 1 .sub.α or 11-deoxy-PGF 1 .sub.α -type products.
EXAMPLE 20
14-Chloro-PGE 1 , methyl ester, or its 15-epimer.
The title compound of this Example is prepared by oxidation of the compound of Example 19, using the procedure described in Example 17, part A.
Using the corresponding 15-epimer, there are prepared 15-epi-14-chloro-PGE 1 , methyl ester.
Following the procedure of Example 20, but using any of the 11-deoxy-PGF 1 .sub.α - or PGF 1 .sub.α -type compounds described following Example 19, there are prepared the corresponding 11-deoxy-PGE 1 - or PGE 1 -type compounds.
Accordingly, following the procedures of Examples 14-20 there are prepared the various 14-chloro-PGF 2 .sub.α -, 2,2-difluoro-PGF 2 .sub.α, 2a,2b-dihomo-PGF 2 .sub.α -, 3-oxa-PGF 1 .sub.α -, 5-oxa-PGF 1 .sub.α -, 4-oxa-PGF 1 .sub.α -, cis-4,5-didehydro-PGF 1 .sub.α -, PGF 1 .sub.α -, 2,2-difluoro-PGF 1 .sub.α -, or 2a,2b-dihomo-PGF 1 .sub.α -type compounds or the corresponding PGE-type compounds, optionally substituted at C-15 with methyl or methoxy, at C-16 with one or 2 methyl, or one or 2 fluoro, or phenoxy, or optionally substituted at C-17 with a phenyl or substituted phenyl moiety.
EXAMPLE 21
14-Chloro-16,16-dimethyl-PGF 2 .sub.β, methyl ester (Formula LXXVII: R 3 and R 4 of the L 1 moiety are methyl, M 1 is ##STR96##
R 1 is methyl, R 7 is n-butyl, R 8 is hydroxy, Y 2 is trans-CH= C(Cl)--, and Z 2 is cis-CH=CH-(CH 2 ) 3 --).
Refer to Chart F.
A solution of 0.3 g. of 14-chloro-16,16-dimethyl-PGE 2 , methyl ester, in 15 ml. of methanol is cooled to -15° C. Thereafter 16 mg. of borohydride is added. After 45 minutes, 2 ml. of 50 percent acetic acid in water is slowly added. The reaction mixture is then allowed to warm to ambient temperature and then evaporated at reduced pressure. The residue is then shaken with ethyl acetate and water. The organic phase is then washed with aqueous sodium bicarbonate, brine, and then dried and evaporated to yield crude product. A column of 25 g. of silica gel packed in ethyl acetate is eluted with 70-100 percent ethyl acetate in cyclohexane. Crude product is then rechromatographed eluting with 0.5 to 3 percent methanol in methylene chloride. Rechromatographing yields the 9β-epimer.
Using the corresponding 15-epimeric starting material the corresponding 15-epimeric product is prepared.
Following the procedure of Example 21, but using the various PGE 2 -, 11-deoxy-PGE 2 -, PGE 1 -, or 11-deoxy-PGE 1 -type compounds described in the preceding examples, there are obtained the corresponding PGF 2 .sub.β, 11-deoxy-PGF 2 .sub.β, PGF 2 .sub.β, or 11-deoxy-PGF 1 .sub.β -type compounds.
EXAMPLE 22
14-Chloro-16,16-dimethyl-PGA 2 (Formula LXXVIII: R 3 and R 4 of the L 1 moiety are methyl, M 1 is ##STR97##
R 1 is hydrogen, R 7 is n-butyl, Y 2 is trans-CH=C(Cl)--, and Z 2 is cis-CH=CH--(CH 2 ) 3 --).
Refer to Chart F.
A solution of 14-chloro-16,16-dimethyl-PGE 2 (300 mg.), 4 ml. of tetrahydrofuran, and 4 ml. of 0.5 normal hydrochloric acid is left standing at ambient temperature for 5 days. Brine and dichloromethane in ether (1:3) are added and the mixture is stirred. The organic phase is separated, dried, and concentrated. The residue is dissolved in diethyl ether and the solution is extracted with aqueous sodium bicarbonate. The aqueous phase is acidified with dilute hydrochloric acid and then extracted with dichloromethane. This extract is then dried and concentrated to yield the title compound.
Following the procedure of Example 22, but using any of the PGE 2 - or PGE 1 -type compounds described above there are respectively prepared the corresponding PGA 2 - or PGA 1 -type compounds.
EXAMPLE 23
14-Chloro-16,16-dimethyl-PGB 2 (Formula LXXIX: R 3 and R 4 of the L 1 moiety are methyl, M 1 is ##STR98##
R 1 is hydrogen, R 7 is n-butyl, Y 2 is trans-CH=C(Cl)--, and Z 2 is cis-CH=CH--(CH 2 ) 3 --).
Refer to Chart F.
A solution of 14-chloro-16,16-dimethyl-PGE 2 (200 mg.) and 100 ml. of 50 percent aqueous methanol containing about 1 g. of potassium hydroxide is kept at ambient temperature for 10 hours under nitrogen atmosphere. The resulting solution is then cooled to 10° C. and neutralized by addition of 3 normal hydrochloric acid at 10° C. This solution is then extracted repeatedly with ethyl acetate and the combined organic extracts are washed with water, then washed with brine, dried, and concentrated to yield the title compound.
Following the procedure of Example 23, but using any of the PGE 2 or PGE 1 -type compounds described in the above Examples, there are prepared the corresponding PGB 2 and PGB 1 -type compounds.
EXAMPLE 24
14-Chloro-16,16-dimethyl-PGF 2 .sub.α sodium salt.
A solution of 14-chloro-16,16-dimethyl-PGF 2 .sub.α (100 mg. in 50 ml. of water ethanol mixture (1:1) is cooled at 5° C. and neutralized with an equivalent amount of 0.1 normal aqueous sodium hydroxide solution. The neutral solution is then concentrated to a residue of the title compound.
Following the procedure of Example 24, using potassium hydroxide, calcium hydroxide, tetramethyl ammonium hydroxide, or benzyltrimethylammonium hydroxide in place of sodium hydroxide there is obtained the corresponding salts of 14-chloro-16,16-dimethyl-PGF 2 .sub.α. Likewise following the procedure of Example 24 each of the various other prostaglandin-type acids described above is transformed to the corresponding sodium, potassium, calcium, trimethylammonium, or benzyltrimethylammonium salt.
EXAMPLE 25
3-oxa-3,7-inter-m-phenylene-4,5,6-trinor-PGF 1 .sub.α (Formula XC: R 1 is hydrogen, R 3 and R 4 of the L 1 moiety are hydrogen, g is one, and R 7 is n-butyl) or 3,7-inter-m-phenylene-4,5,6-trinor-PGF 1 .sub.α.
Refer to Chart G.
A. Optically Active Bicyclo[3.1.0]-hex-2-ene-6-endo-carboxaldehyde.
Following the procedure of Preparation 1 of U.S. Pat. No. 3,711,515, racemic bicyclo[3.1.0]hex-2-ene-6-endo-carboxaldehyde is prepared from bicyclo[2.2.1]hepta-2,5-diene and peracetic acid.
The racemic compound is resolved by the procedure of Example 13 of U.S. Pat. No. 3,711,515, forming an oxazolidine as follows:
Racemic bicyclo[3.1.0]hex-2-ene-6-endo-carboxaldehyde (12.3g.) and 1-ephedrine (16.5 g.) are dissolved in about 150 ml. of benzene. The benzene is removed under vacuum and the residue taken up in about 150 ml. of isopropyl ether. The solution is filtered, then cooled to -13° C. to yield crystals of 2-endo-bicyclo[3.1.0]hex-2-en-6-yl-3,4-dimethyl-5-phenyl-oxazolidine, 11.1 g., m.p. 90°-92° C. Three recrystallizations from isopropyl ether, cooling each time to about -2° C., yield crystals of the oxazolidine, 2.2 g., m.p. 100°-103° C., now substantially a single isomeric form as shown by NMR.
The above re-crystallized oxazolidine (1.0 g.) is dissolved in a few ml. of dichloromethane, charged to a 20 g. silica gel column and eluted with dichloromethane. The silica gel is chromatograph-grade (Merck), 0.5-0.2 mm. particle size, with about 4-5 g. of water per 100 g. Fractions of the eluate are collected, and those shown by thin layer chromatography (TLC) to contain the desired compound are combined and evaporated to an oil (360 mg.). This oil is shown by NMR to be the desired title compound, substantially free of the ephedrine, in substantially a single optically-active isomeric form. Points on the circular dichroism curve are (λ in nm., θ). 350, 0; 322.5, 4.854; 312, -5,683; 302.5, -4,854; 269, 0; 250, 2,368; 240, 0; and 210, -34,600.
B. 1-Bicyclo[3.1.0]hex-2-ene-6-endo-carboxaldehyde Neopentyl Glycol Acetal (Formula LXXXI: R 55 and R 56 taken together are --CH 2 --C(CH 3 ) 2 --CH 2 -- and ˜ is endo).
A mixture of 2,2-dimethyl-1,3-propanediol (900 g.), 5 l. of benzene, and 3 ml. of 85 percent phosphoric acid is heated at reflux. To it is added, in 1.5 hours, a solution of optically active bicyclo[3.1.0]hex-2-ene-6-endo-carboxaldehyde (part A, 500 g.) in 1 liter of benzene. Provision is made to take off azeotropically distilled water with a Dean-Stark trap. After 3 hours the mixture is cooled and extracted with 2 liters of 5 percent sodium bicarbonate. The organic phase is dried over sodium sulfate and concentrated under reduced pressure. The resulting semisolid residue is taken up in methanol and recrystallized, using a total of 1200 ml. of methanol to which 600 ml. of water is added, then chilled to -13° C. to yield 300 g. of the title compound, m.p. 52°-55° C., and having NMR peaks at 0.66, 1.20, 0.83-2.65, 3.17-3.8, 3.96, and 5.47-5.88 δ, [α] D -227° (C= 0.8976 in methanol), and R f 0.60 (TLC on silica gel in 25 percent ethyl acetate in mixed isomeric hexanes). Further work-up of the mother liquors yields 50-100 g. of additional product.
C. d-8-(m-Acetoxyphenyl)-7-oxa-tricyclo-[4.2.0.0 2 ,4 ]-octene-6-endo-carboxaldehyde Neopently Glycol Acetal (Formula LXXXII R 55 and R 56 taken together are --CH 2 --C(CH 3 ) 2 --CH 2 --, R 63 is ##STR99## and ˜ is endo).
A solution of the formula LXXXI l-bicyclo[3.1.0]hex-2-ene-6-endo-carboxaldehyde neopentyl glycol acetate (Part B, 5.82 g.) and m-acetoxy-benzaldehyde (1.64 g.) in 25 ml. of benzene is charged to a Pyrex photolysis vessel equipped with an immersible water-cooled cold-finger and a fritted gas inlet tube. Dissolved oxygen is removed by bubbling nitrogen through the solution. The mixture is then irradiated at 350 nm. with a Rayonet Type RS Preparative Photochemical Reactor (The Southern New England Ultraviolet Co., Middletown, Conn.) equipped with six RUL 3500 A lamps. After 24 hours the photolysate is concentrated under reduced pressure to a pale yellow oil, 10 g., which is subjected to silica gel chromatography. Elution with 10-70 percent ethyl acetate in Skellysolve B (mixture of isomeric hexanes) yields separate fractions of the recovered starting materials and the formula LXXXII title compound, a pale yellow oil, 0.86 g., having NMR peaks at 0.68, 1.20, 0.8-2.5, 2.28, 2.99, 3,12-3.88, 3.48, 4.97-5.52, and 6.78-7.60 δ; infrared absorption bands at 3040, 2950, 2860, 2840, 1765, 1610, 1590, 1485, 1470, 1370, 1205, 1115, 1020, 1005, 990, 790, and 700 cm. - 1 ; mass spectral peaks at 358, 357, 116, 115, 108, 107, 79, 70, 69, 45, 43, and 51; [α] D +55° (C=0.7505 in 95 percent ethanol); and R f 0.18 (TLC on silica gel in 25 percent ethyl acetate is mixed isomeric hexanes).
D. d-2-Exo[m-(pivaloyloxy)benzoyl]-3-exo-bicyclo-[2.1.0]hexane-6-endo-carboxaldehyde Neopentyl Glycol Acetal (Formula LXXXIV: R 55 and R 56 taken together, R 68 is ##STR100## and ˜ is endo).
A mixture gel lithium (0.25 g.) in 70 ml. of ethylamine is prepared at 0° C. and cooled to -78° C. A solution of the formula LXXXII d-8-(m-acetoxyphenyl)-7-oxa-tricyclo-[4.2.0.0 2 ,4 ]-octane-6-endo-carboxaldehyde neopentyl glycol acetal (part C 1.83 g.) in 10 ml. of tetrahydrofuran is added dropwise in about 5 minutes. After stirring at -78° C. for about 3.5 hours the reaction is quenched with solid ammonium chloride and water-tetrahydrofuran. Unreacted lithium is removed, the mixture is warmed slowly to about 25° C., and ethylamine is removed. The residue is neutralized with dilute acetic acid, mixed with 200 ml. of brine, and extracted with ethyl acetate. The organic phase is washed with brine and a mixture of brine and saturated aqueous sodium bicarbonate (1:1), and dried over sodium sulfate. Concentration under reduced pressure yields the formula LXIII diol as a pale tan foamed oil, 1.64 g., having R f 0.03 (TLC on silica gel in 25 percent ethyl acetate in mixed isomeric hexanes).
The product of the preceeding paragraph is dissolved in 30 ml. of pyridine and treated with 1.5 ml. of pivaloyl chloride over a period of 22 hours at about 25° C. The reaction mixture is mixed with water, then brine and extracted with ethyl acetate. The organic phase is washed successively with brine, water, saturated aqueous copper (II) sulphate, saturated aqueous sodium bicarbonate, and brine, and dried over sodium sulfate. Concentration under reduced pressure yields a residue, 2.53 g., which is subjected to silica gel chromatography to yield the formula LXXIV title compound, 1.87 g., having NMR peaks at 0.71, 1.20, 1.33, 0.9∝3.1, 3.28-4.00, 4.17, 4.7-5.2, and 6.77-7.53 δ; mass spectral peaks at 486, 485, 115, 73, 72, 57, 44, 43, 42, 41, 30, 29, 15; [α] D +10° (C=0.8385 in ethanol); and R f 0.50 (TLC on silica gel in 25 percent ethyl acetate in mixed isomeric hexanes).
E. 2-Exo[m-(pivaloyloxy)benzyl]-3-exo-(pivaloyloxy)-bicyclo[3.1.0]hexane-6-endo-carboxaldehyde (Formula LXXXV: R 66 is ##STR101## and ˜ is endo).
The formula LXXXIV acetal, i.e. d-2-exo-(m-pivaloyloxy)-benzyl]-3-exo-(pivaloyloxy)-bicyclo[3.1.0]hexane-6-endo-carboxaldehyde neopentyl glycol acetal (part D, 0.48 g.) is treated at 0° C. with 25 ml. of 88 percent formic acid for 4 hours. The mixture is diluted with 200 ml. of brine and extracted with ethyl acetate. The organic phase is washed with brine and saturated aqueous sodium bicarbonate, and dried over magnesium sulfate. Concentration under reduced pressure yields an oil, 0.55 g., which is subjected to silica gel chromatography. Elution with 5-15 percent ethyl acetate in Skellysolve B yields mthe formula LXXXV title compound as an oil, 0.37 g., having NMR peaks at 1.20, 1.33, 0.6-3.2, 5.1-5.5, 6.6-7.5, and 9.73 δ; and R f 0.50 (TLC on silica gel in 25 percent ethyl acetate in mixed isomeric hexanes).
F. 2-Exo-[m-(pivaloyloxy)benzyl]-3-exo-(pivaloyloxy)-6-endo-(cis-1-heptenyl)-bicyclo[3.1.0]hexane (Formula LXXXVI: R 3 and R 4 of the L 1 moiety are both hydrogen, R 7 is n-butyl, R 66 is ##STR102## R 53 is hydrogen, and ˜ is endo); and 2-Exo-(m-hydroxybenzyl)-3-exo-hydroxy-6-endo-(cis-1-heptenyl(bicyclo[3.1.0]hexane (Formula LXXXVII: R 3 and R 4 of the L 1 moiety are both hydrogen, R 7 is n-butyl, R 53 and R 66 are hydrogen, and ˜ is endo).
A Wittig ylid reagent is prepared in 10 ml. of benzene from n-hexyltriphenylphosphonium bromide (0.79 g.) and n-butyllithium (0.6 ml. of 2.32 M. solution in hexane) at about 25° C. for 0.5 hours. After the precipitated lithium bromide has settled, the solution is removed and added to a cold (0° C.) slurry of the formula LXXXValdehyde (part E, (0.37 g.). After 15 minutes there is added 1.0 ml. of acetone and the mixture is heated to 60° C. for 10 minutes. The mixture is concentrated under reduced pressure. The residue is washed with 10 percent ethyl acetate in Skellysolve B and these washings are concentrated to the formula LXXXVI title compound, an oil, 0.33 g. having NMR peaks at 1.18, 1.33, 0.6-3.2, 4.5-6.0, and 6.67-7.62 δ; and R f 0.78 TLC on silica gel in 25 percent ethyl acetate in Skellysolve B).
The above product of the preceeding paragraph is transformed to the formula LXXXVII diol by treatment with sodium methoxide (2.5 ml. of a 25 percent solution in methanol) for 4 hours, followed by addition of 0.5 g of solid sodium methoxide and further stirring for 15 hours at 25° C., then at reflux for 6 hours. The mixture is cooled, mixed with 300 ml. of brine, and extracted with ethyl acetate. The organic phase is washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure to residue, 0.27 g. The residue is subjected to silica gel chromatography, eluting with 25-35 percent ethyl acetate in Skellysolve B, to yield the formula-LXXXVII title compound as an oil, 0.21 g., having NMR peaks at 0.87, 0.6-3.25, 3.88-4.35, 4.82-5.92, and 6.47-7.33 δ; and R f 0.13 (TLC on silica gel in 25 percent ethyl acetate in Skellysolve B).
G. 2- Exo-{m-[(methoxycarbonyl)methoxybenayl]}3-exo-hydroxy-6-endo-(cis-1-heptenyl)bicyclo[3.1.0]hexane (Formula LXXXVIII: R 3 and R 4 of the L 1 moiety are both hydrogen, g is one, R 7 is n-butyl, R 1 R 53 , and R 66 are hydrogen, and ˜ is endo).
The formula LXXXVII diol, i.e. 2-exo(m-hydroxybenzyl)-3-exo-hydroxy-6-endo(cis-1-heptenyl)bicyclo[3.1.0]hexane (part F, 0.19 g.) is treated in 8 ml. of dioxane with bromacetic acid (0.61 g.) and 6 ml. of 1N aqueous sodium hydroxide. After the mixture has been heated at reflux for 3 hours, with sodium hydroxide solution added when necessary to maintain a pH of about 10, the mixture is cooled, diluted with 100 ml. of water, and extracted with diethyl ether. The aqueous phase is acidified to pH 1-2 and extracted with ethyl acetate to yield the formula-LXXXVII title compound, a pale yellow oil, 0.20 g. Recovered formula LXXXVII diol is obtained from the diethyl ether organic phase on drying and concentrating, 0.025 g.
H. 3-Oxo-3,7-inter-m-phenylene-4,5,6-trinor-PGF 1 .sub.α (Formula XC: R 3 and R 4 of the L 1 moiety and R 5 and R 6 of the M 9 moiety are all hydrogen, R 7 is n-butyl, g is one, and R 1 is hydrogen).
The formula LXXXVIII alkene is transformed to formula XC compound applying the procedure disclosed in U.S. Pat. No. 3,711,515. Thus, compound LXXXVIII (part G) is hydroxylated by the procedures of Example 6 of that patent to the formula LXXXIX glycol of Chart G, using osmium tetroxide either alone or in combination with N-methylmorpholine oxide-hydrogen peroxide complex.
The glycol is then either (1) sulfonated, for example to yield the bismesylate, and then hydrolyzed to a mixture of the title compound and its 15-epimer, applying the procedures of Example 7 of that patent, or (2) treated with substantially 100 percent formic acid to form the diformate of VIII and thereafter hydrolyzed to a mixture of the title compound and its 15-epimer, applying the procedures of Examples 20 and 21 of that patent. The epimers are separated by silica gmel chromatography to yield the formula XC compound or its 15-epimer.
A third route from glycol LXXXIX to the formula XC compound is by way of cyclic ortho ester ##STR103## wherein R 74 , R 75 , and ˜ are as defined above. The glycol is treated as a 1-20 percent solution in benzene with trimethyl orthoformate (1.5-10 molar equivalents) and a catalytic amount (1 percent of the weight of the glycol) of pyridine hydrochloride at about 25° C. The reaction is followed by TLC (thin layer chromatography) and is complete in a few minutes. There is thus obtained the cyclic ortho ester in 100 percent yield.
The cyclic ester is then treated with 20 volumes of 100 percent formic acid at about 25° C. In about 10 minutes the reaction mixture is quenched in water or aqueous alkaline bicarbonate solution and extracted with dichloromethane. The organic phase is shaken with 5 percent aqueous sodium bicarbonate, dried over sodium sulfate, and concentrated to yield the corresponding diester. The diester is contacted with 10-50 volumes of anhydrous methanol and 10-20 percent of its weight of potassium carbonate at about 25° C. until the ester groups are removed. The mixture of epimers thusly obtained is separated by silica gel chromatography yielding the two 15-epimeric forms of the formula XC compound.
1. 2-Exo-[m-(carboxyethyl)benzyl]-3-exo-hydroxy-6-endo(cis-1-heptenyl)bicyclo-[3.1.0]hexane (Formula CII: Z 3 is methylene, g is one, R 3 and R 4 of the L 1 moiety are hydrogen, R 7 is n-butyl, R 1 and R 53 are hydrogen and ˜ is endo).
With respect to Chart H, there is first prepared the formula XCVII oxetane. Following the procedures of parts B and C, but replacing the m-acetoxybenzaldehyde of part B with the aldehyde of the formula ##STR104## wherein R 69 is as defined above, the corresponding formula XCVII oxetanes are obtained with a fully developed side chain.
Thereafter, following the procedures of parts D, E, and F, but replacing the formula LXXXII oxetane of part D withm the oxetane obtained by the procedure of the preceeding paragraph of this part, there are obtained the corresponding formula CI products.
Finally, the blocking groups on each CI compound are removed by methods disclosed herein or known in the art to yield the formula CII compound.
J. 3,7-inter-m-phenylene-4,5,6-trinor-PGF 1 α. Following the procedures of part H, the formula CII alkene is transformed in several steps to the title product.
Following the procedure of Example 25 or optionally following the procedure described in the text accompanying Charts I or J, there are prepared the various 3,7-inter-m-phenylene-3-oxa-4,5,6-trinor- or 3,7-inter-m-phenylene-4,5,6-trinor-PGF 1 .sub.α -type compounds described in Charts G, H, I, and J, particularly those optionally substituted at C-16 with methyl, fluoro, phenoxy, or substituted phenoxy, or at C-17 with phenyl or substituted phenyl.
EXAMPLE 26
15-Methyl-13,14-didehydro-PGF 2 .sub.α, methyl ester (Formula CLXXXII: R 1 and R 5 are methyl, R 3 and R 4 of the L 1 moiety and R 6 of the M 1 moiety are all hydrogen, R 7 is n-butyl, Y 1 is --C.tbd.C--, Z 1 is cis--CH=CH--(CH 2 ) 3 - and .tbd.is ##STR105##
Refer to Charts L and R.
A. 15-Keto-PGF 2 .sub.α, methyl ester, (14.4 g.) a formula CXXXII compound, in pyridine (35 ml.) is treated with benzoyl chloride (10.5 ml.) and the reaction is allowed to continue for 2 hours. Thereafter, the resulting mixture is diluted with ice water, cooled, and diluted with ice cold 10 percent sulfuric acid and methylene chloride. The layers are then separated and the organic layer is then dried and evaporated yielding 24.18 g. of crude formula CXXXIII product (R 16 is benzoyloxy). Chromatographic purification of this crude product (15.8 g.) on silica gel (600 g.) eluting with 15 percent ethyl acetate in hexane yields 13.6 g. of pure compound.
B. The reaction product of part A (5.0 g.) in carbontetrachloride (35 ml.) is cooled to freezing and bromine (1.38 g.) is added dropwise. The reaction is then diluted with methylene chloride, washed with sodium bicarbonate, dried, and evaporated to yield 5.6 g. of a crude 13,14-dibromo product. This crude dibromo product in pyridine (25 ml.) is heated to 90°-95° C. for 1.5 hours. The mixture is then allowed to stand at room temperature for 24 hours and thereafter diluted with methylene chloride. The resulting dark solution is then partitioned with ice cold 5 percent sulfuric acid. The organic extract is washed with brine and sodium bicarbonate, dried, and evaporated to yield 5 g. of crude formula CXXXIV product. Chromatographic purification on silica gel (320 g.), eluting with 5 percent ethyl acetate in benzene, yields 2.13 g. of product.
C. A solution of the reaction product of part B (6.32 g.) in tetrahydrofuran (45 ml.) at -78° C. is treated dropwise with excess ethereal methyl magnesium bromide. The reaction proceeds for 5 minutes, and is thereafter quenched by addition of aqueous potassium bisulfate. The reaction is then diluted with diethyl ether, washed with brine, dried, and evaporated to yield 6.5 g. of crude formula CXXXV compound. The crude product is then purified on silica gel (315 g.), eluting with 7.5 percent ethyl acetate in benzene, yielding 4.28 g. of the formula CXXXV compound as a mixture of C-15 epimers.
D. A solution of the reaction product of part C above (4.28 g.) in methanol (45 ml.) is treated with potassium carbonate (1.5 g.) at ambient temperature for 72 hours. The resulting solution is thereafter concentrated under reduced pressure, diluted with 5 percent sodium chloride solution, and extracted with methylene chloride. The aqueous phase is then cooled, acidified with 0.2 molar potassium bisulfate, and thereafter extracted successively with methylene chloride in methyl acetate. The carboxylic acid containing fraction is washed with brine, dried and evaporated to yield 3.2 g. of the formula CXXXVI compound (R 1 is hydrogen) as an epimeric mixture. This epimeric mixture is then esterified with excess diazomethane, yielding 2.32 g. of the corresponding methyl ester. High pressure liquid chromatography of this mixture of methyl esters on silica gel (512 g.) yields 15-epi-15-methyl-14-bromo-PGF 2 .sub.α, methyl ester, (0.75 g.) and 15-methyl-14-bromo-PGF 2 .sub.α, methyl ester (0.21 g.). Additional chromatographic runs yield 0.26 g. of the (15S)-compound.
The reaction product of part A exhibits NMR absorption at 0.89, 1.3-1.5, 3.61, 5.25-5.75, 6.3, 6.8-7.25, 7.25-7.7, and 7.75-8.2 δ. Infrared absorptions are observed at 1250, 1575, 1594, 1625, 1680, and 1740.
The reaction product of part B exhibits NMR adsorptions at 0.70-1.1, 1.1-3.05, 3.63, 5.25-5.8, 7.17, and 7.2-8.25 δ. The mass spectrum shows peaks at 652, 530, 451, 408, 328, 497, and 105. Characteristic infrared absorptions are observed at 1720, 1610, and 1270 cm. - 1 .
The (15RS) epimeric mixture produced in step 3 exhibits NMR absorptions at 0.8-1.1, 1.1-3.4, 1.48, 3.62, 3.9-5.8, 6.15, 6.06, and 7.10-8.2 δ.
For 15-methyl-14-bromo-PGF 2 .sub.α, methyl ester, NMR absorptions are observed at 0.7-1.1, 1.1-1.3, 1.49, 3.68, 3.85-4.4, 5.2-5.6, and 5.90 δ. The mass spectrum shows base peak absorption at 604.2587, and other peaks at 586, 571, 533, 525, 507, 347, and 217. For 15-epi-15-methyl-14-bromo-PGF 2 .sub.α, methyl ester, NMR absorptions are observed at 0.7-1.1, 1.1-3.4, 1.47, 3.8-4.4, 4.25-5.6, and 5.93 δ. Mass spectrum shows base peak absorption at 504.2615 and other peaks at 586, 573, 571, 533, 525, 514, 507, 496, 437, and 217.
E. A solution of the reaction product of part D, the 15-epi compound (0.19 g.) in dimethylsulfoxide (9 ml.) is treated with 0.5 molar potassium tert-butoxide in dimethyl sulfoxide (0.9 ml.). Silver nitrate impregnated silica gel thin layer chromatography is used to monitor the progress of the reaction. After 2 hours, the reaction being complete, the reaction mixture is diluted with diethyl ether, washed with ice cold potassium bisulfate, a 5 percent sodium chloride solution, and a 5 percent sodium bicarbonate solution. Thereafter drying and evaporation of solvent yields -0.126 g. of crude (15R) title product.
The 15-epimer is prepared by the above process or is alternatively prepared by saponification of the methyl ester of the formula CXXXVI compound, dehydrohalogenation of the saponified product, and finally methyl esterification of the dehydrohalogenated product. According to this route a solution of the reaction product of part D (0.55 g.) in methanol ((30 ml.) is treated with 2N sodium hydroxide (5 ml.) for 18 hours. The reaction is thereafter diluted with benzene and 0.2 M potassium bisulfate solution. The organic phase is then washed with 5 percent sodium chloride solution, dried, and evaporated to yield 0.49 g. of 15-epi-15-methyl-14-bromo-PGF 2 .sub.α. NMR absorptions are observed at 0.7-1.1, 1.1-3.4, 3.7-4.4, 5.1-5.75, and 5.95 δ. Characteristic infrared absorptions are observed at 3300, 2600, and 1725 cm. - 1 . Thereafter dehydrohalogenation proceeds by reacting the above free acid (0.49 g.) in 10 percent methanolic dimethylsulfoxide (7 ml.) with sodium methoxide (4.43 mmol) in 10 percent methanolic dimethyl sulfoxide (10.2 ml.). This mixture reacts for 20 hours. Thereafter the reaction mixture is diluted with benzene, washed with ethyl acetate and benzene (1:1). The combined organic extracts are then washed with saturated sodium chloride, dried, and evaporated to yield 0.31 g. of crude 15-epi-15-methyl-13,14-didehydro-PGF 2 .sub.α. This crude product is then esterified with excess diazomethane, under a nitrogen atmosphere, followed by evaporation to yield 2.8 g. of crude methyl ester. Purification on silica gel (25 g.) eluting with methylene chloride in acetone yields 0.211 g. of pure 15-epi-15-methyl-13,14-didehydro-PGF 2 .sub.α, methyl ester. For the free acid NMR absorptions are observed at 0.7-1.1, 1.1-3.2, 1.45, 4.0-4.5, and 5.4-6.0 δ. Characteristic adsorptions are observed at 3200 to 3400, 2600 to 2700, 2220, and 1710 cm. - 1 . For the methyl ester NMR absorptions are observed at 0.8-1.1, 1.1-3.2, 1.46, 4.0-4.5, 5.3-5.6 δ.
Following the alternate procedure described above for the preparation of 15-epi-15-methyl-13,14didehydro-PGF 2 .sub.α, methyl ester, there is prepared 15-methyl-13,14-didehydro-PGF 2 .sub.α, methyl ester. Accordingly, a solution of 15-methyl-14-bromo-PGF 2 .sub.α, methyl ester (0.41 g.) in methanol (25 ml.) is treated with 10 percent aqueous sodium hydroxide (6 ml.) and the resulting reaction is allowed to proceed overnight at ambient temperature. The corresponding acid is thereafter isolated as in the procedure described above for the preparation of 15-epimer to yield 0.34 g. of crude free acid.
Without further purification 0.32 g. of the free acid obtained above in a mixture of dimethylsulfoxide in methanol (9:1 10 ml.) is treated with 0.43 M sodium methoxide in a mixture of dimethyl sulfoxide and methanol (9:1; 6.6 ml.). After 20 hours the resulting solution is partitioned by adding ice old 0.2 M potassium bisulfate in benzene. The aqueous phase is extracted with the mixture of benzene and ethyl acetate (1:1) and the combined extracts are washed with brine, dried, and evaporated to yield 0.180 g. of crude 15-methyl-13,14-didehydro-PGF 2 .sub.α. After diazomethane esterification (following the procedure described above) crude title product is prepared which is subjected to silica gel chromatography (25 g.), eluting with acetone and methylene chloride (4:1). Thereby pure 15-methyl-13,14-didehydro-PGF 2 .sub.α, methyl ester (0.109 g.) is obtained. NMR absorptions are observed at 0.7-1.1, 1.1-3.5, 1.46, 3.69, 4.0-4.5, and 5.3-5.7 δ. The mass spectrum shows base peak absorption at 581.3508 and other peaks at 596, 525, 506, 491, 435, 416, 345, 255, and 217. Characteristic infrared absorptions are observed at 3350, 2900, 2220, and 1740 cm. - 1 .
Following the procedure of Example 26, but using in place of 15-keto-PGF 2 .sub.α, methyl ester, each of the various 15-keto-PGF-type compounds known in the art or readily available by methods known in the art, there are prepared the corresponding 13,14-didehydro-PGF-type products. Accordingly, 3.7-inter-m-phenylene-3-oxa-4,5,6-trinor-PGF 1 .sub.α is transformed to 15-keto-3,7-inter-m-phenylene-3-oxa-4,5,6-trinor-PGF 1 .sub.α, and this 15-keto compound is transformed following the procedure of Example 26 to 3,7-inter-m-phenylene-3-oxa-4,5,6-trinor-13,14-didehydro-PGF 1 .sub..alpha.. Likewise, 3,7-inter-m-phenylene-4,5,6-trino-PGF 1 .sub.α is transformed to 3,7-inter-m-phenylene-4,5,6-trinor-13,14-didehydro-PGF 1 .sub.α. Further, following the procedure described in Examples 4-16 and Example 19, but omitting the 2-chlorination of Example 4, there are prepared various PGF-type compounds which are transformed, as described above to corresponding 15-keto-PGF-type compounds. Each of these 15-keto-PGF-type compounds are transformed according to the procedure of Example 26 to the corresponding 13,14-didehydro-PGF-type compound. Accordingly, each of the various 13,14-didehydro-PGF 301 -type compounds disclosed herein is prepared according to the procedure of Example 26, by selection of the appropriate PGF.sub.α-type starting material.
EXAMPLE 27
15-Methyl-13,14-didehydro-PGE 2 , methyl ester (Formula CLXXXII: R 1 and R 5 are methyl, R 3 and R 4 of the L 1 moiety and R 6 of the M 1 moiety are all hydrogen, R 7 is n-butyl, R 8 is hydroxy, Y 1 is --C.tbd.C--, and Z 1 is cis-CH=CH-(CH 2 ) 3 -) or its 15-epimer.
Refer to Chart P and R.
A. A solution of 15-methyl-13,14-didehydro-PGF 2 .sub.α, methyl ester (Example 26, 0.142 g.), in acetone (18 ml.) at -45° C. is treated with trimethylsilydiethylamine (0.6 ml.). After 2.5 hours additional reagent (2.1 ml.) is added and the reaction is continued for 5 hours. The resulting mixture is then diluted with pre-cooled diethyl ether and partitioned wih aqueous sodium bicarbonate solution. The organic layer is then dried and evaporated to a yellow oil (15-methyl-13,14-didehydro-PGF 2 .sub.α, methyl ester, 11-(trimethylsilyl ether).
B. The oil obtained in part A is thereafter dissolved in methylene chloride (10 ml.) and thereafter added to a solution of CrO 3 (0.26 g), methylene chloride (20 ml.), and pyridine (0.4 ml.) at 0° C. This oxidation mixture is then vigorously agitated at 0° C. for 5 minutes and thereafter at ambient temperature for 10 minutes. The resulting suspension is then filtered through silica gel, with the combined filtrate and methylene chloride components being thereafter evaporated to yield 0.103 g. of 15-methyl-13,14-didehydro-PGD 2 , methyl ester, 11m-trimethylsilylether (a formula CLXXIII compound).
C. Crude reaction product of part B above in methanol (20 ml.) is treated with water (10 ml.) and acetic acid (1 ml.) and reacted for 5 minutes at 0° C. and thereafter stirred for 10 minutes at ambient temperature. The reaction is then diluted with diethyl ether and partitioned with 0.2 M sodium bisulfate. The organic layer is then washed with sodium chloride and sodium bicarbonate solutions, dried, and evaporated to yield 0.082 g. of crude title product.
Following the procedure described above, the corresponding 15-epimer is obtained.
For 15-methyl-13,14-didehydro-PGE 2 , methyl ester, the mass spectrum shows base peak absorption at 407.2981 and other peaks at 522, 491, 451, 432, 361, 307, 277, and 187. For the 15-epimer, NMR absorptions are observed at 0.8-1.1, 1.1-3.2, 1.48, 3.68, 4.1-4.7, and 5.3-5.6 δ. The mass spectrum shows base peak absorption at 507.2981, 522, 491, 451, 432, 361, 307, 277, and 187. Characteristic infrared absorptions are observed at 3300, 2257, and 1740 cm. - 1 .
Following the procedure of Example 27, the various 13,14-didehydro-PGF-type compounds described following Example 26 are transformed to corresponding 13,14-didehydro-PGE-type compounds.
EXAMPLE 28
15-Methyl-13,14-didehydro-PGF 1 .sub.α, methyl ester, or its 15-epimer.
Refer to Charts L and R.
A. A solution of 8.5 g. of PGF 1 .sub.α, methyl ester in dioxane (60 ml.) is treated with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (6.8 g.). The reaction proceeds for 21 hours and thereafter the suspension so formed is filtered, the filter cake being washed with dioxane and the combined filtrate and wash concentrated under reduced pressure. The residue is triturated with methylene chloride, filtered, and the solvent removed to yield 11.6 g., of crude 15-keto-PGF 1 .sub.α, methyl ester. Crude product is chromatographed on silica gel (450 g.), eluting with hexane and ethyl acetate (1:1). Pure compound (7.04 g.) is thereby obtained. NMR absorptions are observed at 0.89, 1.05-2.05, 2.05-2.75, 3.20-3.8, 3.67, 6.13, and 6.76 δ.
B. A solution of the reaction product of part A (7.07 g.) in pyridine (40 ml.) is treated with benzoyl chloride (6.3 ml.) and the reaction is allowed to proceed to ambient temperature for 3 hours. The resulting mixture is then diluted with ice water and extracted with methylene chloride. The methylene chloride extract is washed with solutions of ice cold dilute sulfuric acid, sodium bicarbonate, and sodium chloride. The washed extract is then dried and evaporated to yield 11.4 g. of a viscous oil. This oil is chromatographed on silica gel (200 g.) and pure product is obtained diluting with hexane in ethyl acetate (85:15). Accordingly, there is recovered pure 15-keto-9,11-dibenzoyl-PGF 1 .sub.α, methyl ester (10.76 g.). NMR absorptions are observed at 0.89, 1.5-1.80, 2.0-2.3, 2.3-2.7, 3.63, 5.1-5.65, 6.26, 6.92, 7.2-7.7, and 7.8-8.2 δ.
C. A solution of the reaction product of part B (4.77 g.) in carbon tetrachloride (20 ml.) is treated dropwise with a solution of bromine (8.2 mmol.) in tetrachlorethane (30 ml.). Coloration is observed to disappear in 10 minutes. The solvent is then removed under reduced pressure to yield 5.0 g. of 13,14-dibromo-9,11-dibenzoyl-15-keto-PGF 1 .sub.α, methyl ester. NMR absorptions are observed at 0.9, 1.10-2.0, 2.0-3.3, 3.65, 4.4-4.95, 5.08, 5.45-5.85, 7.10-7.8, and 7.9-8.2 δ.
D. The reaction product of part C (2.56 g.) in pyridine (18 ml.) is heated at 90°-95° C. for 1 hour. Thereafter the resulting dark green solution is diluted with methylene chloride, washed with ice cold 10 percent sulfuric acid, 5 percent sodium bicarbonate, and 5 percent sodium chloride solutions, dried, and evaporated. This process is then repeated for 2 additional runs and 9.0 g. of crude product is thereby recovered. Crude product is chromatographed on silica gel (210 g.), eluting with hexane and ethyl acetate (85:15). Thereby 5.5 g. of pure 14-bromo-9,11-dibenzoyl-15-keto-PGF 1 .sub.α, methyl ester is prepared. NMR absorptions are observed at 0.92, 1.1-2.0, 2.0-2.6, 2.6-3.1, 3.64, 5.1-5.7, 7.12, 7.2-7.7, and 7.8-8.7 δ.
E. A solution of the reaction product of part D above (0.43 g.) in tetrahydrofuran (15 ml.) is cooled to -78° C. and treated with ethereal methyl magnesium bromide (1.6 ml.) in tetrahydrofuran (10 ml.). After 3.5 hours the reaction mixture thereby obtained is poured with stirring into a cold mixture of diethyl ether and saturated ammonium chloride. The combined ethereal extracts are then washed with sodium chloride, dried and evaporated to yield 0.43 g. of crude (15RS)-15-methyl-14-bromo-9,11-dibenzoyl-PGF 1 .sub.α, methyl ester. Chromatographing on silica gel (25 g.), eluting with benzene in acetone (97:3) yields 0.280 g. of pure product. NMR absorptions are observed 0.83, 1.0-2.0, 1.47, 2.0-3.4, 3.63, 5.0-5.8, 6.13, 7.2-7.7, and 7.8-8.2 δ.
F. A solution of the reaction product of part E above (0.28 g.) in methanol (15 ml.) is treated with potassium carbonate (0.1 g.). The solution is stirred for 24 hours, thereafter being concentrated under reduced pressure, diluted with sodium chloride solution and extracted with ethyl acetate. Thereby, 0.197 g. of crude deacylated product is obtained. This crude product (0.19 g.) is then chromatographed on silica gel (25 g.) eluting with methylene chloride in acetone (85:15). Thereby 43 mg. of 14-bromo-15-methyl-PGF 1 .sub.α, methyl ester, and 40 mg. of 15-epi-14-bromo-15-methyl-PGF 1 .sub.α, methyl ester is obtained. For the (15S) product NMR absorptions are observed at 0.88, 1.10-2.1, 1.45, 2.1-2.7, 3.67, 3.8-4.4, and 5.92 δ. Mass spectrum shows peaks at 426, 395, and 372. For the 15-epimeric product NMR absorptions are observed at 0.88, 1.10-2.1, 1.45, 2.1-2.5, 2.5-3.3, 3.67, 3.8-4.4, and 5.97 δ. The mass spectrum shows peaks at 408 and 329.
G. A solution of potassium t-butoxide (0.37 g.) in tert-butanol (15 ml.) is treated with the reaction product of part F above (0.35 g.). After 3.5 hours the reaction mixture is diluted with diethyl ether and one percent aqueous potassium bisulfate is added. The aqueous phase is extracted with diethyl ether and benzene solutions and the combined organic extracts washed with brine, dried, and evaporated to yield 0.35 g. of crude product. The crude product is then purified on silica gel eluting with 40 percent ethyl acetate in benzene. Thereby 78 mg. of 15-methyl-13,14-didehydro-PGF 2 .sub.α is obtained.
Esterification of the product of the preceeding paragraph with diazomethane and thereafter chromatographing on silica gel, eluting with 12 percent acetone in methylene chloride yields 38 mg. of pure title product. The melting point is 50° C. The mass spectrum shows peaks at 598, 583, 527, 508, 469, 411, 217, and 187. Characteristic infrared absorptions are observed at 1740 and 2220.
Following the procedure of part G above 0.362 g. of 15-epi-15-methyl-14-bromo-PGF 1 .sub.α, methyl ester is transformed to 30 mg. of the 15-epimeric title product. NMR absorptions are observed at 0.9, 1.45, 2.1-2.4, 3.67, and 4.0-4.4 δ. The mass spectrum shows peaks at 598, 583, 508, 493, 477, 469, 411, 217, and 187. Characteristic infrared absorptions are observed at 1740 and 2240 cm.sup. -1 .
EXAMPLE 29
13,14-Didehydro-PGF 1 .sub.α, methyl ester or its 15-epimer.
A. Sodium borohydride (0.44 g.) in methanol (30 ml.) at -35° C. is treated with a solution of the reaction product of Example 28, part D (5.04 g.) and methanol. The solution is stirred for 20 minutes, quenched with acetic acid (20 ml.), diluted with diethyl ether, and ice cold 0.2 M sulfuric acid is added. The combined organic extracts are washed with sodium bicarbonate and saline solutions, dried, and evaporated. The crude residue, 14-bromo-(15RS)-9,11-dibenzoyl-PGF 1 .sub.α, methyl ester (5.0 g.) is used without further purification. NMR absorptions are observed at 0.7-1.0, 1.0-1.9, 1.9-2.3, 2.3-3.3, 3.63, 3.9-4.3, 5.0-5.6, 6.02, 7.2-7.7, and 7.2-8.2 δ.
B. A solution of the reaction product of part A above (5.0 g.) in methanol (35 ml.) is treated with potassium carbonate (1.5 g.) and agitated for 20 hours. The resulting suspension is then concentrated under reduced pressure, diluted with water, and extracted with ethyl acetate. Drying and evaporation of solvent yields 4.52 g. of crude epimerically mixed deacylated product. The aqueous phase above is acidified and extracted with ethyl acetate to yield 0.45 g. of the free acid of the above epimerically mixed acylated product. These acids are esterified with excess ethereal diazomethane and the combined methyl ester fractions are combined on silica gel eluting with methylene chloride and acetone (7:3) yielding 1.38 g. of 14-bromo-PGF 1 .sub.α, methyl ester and 1.23 g. of 15-epi-14-bromo-PGF 1 .sub.α, methyl ester. For the (15S) compound NMR absorptions are observed at 0.7-1.1, 1.1-2.0, 2.0-2.6, 2.6-3.5, 3.68, 3.75, 4.4, and 5.85 δ. The mass spectrum shows peaks at 414, 412, 360, 358, 351, 333, 279, and 278.
For the 15-epimeric product NMR absorptions are observed at 0.7-1.10, 1.1-2.0, 2.0-2.5, 2.5-3.5, 3.68, 3.8-4.5, and 5.88 δ. The mass spectrum shows peaks at 360, 258, 333, 279, and 278.
C. A suspension of 50 percent sodium hydride (0.7 g.) in dimethylsulfoxide (10 ml.) is treated with tert-butanol (1.3 ml.) and stirred until the resulting effervescence is ceased. A solution of the reaction product of part B above (1.38 g.) in dimethylsulfoxide (15 ml.) is added. After 20 hours the reaction is diluted with benzene and diethyl ether (1:1), and ice cold potassium bisulfate in water is added. The layers are separated and combined. The organic extracts are washed with a sodium chloride solution, dried, and evaporated. The residue is esterified with diazomethane. The resulting curde ester product (1.13 g.) is chromatographed on silica gel and the product eluted with methylene chloride in acetone (7:3). Thereby 0.61 g. of pure title product is obtained. Melting point is 68° C. NMR absorptions are observed at 0.90, 1.1-2.0, 2.0-3.0, 3.0-3.9, 3.68, and 4.0-4.45 δ. Characteristic infrared absorptions are observed at 1740, 2250, and 3200 to 3600 cm..sup. -1 . Mass spectrum shows peaks at 322, 319, 306, 297, 295, 294, 279, 278, 276, 250, and 222.
Following the procedure of Example 29, 1.23 g. of 15-epi-14-bromo-PGF 1 .sub.α, methyl ester is transformed to 0.53 g. of 15-epi-13,14-didehydro-PGF 1 .sub.α, methyl ester. NMR absorptions are observed 0.90, 1.1-2.0, 2.0-3.4, 3.68, and 3.9-4.7 δ. Characteristic infrared absorptions are observed at 1740, 2250, and 3450. The mass spectrum shows peaks at 350, 337, 332, 319, 306, 297, 295, 294, 279, 278, 276, 250, and 222.
EXAMPLE 30
13,14-Didehydro-PGE 1 , methyl ester or its 15-epimer.
A. A solution of 13,14-didehydro-PGF 1 .sub.α, methyl ester (Example 29, 0.22 g.) in acetone (18 ml.) at -45° C. is treated with trimethylsilyldiethylamine (0.8 ml.) and the resulting mixture stirred for 3.5 hours. Additional silylating agent (0.8 ml.) is added. After 45 minutes the reaction is quenched by sodium bicarbonate solution and extracted wit diethyl ether. Drying and evaporation of solvent yields 0.34 g. of crude 13,14-didehydro-PGF 1 .sub.α, methyl ester, 11,15-bis(trimethylsilyl ether).
B. The reaction product of part A (0.6 g.) in methylene chloride (25 ml.) at 0° C. is treated with chromium trioxide (0.5 g.) methylene chloride (40 ml.) and pyridine (0.8 ml.). The oxidation conditions are then maintained (0° C.) for 5 minutes and thereafter the temperature is allowed to warm to ambient temperature for an additional 10 minutes. The resulting mixture is then diluted with methylene chloride, and filtered through silica gel. The resulting eluant is then evaporated to yield 0.41 g. of crude 13,14-didehydro-PGE 1 , methyl ester, 11,15-bis(trimethylsilyl ether).
C. The product of part B above is combined with a mixture of methanol water and acetic acid (20:10:1, 31 ml.). The reaction is allowed to proceed at 0° C. for 5 minutes and thereafter at ambient temperature for 15 minutes. The resulting product is then diluted with water and extracted with diethyl ether. The combined ethereal extracts are then washed with sodium bicarbonate and brine and dried and evaporated to yield 0.33 g. of crude title product. This crude product is then chromatographed on 25 g. of silica gel eluting with methylene chloride in acetone (9:1) yielding 80 ml. of pure 13,14-didehydro-PGE 1 , methyl ester. Melting point is 46° C. characteristic 0.9, 1.1-2.05, 2.05-3.4, 3.67, and 4.0-4.6 δ. The mass spectrum shows absorptions at 348, 320, 319, 295, 292, and 263. The infrared absorption spectrum shows characteristic absorptions at 1675, 1740, 2220, and 3400 cm..sup. -1 .
Following the procedure of Example 30, parts A, B, and C, 130 mg. of 15-epi-13,14-didehydro-PGF 1 .sub.α, methyl ester is transformed to 26.5 mg. of 15-epi title product. Characteristic infrared absorptions are observed at 1740, 2225, and 3450 cm..sup. -1 . The mass spectrum shows peaks at 348, 320, 319, 317, 295, 292, and 263.
EXAMPLE 31
13,14-Didehydro-PGF 1 .sub.α or its 15-epimer.
Potassium t-butoxide (6.79 g.) in tert-butanol (45 ml.) and methanol (8 ml.) is treated with 14-bromo-PGF 1 .sub.α (3.02 g., see Example 29) and the reaction is allowed to proceed for 25 hours. The resulting reaction mixture is then diluted with diethyl ether, washed with ice cold 8 percent phosphoric acid, and the phases are separated. The aqueous phase is then extracted with benzene, and thereafter extracted with ethyl acetate. The combined organic extracts are then washed with a sodium chloride solution, dried, and evaporated to yield 2.86 g. of title product. The melting point is 74°-75° C. The mass spectrum shows base peak absorption at 642.3961 and other peaks at 627, 571, 552, 537, 481, and 436. Characteristic NMR absorptions are observed at 3150 to 3525, 2700, 2220, 1710, and 1680.
Following the procedure of the preceding paragraph, but using as starting material 15-epi-14-bromo-PGF 1 .sub.α (1.84 g.) there is prepared 15-epi-13,14-didehydro-PGF 1 .sub.α (1.46 g.). The melting point is 95°-96° C. NMR absorptions are observed at 0.8-1.1, 1.1-1.9, 2.0-2.8, and 3.9-4.7 δ. The mass spectrum shows base peak absorptions at 642. 4021 and other peaks at 627, 571, 552, 537, 481, and 217. The infrared absorption spectrum shows characteristic absorptions at 3150 to 3300, 2700, 2220, 1725, and 1700 cm..sup. -1 .
EXAMPLE 32
13,14-Didehydro-16-phenoxy-17,18,19,20-tetranor-8β,12α -PGF 2 .sub.β, methyl ester (Formula CXLVI: R 1 is methyl, R 2 and R 3 of the L 1 moiety and R 5 and R 6 of the M 1 moiety are hydrogen, R 7 is phenoxy, Y 2 is --C.tbd.C--, Z 2 is cis--CH=CH--CH 2 --(CH 2 ) 3 --CH 2 --, R 8 is hydroxy, and M 18 is ##STR106##
Refer to Chart M.
A. To a well stirred mixture of 15.2 g. of a 77 percent sodium hydride dispersion in mineral oil in 2 l. of tetrahydrofuran under a nitrogen atmosphere at 0° C. is added a solution of 92.9 g. of dimethyl-2-oxo-3-phenoxypropyl phosphonate and 220 ml. of tetrahydrofuran. After stirring at 0° for 5 minutes the resulting ylide solution is then stirred at ambient temperature for 75 minutes, thereafter being cooled at 0° C. Into the ylide solution is decanted 3β-benzoyloxy-5β-hydroxy-2α-carboxaldehyde-1β-cyclopentaneacetic acid γ lactone. The resulting mixture is then stirred at ambient temperature for 24 hours. The reaction is thereafter quenched by addition of 2 l. of 2M sodium bisulfate and ice. The aqueous mixture is then extracted well with chloroform. The organic extracts are then combined, washed with water, and saturated with sodium bicarbonate and brine, dried over sodium sulfate, and evaporated to yield a dark oil. This oil is then chromatographed on 2 kg. of silica gel packed in 25 percent ethyl acetate and Skellysolve B. Eluting with 4 l. of 75 percent ethyl acetate in Skellysolve B yields 3β-benzoyloxy-5β-hydroxy-2α-(3-oxo-4-phenoxy-trans-1-butenyl)-1β-cyclopentaneacetic acid γ lactone.
B. Following the procedure of Example 4, part B, the reaction product of part A of this example is transformed to 3β-benzoyloxy-5β-hydroxy-2α-(2-chloro-3-oxo-4-phenoxytrans-1-butenyl)-1β-cyclopentaneacetic acid γ lactone.
C. To the stirred mixture of 2.3 g. of sodium borohydride in 213 ml. of methanol at -20° C. under nitrogen atmosphere is added dropwise 17.7 g. of the reaction product of part B above in 67 ml. of methanol and 200 ml. of tetrahydrofuran. After 1 hour, the resulting mixture is quenched at -20° C. by slow addition of 11 ml. of acetic acid. The resulting solution is then allowed to warm to ambient temperature and diluted with ethyl acetate and washed with 2 M sodium bisulfate, water, and thereafter saturated with sodium bicarbonate and brine, dried over sodium sulfate, and evaporated to yield an oil. This oil containing a mixture of epimers is separated employing high pressure liquid chromatography on a 250 g. column eluting with 10 percent acetone in methylene chloride at 75 pounds per square inch. Pure (15R) and (15S) epimers of 3β-benzoyloxy-5β-hydroxy-2α-(2-chloro-3-hydroxy-4-phenoxy-trans-1-butenyl)-1β -cyclopentaneacetic acid γ lactone.
D. The reaction product of part C (6.8 g.) 10.8 g. of dihydropyran and 0.7 g. of pyridine hydrochloride in 93 ml. of methylene chloride is stirred at ambient temperature for 16 hours. The resulting solution is then filtered through silica gel washing well with ethyl acetate. Evaporation of the filtrate yields 3β-benzoyloxy-5β-hydroxy-2α-(2-chloro-3α-tetrahydropyranyloxy-4-phenoxy-trans-1-butenyl)-1β-cyclopentaneacetic acid γ lactone.
E. The reaction product of part D (8.3 g.) in 167 ml. of dry methanol at ambient temperature under a nitrogen atmosphere is added to 16.7 ml. of a 25 percent solution of sodium methoxide in methanol. After 1 hour the resulting reaction mixture is quenched by addition of 10 ml. of acetic acid. The resulting solution is then evaporated cautiously under reduced pressure. The residue is then cautiously dissolved in saturated sodium bicarbonate and methyl acetate. After equilibration the aqueous phase is separated and extracted well with ethyl acetate. The organic extracts are then combined, washed with brine, dried over sodium sulfate, and evaporated to yield 3β,5β-dihydroxy-2α-(2-chloro-3α-tetrahydropyranyloxy-4-phenoxy-trans-1-butenyl)-1β-cyclopentaneacetic acid γ lactone.
F. A solution of the reaction product of step E (6.8 g.) 6.1 g. of tosyl chloride and 160 ml. of dry pyridine is stirred at 50° C. under a nitrogen atmosphere. After 4 days the resulting solution is diluted with ice and ethyl acetate. To the resulting mixture is added 1 l. of 2M sodium bisulfate in small portions with frequent equilibration. The resulting mixture is then extracted well with ethyl acetate and the organic extracts are combined, washed with water, saturated with sodium bicarbonate and brine, dried over sodium sulfate, evaporated, and azeotroped with benzene to yield 3β-tosyloxy-5β-hydroxy-2α-(2-chloro-3α-tetrahydropyranyloxy-4-phenoxy-trans-1-butenyl)-1β-cyclopentaneacetic acid γ lactone.
G. A mixture of the reaction product of part F (4.8 g.), 8.2 g. of sodium benzoate, in 194 ml. of dimethylsulfoxide is stirred under a nitrogen atmosphere at 80°-85° C. After 3 hours the resulting solution is diluted with ice and diethyl ether. After equilibration the aqueous phase is extracted well with diethyl ether. The organic extracts are then combined, washed with saturated sodium bicarbonate and brine, dried over sodium sulfate, and evaporated to yield 3α-benzoyloxy-5β-hydroxy-2α-(2-chloro-3α-hydroxy-4-phenoxy-trans-1-butenyl)-1β-cyclopentaneacetic acid γ lactone, 3'-tetrahydropyranyl ether.
H. To a stirred solution of the reaction product of part G (3.8 g.) in 77 ml. of dry methanol at ambient temperature under a nitrogen atmosphere is added 7.7 ml. of sodium methoxide in methanol. After 45 minutes the reaction is quenched by addition of 4.6 ml. of acetic acid. The solution is then cautiously evaporated under reduced pressure and the residue cautiously dissolved in saturated sodium bicarbonate and ethyl acetate. After equilibration the aqueous phase is separated and extracted with ethyl acetate. Organic extracts are then combined, washed with brine, dried over sodium sulfate, and evaporated to yield 3α,5β-dihydroxy-2α-(2-chloro-3'α-hydroxy-4-phenoxy-trans-1-butenyl)-1β-cyclopentaneacetic acid γ lactone, 3-tetrahydropyranyl ether.
I. A solution of the reaction product of part H (2.1 g.) 3.1 g. of dihydropyran, and 0.2 g. of pyridine hydrochloride in 30 ml. of methylene chloride is stirred at ambient temperature for 17 hours. The resulting solution is then filtered through silica gel washing well with ethyl acetate. Evaporation of the filtrate yields 3α,5β-dihydroxy-2α-(2-chloro-3α-hydroxy-4-phenoxy-trans-1-butenyl)-1β-cyclopentaneacetic acid γ lactone, bis-(tetrahydropyranyl ether).
J. The reaction product of part I is transformed to 3α,5β-dihyroxy-2α-(2-chloro-3α-hydroxy-4-phenoxy-trans-1-butenyl)-1β-cyclopentaneacetaldehyde γ lactol bis-tetrahydropyranyl ether following the procedure of Example 8, part C. Thereafter, this compound is transformed to 14-chloro-16-phenoxy-17,18,19,20-tetranor-8β,12α-PGF 2 .sub.β, methyl ester, 11,15-bis(tetrahydropyranyl ether) following the procedure of Example 13.
K. A solution of 0.3 g. of the reaction product of part J in 20 ml. of acetic acid, water, and tetrahydrofuran (20:10:3) is heated at 40° C. for 3 hours. The resulting solution is then cooled to ambient temperature and diluted with 20 ml. of water and freeze dried to yield 14-chloro-16-phenoxy-17,18,19,20-tetranor-8β,12α-PGF 2 .sub.β, methyl ester.
L. The reaction product of part K (0.04 g.) and dimethylsulfoxide (10 ml.) is treated with potassium tertbutoxide (40 mg.) and reacted for 28 hours at ambient temperature. The resulting solution is then diluted with diethyl ether and poured into a mixture of ice cold potassium bisulfate and diethyl ether. The resulting mixture is then diluted with benzene, partitioned, washed with a sodium chloride solution, dried, and evaporated. The residue is chromatographed and esterified with excess ethereal diazomethane. The crude methyl ester product is chromatographed on silica gel eluting with methylene chloride in acetone (75:35), yielding pure title product.
Following the procedure of Example 32, the various 8β,12α-PGF 2 .sub.β -type compounds of Chart M are prepared. Further following the procedure of Chart M the various other PGF, PGE, or PGA-type compounds of Chart M are prepared. Further, following the procedure of Example 32, the various 11-deoxy-PGF- or PGE- compounds are prepared.
EXAMPLE 33
3,7-inter-m-Phenylene-4,5,6-trinor-13,14-didehydro-8β,12α-PGF.sub.1.sub.α, methyl ester (Formula CLXVII: R 1 is methyl, Z 1 is ##STR107##
Y 2 is --C.tbd.C--, R 3 and R 4 of the L 1 moiety and R 5 and R 6 of the M 1 moiety are all hydrogen, and R 7 is n-butyl).
Refer to Chart O.
A. Following the procedure of Example 25, the enantiomer of 3,7-inter-m-phenylene-4,5,6-trinor-15-epi-PGF 1 .sub.α is prepared from ent starting material. Thereafter, following the procedure of Examples 26 and 27 there is prepared the enantiomer of 3,7-inter-m-phenylene-4,5,6-trinor-14-chloro-15-epi-PGF 1 .sub.α.
B. Thereafter, following the procedure of Example 22, there is prepared 3,7-inter-m-phenylene-4,5,6-trinor-8β,12α-PGA 2 , a compound according to formula CLXI.
C. The reaction product of part B in 5 ml. of methanol is treated with stirring at -25° C. under nitrogen with a solution of 0.7 ml. of 30 percent aqueous hydrogen peroxide and 0.35 ml. of a 1N sodium hydroxide solution. After 1 hour there is added a 2N hydrochloric acid solution dropwise, thereby adjusting pH to 5 or 6. The resulting mixture is then diluted with brine and extracted with diethyl ether. The organic phase is washed with a sodium bicarbonate and brine, dried over sodium sulfate, and evaporated to yield 3,7-inter-m-phenylene-4,5,6-trinor-14-chloro-8β,12α-PGA 2 , 10,11-epoxide.
D. A mixture of the reaction product of part C (0.20 g.), aluminum amalgam (0.16 g.), 8 ml. of diethyl ether, 1.6 ml. of methanol, and 4 drops of water is stirred at ambient temperature for 2 days. The resulting mixture is then filtered and the filtrate concentrated to yield the title compound as a mixture of 11α and 11β isomers. Separation by silica gel chromatography eluting with ethyl acetate in Skellysolve B yields pure 11α-product, 3,7-inter-m-phenylene-4,5,6-trinor-14-chloro-8β,12α-PGE 2 .
The aluminum amalgam is prepared as follows:
Granular aluminum metal (50 g.) is added to a solution of mercuric chloride (50 g.) in 2 l. of water. The mixture is swirled until hydrogen gas evolution starts to become vigorous (about 30 minutes). Then most of the aqueous solution is decanted and the rest removed by rapid filtration. the amalgamated aluminum is then washed rapidly and successively with two 200 ml. portions of methanol and two 200 ml. portions of anhydrous diethyl ether. The amalgamated aluminum is then covered with anhydrous diethyl ether until ready for use.
E. Following the procedure of Example 21, the product of part D is transformed to 3,7-inter-m-phenylene-4,5,6-trinor-14-chloro-8β,12α-PGF 1 .sub.α. Thereafter, following the dehydrohalogenation procedure of Example 32, there is prepared the title product.
Following the procedure of Example 33, each of the various 8β,12α-PGA-type compounds described herein is transformed to the corresponding 8β,12α-PGF or PGE-type compound.
EXAMPLE 34
17-Phenyl-18,19,20-trinor-13,14-didehydro-11-deoxy-PGE 2 (Formula CLVI: R 1 is hydrogen, R 3 and R 4 of the L 1 moiety and R 5 and R 6 of the M 1 moiety are all hydrogen, R 7 is benzyl, Y 2 is --C.tbd.C--, and Z 1 is cis--CH=CH-- (CH 2 ) 3 --).
Refer to Chart N.
A. Employing 2,3-dichloro-5,6-dicyano-benzoquinone, 15-keto-17-phenyl-18,19,20-trinor-PGF 2 .sub.α is prepared from 17-phenyl-18,19,20-trinor-PGF 2 .sub.α.
B. Thereafter following the procedure of Examples 26 and 27 the reaction product of part A is transformed to 13,14-didehydro-17-phenyl-18,19,20-trinor-PGE 2 , methyl ester.
C. Following the procedure of Example 22, the reaction product of part B is transformed to 13,14-didehydro-17-phenyl-18,19,20-trinor-PGA 2 , methyl ester.
D. To a solution of the reaction product of part C above (0.77 g.) in pyridine (5 ml.) is added acetic anhydride (1.5 ml.). The mixture is then stirred for 4 hours under nitrogen and thereafter water (50 ml.) is added. The resulting mixture is then stirred for 55 minutes and thereafter extracted with ethyl acetate. The combined organic extracts are washed, dried, and concentrated to yield a formula CLIII compound, 13,14-didehydro-17-phenyl-18,19,20-trinor-PGA 2 , 15-acetate.
E. To a stirred solution of the reaction product of step D dissolved in methanol (25 ml.) at -25° C. under a nitrogen atmosphere, a solution of sodium borohydride (2 g.) in 5 ml. of water and 20 ml. of methanol is added. This resulting mixture is then stirred at -20° C. for 20 minutes and 3.5 ml. of acetic acid is thereafter cautiously added. The resulting mixture is concentrated and thereafter 50 ml. of water is added. The pH of the mixture is then adjusted to about 3 addition of citric acid. The mixture is then extracted with dichloromethane and the combined organic extracts are washed with water and brine, dried, and concentrated to yield a formula CLIV compound.
F. To a solution of the reaction product of part E (dissolved in acetone, 50 ml.) at -20° C., there is added dropwise with stirring over a one minute period the Jones reagent (1.5 ml.). This mixture is stirred at -20° C. for 20 minutes and thereafter 1.5 ml. of isopropanol is added and the resulting mixture is stirred at -20° C. for 10 minutes. This mixture is then diluted with 50 ml. of water and extracted with diethyl ether. The combined ethereal extracts are washed with water and brine, dried, and concentrated. The residue is then chromatographed on silica gel, eluting with acetone and methylene chloride. Those fractions containing the 15-acetate, methyl ester of the title compound are combined and concentrated.
G. To a solution of the reaction product of step F dissolved in methanol (15 ml.), there is added sodium hydroxide (0.5 g.) in 3 ml. of water and the resulting mixture is stirred at 25° C. for 17 hours. This mixture is then acidified with 10 ml. of 3N hydrochloric acid and thereafter concentrated to an aqueous residue. The residue is diluted with 25 ml. of water and extracted with diethyl ether. The combined ethereal extracts are washed with brine, dried, and concentrated. The residue is chromatographed on acid washed silica gel, eluting with ethyl acetate and hexane. Those fractions shown to contain pure title compound are combined.
Following the procedure of Example 34, each of the PGF-type compounds described herein is transformed to the corresponding 13,14-didehydro-PGA-type compound, which is in turn transformed to each of the various 13,14-didehydro-11-deoxy-PG-type compounds described herein.
EXAMPLE 35
13,14-Didehydro-16,16-dimethyl-PGF 2 .sub.α, methyl ester.
Refer to Chart R.
A solution of the reaction product of Example 16 in dimethyl sulfoxide (10 ml.) is treated with potassium t-butoxide (40mg.) and reacted for 28 hours at ambient temperature. The resulting solution is then diluted with diethyl ether and poured into a mixture of ice cold potassium bisulfate and diethyl ether. This mixture is then diluted with benzene partitioned, washed with a sodium chloride solution, dried, and evaporated. The residue is then esterified with excess ethereal diazomethane. The crude methyl ester is then chromatographed on silica gel (10 g.) eluting with methylene chloride and acetone (75:35). Thereby, 0.016 g. of title product is recovered. A characteristic IR absorption (--C.tbd.C--) is observed at 2250 cm..sup. -1 . The mass spectrum shows peaks at 327, 320, 304, 303, 302, 295, 284, 263, 247, 245, 235, 227, and 57.
Following the procedure of Example 35, each of the various 14-halo-11-deoxy-PGF.sub.α- or PGF.sub.α-type compounds described above is transformed to a corresponding 13,14-didehydro-11-deoxy-PGF.sub.α- or PGF.sub.α-type product.
Further, following the procedures of the above Examples each of the various 3,14-didehydro-11-deoxy-PGF.sub.α- or PGF.sub.α-type products is transformed to a corresponding 13,14-didehydro-11-deoxy-PGE- or PGE-type product.
Further, following the procedure of the above Examples each of the various 13,14-didehydro-11-deoxy-PGE- or PGE-type products is transformed to the corresponding 13,14-didehydro-11-deoxy-PGF.sub.β- or 11-deoxy-PGF.sub.β-type products.
Further, following the procedure of the above Examples each of the various 13,14-didehydro-PGE-type products is transformed to the corresponding 13,14 -didehydro-PGA- or PGB-type product.
EXAMPLE 36
13,14-Didehydro-PGF 3 .sub.α,13,14-didehydro-16,16-dimethyl-PGF.sub.3.sub.α, and 13,14-didehydro-16,16-difluoro-PGF 3 .sub.α.
A. Grignard reagents are prepared by reacting magnesium turnings with 1-bromo-cis-2-pentene; 1-bromo-1,1-dimethyl-cis-2 -pentene or 1-iodo-1,1-difluoro-cis-2-pentene. 1-lodo-1,1-difluoro-cis-2-pentene is prepared as follows:
2,2-difluoro-acetic acid is esterified with excess ethereal diazomethane. Thereafter the resulting methyl 2,2-difluoro-acetate is iodinized to methyl 2,2-difluoro-2-iodoacetate by the procedure of Tetrahedron Lett. 3995 (1971) (e.g., addition of lithium diisopropylamine to the starting material, followed by treatment with iodine). This product is then reduced to a corresponding aldehyde 2,2-difluoro-2-iodo-acetaldehyde, employing diisobutyl aluminum hydride at -78° C. This aldehyde is then alkylated by a Wittig alkylation, employing the ylid ethyl triphenylphosphorane, (C 6 H 5 ) 3 P=CH 2 --Ch 3 , thereby yielding the title iodide.
B. The Grignard reagent of part A is reacted with 3α-t-butyldimethylsilyloxy-5α-hydroxy-2β-(2-formyl-trans-1-ethenyl)-1α-cyclopentaneacetic acid γ lacetone, thereby preparing a corresponding 2β-[(3RS)-3-hydroxy-trans-1-cis-5-octandienyl] compound which is oxidized to a corresponding 3-oxo compound with the Collins reagent.
C. Following the procedures of the above examples the reaction product of step B is transformed to 13,14-didehydro-PGF 3 .sub.α.
Following the procedure of parts B and C above, but using a methyl or fluoro-substituted Grignard reagent, correspondingly 13,14 -didehydro-16,16-dimethyl-PGF 3 .sub.α or 13,14-didehydro-16,16-difluoro-PGF 3 .sub.α is prepared.
Following the procedure of the above examples, there are prepared the PGF.sub.α- or 8β,12α-PGF.sub.α- type compounds of Tables A, B, C, or D. Further, following the procedure of the above examples, there are prepared PGE- or 8β, 12α-PGE-; PGF.sub.β- or 8β,12αPGF.sub.β-; or PGA- or 8β,12α-PGA-type compounds corresponding to each of the PFG.sub.α- or 8β,12α-PGF.sub.α-type compounds of these tables. Finally, following the procedure of the above examples there are prepared PGB-type compounds corresponding to each of the PGF.sub.α-type compounds of these tables.
In interpreting these Tables, each formula listed in the Table represents a prostaglandin-type product whose complete name is given by combining the name provided in the respective legends below the formula with the prefix found in the "Name" column in the tabular section of the Tables for each example. ##STR108##
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This invention comprises certain analogs of the prostaglandins in which the double bond between C-13 and C-14 is replaced by a triple bond. Also provided in this invention, are novel chemical processes and novel chemical intermediates useful in the preparation of the above prostaglandin analogs. These prostaglandin analogs exhibit prostaglandin-like activity, and are accordingly useful for the same pharmacological purposes as the prostaglandins. Among these purposes are blood pressure lowering, labor induction at term, reproductive-cycle regulation, gastric antisecretory action, and the like.
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CROSS REFERENCE TO RELATED APPLICATION
This application is a continuation of application Ser. No. 09/955,607 filed Sep. 19, 2001 now U.S. Pat. No. 6,956,600.
TECHNICAL FIELD
The present invention relates to combining multiple digital video picture frames into a single spatial multiplex video picture frame to produce a single displayed picture that is a composite of several individual pictures. More particularly, the present invention relates to generating the spatial multiplex video picture frame by altering header information of the individual video picture frames being combined.
BACKGROUND
A motion picture such as broadcast television is made of individual pictures that are rapidly displayed to give the illusion of continuous motion. Each individual picture in the sequence is a picture frame. A digitally encoded picture frame is made of many discrete picture elements, or pixels, that are arranged in a two-dimensional array. Each pixel represents the color (chrominance) and brightness (luminance) at its particular point in the picture. The pixels may be grouped for purposes of subsequent digital processing (such as digital compression). For example, the picture frame may be segmented into a rectangular array of contiguous macroblocks, as defined by the ITU-T H series coding structure. Each macroblock typically represents a 16×16 square of pixels.
Macroblocks may in turn be grouped into picture frame components such as slices or groups of blocks, as defined under the ITU-T H.263 video coding structure. Under H.263, a group of blocks is rectangular and always has the horizontal width of the picture, but the number of rows of group of blocks per frame depends on the number of lines in the picture. For example, one row of a group of blocks is used for pictures having 4 to 400 lines, two rows are used for pictures having 404 to 800 lines, and four rows are used for pictures having 804 to 1152 lines. A slice, on the other hand, is a flexible grouping of macroblocks that is not necessarily rectangular. Headers within the encoded video picture bit stream identify and provide important information about the various subcomponents that make up the encoded video picture. The picture frame itself has a header, which contains information about how the picture frame was processed. Each group of blocks or slice within a video picture frame has a header that defines the picture frame component as being a slice or group of blocks as well as providing information regarding the placement of the component within the picture frame. Each header is interpreted by a decoder when decoding the data making up the picture frame in preparation for displaying it.
In certain applications, displaying multiple picture frames within a single display is desirable. For example, in videoconferencing situations it is useful for each participant to have a video display showing each of the other participants at remote locations. Visual cues are generally an important part of a discussion among a group of participants, and it is beneficial for each participant's display to present the visual cues of all participants simultaneously. Any method of simultaneously displaying all the conference participants is called a continuous presence display. This can be accomplished by using multiple decoders and multiple video displays at each site, or by combining the individual video pictures into a single video picture in a mosaic arrangement of the several individual pictures (called a spatial multiplex).
Multiplexing picture frames into a single composite picture frame requires some form of processing of each picture frame's encoded data. Conventionally, a spatial multiplex video picture frame could be created by completely decoding each picture frame to be multiplexed to a baseband level, multiplexing at the baseband level, and then re-encoding for transmission to the various locations for display. However, decoding and re-encoding a complete picture frame is computationally intensive and generally consumes a significant amount of time.
The H.263 standard provides a continuous presence multipoint and video multiplex mode that allows up to four individual picture frames to be included in a single bitstream, but each picture frame must be individually decoded by individual decoders or by one very fast decoder. No means of simultaneously displaying the pictures is specified in the standard. Additionally, time-consuming processing must be applied to the picture frames after they have been individually decoded to multiplex them together into a composite image for display.
Therefore, there is a need in the art for a method and system that can spatially multiplex multiple picture frames into a single picture frame without requiring each individual picture frame to be fully decoded when being multiplexed and without requiring additional processing after decoding to multiplex the picture frames.
SUMMARY
The present invention spatially multiplexes several picture frames into a single spatial multiplex video picture frame by manipulating header information for the picture frame components, such as the groups of blocks or slices, containing the picture frame data. A picture header associated with each picture frame is removed and a new picture header is generated that applies to the spatial multiplex video picture frame that is a composite of all of the individual picture frames. The new header provides an indication of a slice format for the spatial multiplex video picture frame. The component headers of each picture frame are altered to set a slice format based picture position for the picture frame within the picture that results from the spatial multiplex video picture frame. The slice format is prevalent within the H.263 standard. Thus, only the component headers need to be decoded and re-encoded to establish the spatial multiplex video picture frame.
The spatial multiplex video picture frame results from concatenating the new picture header together with the picture frames having the altered component header information. The spatial multiplex video picture frame may then be decoded as if it were a single picture frame to display the composite of the several individual picture frames. Displaying the spatial multiplex video picture frame allows the individual picture frames to be viewed simultaneously on one display screen.
The system that multiplexes the individual picture frames may be a scalable facility such that as the need for picture frame multiplexing increases, the system may be expanded to fill the need. The system includes a plurality of computing devices, such as single board computers, linked to a data packet switch through a serial interface. Each computing device within the system has the ability to combine individual picture frames into a single spatial multiplex video picture frame by altering the headers of the picture frame components to set a slice format based picture position for the picture frames. As the need for additional processing arises, additional computing devices in communication with the data packet switch may be added to provide additional capacity.
The present invention may be employed in a networked environment where a processing device, such as a network server, communicates with several client devices, such as videoconferencing devices. The processing device receives the multiple picture frames from various communication channels in the network. For example, the processing device may receive a stream of video picture frames from each participant in a videoconference through the network. The processing device then multiplexes the individual picture frames into a spatial multiplex video picture frame by altering the component header information to produce a slice based picture position for each frame. The spatial multiplex video picture frame is transmitted back through the communication channels of the network where it can be displayed by the display screen of the client devices.
The present invention may also be employed in a networked environment where each video site, such as a videoconferencing device, generates video picture frames. The picture frames are transmitted to other video sites in the network, and picture frames produced by other video sites are received. The video site multiplexes the picture frames to produces the multiplexed composite picture frame by altering the component header information to set a slice format based picture position. The video site may then decode the spatial multiplex video picture frame and display it.
The various aspects of the present invention may be more clearly understood and appreciated from a review of the following detailed description of the disclosed embodiments and by reference to the drawings and claims.
DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a composite picture frame and slice structure, an individual picture frame that may be multiplexed into the composite picture frame, and alternative picture frame structures.
FIG. 2 is an exemplary picture layer syntax of a picture frame under the H.263 standard.
FIG. 3 is an exemplary group of blocks layer syntax under the H.263 standard.
FIG. 4 is an exemplary slice layer syntax under the H.263 standard.
FIG. 5 is an operational flow for multiplexing picture frames utilized by one embodiment of the present invention.
FIG. 6 is an operational flow of the group of blocks to slice format conversion utilized by the embodiment.
FIG. 7 . is a block diagram of an embodiment employing single-point processing in a network environment.
FIG. 8 is a block diagram of an embodiment employing on-site processing in a networked environment.
FIG. 9 is a block diagram of an embodiment of a scalable multiplexing facility.
DETAILED DESCRIPTION
FIG. 1 illustrates a display of a spatial multiplex video picture frame 100 made up of individual picture frames 102 . As shown, the spatial multiplex video picture frame 100 includes sixteen picture frames 102 of individual people participating in a videoconference where the picture frames 102 form a mosaic pattern. Because each participant is always in view, the spatial multiplex video picture frame 100 is referred to as a continuous presence display. As will be discussed below, each individual picture frame 102 of the spatial multiplex video picture frame 100 is initially a normal picture frame 104 that may be displayed in full size on a display screen. The picture frame 104 may be represented as data that is encoded and segmented in various ways.
For the example shown, the picture frame 104 may have been transmitted in a quarter-size common image format (QCIF) indicating a pixel resolution of 176×144. In such a case, the spatial multiplex video picture frame 100 is decoded as a 4CIF picture indicating a resolution of 704×576 because it contains sixteen QCIFs where four QCIFs form a CIF size image. It is to be understood that other picture size formats for the individual picture frames 104 and for the spatial multiplex video picture frame 100 are possible as well. For example, the multiplexed image may contain 64 individual QCIF picture frames and therefore have a 16CIF size.
The group of blocks format 110 is one alternative for segmenting and encoding the picture frame 104 . The picture frame 104 of the group of blocks format 110 includes one or more rows of picture components known as groups of blocks 124 . In the example, shown, the QCIF frame 104 has three rows of groups of blocks. A picture header 122 is also included. The picture header provides information to a decoder when the picture frame 104 is to be displayed in full size and tells the decoder that the picture frame 104 has a group of blocks format 110 .
Each row 124 is made up of an array 112 of macroblocks 128 that define the luminance and chrominance of the picture frame 104 . Each row 124 also includes a header 126 that tells the decoder the position within the picture frame 104 where the row of group of blocks 124 belongs. In the example shown, the group of blocks 124 has two rows of macroblocks 128 because it is intended for the picture frame 104 to be displayed with 404 to 800 total lines. In reality, a group of blocks 124 will have many more macroblocks 128 per row than those shown in FIG. 1 .
As discussed above, the group of blocks format defined by the H.263 standard requires that the row 124 always extends to the full width of the picture. Therefore, a direct remapping of a group of blocks format 110 to a spatial multiplex video picture frame 100 is not possible because the spatial multiplex video picture frame 100 requires individual frames to have a width that may be less than the full width of the picture. In the videoconferencing context, several participants may need to be displayed across the width of the picture as shown in FIG. 1 , and a group of blocks format 110 does not permit such remapping.
An alternative format for segmenting and encoding the picture frame 104 is the slice format 106 , such as defined by the H.263 standard. The slice format 106 is more flexible and does not require each slice to maintain the full width of the picture. The slice format 106 includes one or more picture components known as slices 116 that may or may not extend across the full width of the picture, and a picture header 114 that specifies to the decoder that the picture frame 104 has a slice format. Each slice 116 is made up of a grouping 108 of macroblocks 120 . Each slice 116 also has a slice header 118 that indicates to the decoder the relative position of the slice in the picture 104 .
The slice format 106 of the picture frame 104 allows the picture frame 104 to be multiplexed into the composite picture frame 100 with minimal decoding. The spatial multiplex video picture frame 100 may be created in a slice format 130 of many slices 134 corresponding to the slices 116 of the individual picture frames 102 forming the composite. As shown, the slices 134 have a width that is less than the picture width so that multiple slices 134 are provided for each row of slices of the picture. A new picture header 132 is also generated to indicate to the decoder that the picture frame 100 is of the slice format 130 and is of a 4CIF size, 16CIF size, and so on. The header, such as 118 , of each slice 134 is modified to properly position the slice within the spatial multiplex video picture frame 100 .
FIG. 2 shows the picture layer syntax 200 that is made up of the picture header included at the beginning of each picture frame as well as the group of block layer or slice layer. The picture layer syntax 200 includes a picture start code (PSC) 202 that signifies the beginning of a new picture frame. A temporal reference (TR) 204 follows in the bitstream and provides a value indicating the timing of display of the picture frame relative to a previous frame and the picture clock frequency. A PTYPE block 206 follows and provides information about the picture such as whether the source format of the picture frame is a quarter-size common image format (QCIF), a CIF format, or other.
The picture layer syntax 200 may also include a PLUS HEADER block 208 that contains information about the picture frame, including whether the frame consists of groups of blocks or slices. A PQUANT block 210 provides quantizer information to configure the quantization parameters used by the decoder. An optional continuous presence multipoint (CPM) block 212 signals the use of continuous presence multipoint and video multiplex mode discussed above that permits multiple individual frames to be included in the bitstream. As discussed the CPM mode causes the individual frames to maintain their identities as individual frames and requires that they be individually decoded and then processed to form a single image. A picture sub-bitstream indicator (PSBI) 214 may be included if CPM mode is indicated. CPM mode may be implemented in conjunction with the logical operations of FIGS. 5 and 6 to provide sub-bitstreams that are themselves multiplexed bitstreams, or CPM may be turned off if only the logical operations of FIGS. 5 and 6 are desired for providing continuous presence video.
A temporal reference for B-picture parts (TRB) 216 may be included if a PB-frame is indicated by the PTYPE block 204 or PLUS HEADER block 208 . A DBQUANT block 218 may also be included if a PB-frame is indicated to indicate the relation of the BQUANT quantization parameter used for B-picture parts in relation to the QUANT quantization parameter used for P-picture parts. A PEI block 220 includes a bit that signals the presence of the supplemental enhancement information (PSUPP) block 222 . PSUPP block 222 defines extended capabilities for picture decoding. The group of blocks (GOB) layer 224 or slice layer 226 then follows in the bitstream. The GOB layer 224 contains each group of block of the picture frame and is discussed in more detail in FIG. 3 . Slice layer 226 contains each slice of the picture frame and is discussed in more detail in FIG. 4 .
The ESTUF block 228 is included to provide mandatory byte alignment in the bitstream. The end of sequence (EOB) block 234 may be included to signal the end of the sequence of group of blocks or slices. Alternatively, the end of sub-bitstream sequence (EOSBS) block 230 may be included to indicate an end of a sub-bitstream when in CPM mode. An ending sub-bitstream indicator (ESBI) block 232 is included to provide the sub-bitstream number of the last sub-bitstream. The PSTUF block 236 is included to provide byte alignment for the PSC of the next picture frame.
FIG. 3 shows the group of blocks layer syntax 300 that is made up of the component header and the macroblocks of the array forming a group of blocks and that would be found in each group of blocks of the group of blocks layer 224 of FIG. 2 . A GSTUF block 302 is included to provide byte alignment for a group of blocks start code (GBSC) 304 . The GBSC 304 indicates to the decoder the start of a group of blocks. A group number (GN) block 306 indicates the group of block number that defines the position of the group of blocks in the picture frame. A GOB sub-bitstream indicator (GSBI) 308 may be included when in CPM mode to indicate the sub-bitstream number.
A GOB frame ID (GFID) 310 is included to indicate the particular frame that the group of blocks corresponds to. GQUANT block 312 provides quantizer information to control the quantization parameters of the decoder. A temporal reference indicator (TRI) block 314 is included to indicate the presence of a temporal reference when operating in a reference picture mode. A temporal reference (TR) block 316 is included to provide a value indicating the timing of display of the group of blocks relative to a previous group of blocks and the picture clock frequency. A temporal reference for prediction indication (TRPI) block 318 is included to indicate the presence of a temporal reference for prediction field (TRP) 320 . The TRP field 320 indicates the temporal reference to be used for prediction of the encoding.
A back channel message indication (BCI) field 322 is included to indicate whether a message is to be delivered from the decoder back to the encoder regarding conditions of the received coded stream. A back channel message (BCM) layer 324 contains a message that is returned from a decoder to an encoder in order to tell whether forward-channel data was correctly decoded or not. A macroblock (MB) layer 326 contains a macroblock header and the macroblock data for the group of blocks.
FIG. 4 shows the slice layer syntax 400 that is made up of the component header and the macroblocks of the array forming a slice and that would be found in each slice of the slice layer 226 of FIG. 2 . An SSTUF block 402 is included to provide byte alignment for a slice start code (SSC) block 404 indicating the beginning of a slice. A first slice emulation prevention bit (SEPB 1 ) 406 is included to prevent start code emulation after the SSC block 404 . A slice sub-bitstream indicator (SSBI) block 408 is included when in CPM mode to indicate the sub-bitstream number of the slice. A macroblock address (MBA) field 410 is included to indicate the first macroblock of the slice as counted from the beginning of the picture in scanning order to set the position of each slice in the picture frame.
A second slice emulation prevention bit (SEPB 2 ) block 412 is also included to prevent start code emulation after the MBA field 410 . An SQUANT block 414 is included to provide quantizer information that controls the quantization parameters of the decoder. A slice width indication (SWI) block 416 is provided to indicate the width of the current rectangular slice whose first macroblock is specified by the MBA field 410 . A third slice emulation prevention bit (SEPB 3 ) 418 is included to prevent start code emulation after the SWI block 416 . A slice frame ID (GFID) 420 is included to indicate the particular picture frame that the slice corresponds to. The TRI field 422 , TR field 424 , TRPI field 426 , TRP field 428 , BCI field 430 , BCM layer 432 , and MB layer 434 are identical to the fields of FIG. 3 that go by the same name.
The operational flow of the process 500 for multiplexing individual picture frames containing the GOB syntax 300 or the slice syntax 400 into a single picture frame is shown in FIG. 5 . In this embodiment of the operational flow, it is assumed that the single picture frames are originating from encoder devices and are being processed by one or more decoder devices after transfer, such as through a network medium as shown in the systems of FIGS. 7 and 8 . The process 500 begins at call operation 502 where the two devices passing the picture data establish a common mode of operation suitable for generating continuous presence video. The common mode of operation includes a consistent usage of header information so that, for example, back channel messaging is employed between the encoder and decoder or other enhanced capabilities are realized. After communication is established, start operation 504 causes one device of the connection to broadcast a start indicator that allows synchronization of transmission of the individual picture frames from the various sources, such as the remote locations of the video conference.
Once the picture frames to be included in the multiplexed frame have been received, header operation 506 reads the picture layer header, such as shown in FIG. 2 , for each individual picture frame and discards them. This requires that only the picture header be decoded. A single new picture layer header that applies to the spatial multiplex video picture frame is created and encoded at header operation 506 . The single new picture layer header provides in the PTYPE field 206 an indication that the spatial multiplex video picture frame is of a size capable of including the number of individual frames being multiplexed. The PLUS HEADER field 208 of the new picture header is configured to indicate a rectangular slice format.
After substituting the new picture header, the component header of one of the individual frames is interpreted at read operation 508 in preparation for subsequent processing discussed below including conversion to a slice format and repositioning within the multiplexed image. Query operation 510 detects whether the picture header read in header operation 506 for the current picture frame indicates a group of blocks format. If a group of blocks format is detected, then conversion operation 512 converts the group of blocks headers into slice headers. Conversion operation 512 is discussed in greater detail below with reference to FIG. 6 . If a group of blocks format is not detected, then the conversion operation 512 is skipped since a slice format is already present in the picture frame.
After finding or converting to a slice format, macroblock operation 514 alters the MBA 410 within each slice of each picture frame to position the slice within a particular region of the spatial multiplex video picture frame. For example, one individual picture frame must go in the top left-hand corner of the multiplexed picture so the top-leftmost slice of that picture frame is given an MBA 410 corresponding to the top left-hand corner position. The component header is also re-encoded at this operation after the MBA 410 has been altered. The slice is then inserted into the proper location in the continuous presence picture stream by concatenating the bits of the slice with the bits already present in the picture stream including the new picture header at stream operation 516 . The picture stream may be delivered as it is being generated at transmit operation 518 wherein the current slice is written to an output buffer and then transmitted to a network interface.
After writing the slice to the output buffer, query operation 520 detects whether the last slice was the end of the continuous presence or spatial multiplex video picture frame. If it was not the last slice of the multiplexed frame, then flow returns to read operation 508 where the header of the next group of blocks or slice to be included in the spatial multiplex video picture frame is read. If query operation 520 determines that the last slice was the end of the spatial multiplex video picture frame, then flow returns to header operation 506 wherein the picture headers for the next set of individual picture frames are read and discarded.
FIG. 6 shows the operational flow of the conversion operation 512 . Conversion operation 512 begins at alignment operation 602 where the GSTUF field of the GOB syntax 300 is converted to an SSTUF field of the slice syntax 400 by adjusting the length of the stuff code to provide byte alignment of the next code element. At start code operation 604 , the GBSC 304 is maintained because it is already identical to the SSC 404 needed in the slice syntax 400 . At prevention operation 606 , the SEPB 1 406 is inserted into the bitstream to later prevent start code emulation when being decoded.
Translation operation 608 converts the GSBI 308 to the SSBI 408 . During this operation, GSBI ‘00’ becomes SSBI ‘1001’, GSBI ‘01’ becomes SSBI ‘1010’, GSBI ‘10’ becomes SSBI ‘1011’, and GSBI ‘11’ becomes SSBI ‘1101’. At MBA operation 610 , the GN 306 is replaced by an MBA 410 chosen to place the slice in its designated location within the composite picture frame resulting from multiplexing the individual picture frame bitstreams. Prevention operation 612 then places a SEPB 2 into the bitstream to prevent start code emulation. At quantizer operation 614 , GQUANT is maintained in the bitstream after SEPB 2 because GQUANT is already identical to SQUANT 414 .
Slice operation 616 then sets the width of the slice, or SWI 416 , to the width of the GOB in terms of the number of macroblocks. This is possible because the slice structure selection (SSS) field (not shown) of the PLUS HEADER field 208 of the picture syntax 200 of FIG. 2 has been set to the rectangular slice mode in header operation 506 of FIG. 5 . Prevention operation 618 then inserts a SEPB 3 into the bitstream to prevent start code emulation when the slice is decoded. At GFID operation 620 , the GFID 310 is maintained in the bitstream after SEPB 3 because it is already identical to GFID 420 . In substitute operation 622 , all remaining portions of the GOB syntax 300 are maintained in the bitstream because they are also identical to the remaining portions of the slice syntax 400 .
FIG. 7 . shows one network environment for hosting a continuous presence videoconference. A server 702 communicates through bi-directional communication channels 716 with client devices 704 , 706 , 708 , and 710 . Each client device, such as a personal computer or special-purpose videoconferencing module, is linked to a camera 712 or other video source and a video display 714 . The client devices transmit sequences of encoded picture frames produced by the camera 712 or other video source to the server 702 though the communication channels 716 . The server 702 then employs the processes of FIGS. 5 and 6 to combine all of the encoded picture frames into an encoded spatial multiplex video picture frame. The server 702 then transmits the spatial multiplex video picture frame back through the communications channels 716 to the client devices where it is decoded and displayed on each display screen 714 . Thus, the client devices may include encoder and decoder processing but do not need to include the multiplexing processing discussed above.
Four client devices are shown only for exemplary purposes, and it is to be understood that any number of client devices may be used subject to the limitation on the total number of individual frames to be included on the display 714 . It is also to be understood that each individual frame to be included in the multiplexed frame through the processes of FIGS. 5 and 6 does not have to be of the same size, such that one frame may occupy more screen area than others. For example, the frame showing the person currently speaking in a videoconference may be enlarged relative to frames showing other participants. One skilled in the art will recognize that negotiation between participating devices can be established such that mode switching can occur to permit one or more participants to provide one image size (e.g., QCIF) while other participants provide a different image size (e.g., CIF), subject to the ability to combine the image sizes into a composite that will fit on the intended display. Furthermore, it is to be understood that the server 702 may customize each videostream being returned to each client device 704 , 706 , 708 , and 710 , such as by removing the frame provided by the recipient client device from the spatial multiplex being returned or creating the spatial multiplex from some other subset.
The communication channel between the client devices 704 , 706 , 708 , and 710 and the server 702 can be of various forms known in the art such as conventional dial-up connections, asymmetric digital subscriber lines (ADSL), cable modem lines, Ethernet, and/or any combination. An Internet Service Provider (ISP) (not shown) may be provided between the server 702 and each client device, or the server 702 may itself act as an ISP. The transmissions through a given channel 716 are asymmetric due to one picture frame being transmitted to the server 702 from each client device while the server 702 transmits a concatenation of picture frames forming the multiplexed bitstream back to each client device. Therefore, ADSL is well suited to picture frame transfer in this network configuration since ADSL typically provides a much greater bandwidth from the network to the client device.
FIG. 8 shows an alternative network configuration where each client device 802 , 804 , 806 , and 808 has its own processing device performing the operations of FIGS. 5 and 6 . Each client device is linked to a camera 810 or other video source and a display 812 . A bi-directional communication path 814 interconnects each client device to the others. The bi-directional communication paths 814 can also be of various forms known in the art such as conventional dial-up connections, asymmetric digital subscriber lines (ADSL), cable modem lines, Ethernet, and/or any combination. One or more ISPs (not shown) may facilitate transfer between a pair of client devices.
Each client device generates an encoded picture frame sequence that is transmitted to the other client devices. Thus, each client device receives an encoded picture frame from the other client devices. The client device may then perform the multiplexing operations discussed above to create the spatial multiplex video picture frame that is displayed.
Multiplexing the individual picture frames together at each client device where the spatial multiplex video picture frame will be displayed allows each client device to have control over the spatial multiplex video picture frame it will display. For example, the client device can choose to exclude certain picture frames or alter the displayed size of particular picture frames. In a videoconference, the client device may choose to eliminate the picture frame that it generates and sends to others from the spatial multiplex video picture frame that it generates and displays. Because each client device performs the multiplexing operations, the communication paths 814 carry only the individual picture frame sequences generated by each sending client device rather than spatial multiplex video picture frame sequences.
FIG. 9 shows an example of a scalable multi-point conferencing facility 900 . The facility includes a packet switch 902 , such as a multi-gigabit Ethernet switch, linked to several processing modules, such as single board computers (SBCs) 904 , 906 , and 908 . An SBC generally refers to a computer having a single circuit board including memory, magnetic storage, and a processor for executing a logical process such as those of FIGS. 5 and 6 . The processing modules may include general-purpose programmable processors or dedicated logic circuits depending upon the performance necessary. Because the operations of FIGS. 5 and 6 to be performed by the processing modules requires only decoding of header information, programmable processors are adequate for continuous presence processing in real time for most implementations.
The processing modules are linked to the packet switch 902 through high-speed serial interfaces 910 , such as Fast/Gigabit Ethernet. The packet switch 902 receives encoded picture frame sequences from client devices, such as discussed with reference to FIG. 7 , but possibly from several videoconferencing sessions. The packet switch 902 may then send all picture frame sequences corresponding to a particular videoconference to one of the processing modules 904 , 906 , or 908 . The processing module multiplexes the picture frames to generate a spatial multiplex video picture frame and sends the spatial multiplex video picture frame sequence back to the packet switch 902 . The packet switch 902 then delivers the spatial multiplex video picture frame sequence back to client devices of the particular videoconference.
Thus, the scalable multi-point conferencing facility 900 can provide multiplexing services for multiple videoconference groups simultaneously. As the number of videoconference groups at any given time increases or decreases, the processing modules employed by the packet switch 902 can be added or removed from active service and made available for other duties when not needed by packet switch 902 .
Although the present invention has been described in connection with various exemplary embodiments, those of ordinary skill in the art will understand that many modifications can be made thereto within the scope of the claims that follow. Accordingly, it is not intended that the scope of the invention in any way be limited by the above description, but instead be determined entirely by reference to the claims that follow.
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Multiple video picture frames are combined into a spatial multiplex video picture frame that may be fully decoded and displayed. The video display of the spatial multiplex video picture frame is a composite combination of all of the video picture frames that have been combined, and may have an appearance such as a mosaic. Multiplexing the video picture frames involves removing picture headers, creating a picture header for the spatial multiplex video picture frame, and altering the headers of individual components of each video picture frame. The new header for the spatial multiplex video picture frame indicates a slice format frame, and headers of the individual components are altered to provide a slice format based picture position for each video picture frame. The headers of the individual components are altered to become slice based, such as in accordance with the ITU-T H.263 video standard, prior to establishing the slice based picture position if the frames are not already of the slice format.
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FIELD OF THE INVENTION
[0001] The present invention relates generally to vents and ducts for gas transport and, more particularly, to ducts of the type commonly installed as exhaust transition ducts for household and commercial clothes dryers and as air ducts in heating, ventilation, and air conditioning (HVAC) systems.
BACKGROUND OF THE INVENTION
[0002] Air ducts for ventilation systems are well known. They are typically used to direct air flow for heating and air conditioning systems. Another common application is for the exhaust vent of clothes dryers.
[0003] A very typical and common exhaust vent for clothes dryers is fabricated of a resilient wire helix which is covered with vinyl tubing, which lacks structural integrity and is generally not flame resistant or with aluminum tubing, which lacks structural integrity. The lack of structural integrity typically results in sagging and crinking of the duct. Ducts of these types also tend, over time, to become lined with lint from the clothes dried in the dryer, posing a fire hazard. According to the Consumer Products Safety Commission, there are over 15,000 fires annually associated with clothes dryers, causing deaths and injuries and some $90 million in damages. It is generally recommended by clothes dryer manufacturers not to use vinyl ducts such as these for dryer exhaust transition ducts.
[0004] Representative of the prior art in ventilation systems is U.S. Pat. No. 5,281,187, included herein by reference, to Whitney for a “Unitary Vent and Duct Assembly” which discloses a “semi-rigid flexible duct” for a ventilation system installed with a suspended ceiling structure. The duct taught in this patent is actually a solid aluminum tube which is corrugated or “accordion-folded” so that it can be compressed or compacted for storage or shipping. The corrugated aluminum tube duct taught therein, is meant to be coupled to a duct assembly of which it is an integral part, which is intended only for installation within a framed section of a suspended or dropped ceiling. However, once such a tube has been compressed and then re-extended for installation, it may not be likely to maintain its rigidity, depending on the thickness of the aluminum. A tube of this type that will maintain its rigidity, by virtue of its being fabricated of solid metal, will be heavy and expensive and can be unwieldy to install. The corrugated aluminum, when extended after compression, will have significant ridges and other obtrusive topographical features along its interior due to the corrugations, which will cause frictional resistance to the air flow within, a further disadvantage.
[0005] Corrugated aluminum is also employed for the exhaust vent of clothes dryers, as, for example, in U.S. Pat. Nos. 5,121,948, 5,133,579, and 5,145,217, which also solve the above-described problem of insufficient rigidity by using totally rigid segments. Even though the aluminum tubing itself is obviously fire resistant, the ridges and other internal topographical features similar to those mentioned hereinabove with respect to the Whitney patent, also cause fictional resistance to the air flow within, permitting accumulation of lint, which, as stated hereinabove, presents a fire hazard.
[0006] U.S. Pat. No. 5,526,849, included herein by reference, to Gray for a “Flexible Duct” discloses a duct and a method for manufacture thereof. The duct disclosed therein is formed of plastic tapes wound on a rotating mandrel with a wire resilient helix and a yarn helix therebetween. The duct so produced, while flame resistant, has rigidity limited to that provided by the wire helix. The additional yarn helix complicates the manufacturing process and adds to the internal topographical features of the duct, increasing friction and the possibility of lint accumulation therein, as described above.
SUMMARY OF THE INVENTION
[0007] The present invention seeks to provide a flexible duct for a ventilation system, and particularly for clothes dryer exhaust, that is fire resistant and that is lighter in weight and less expensive than those used in the prior art, while maintaining rigidity and structural integrity, even after having been compressed to a compacted configuration for shipping and storage and then re-extended for installation. Further, the duct should have minimal internal topographical features or structure, even after having been compressed to a compacted configuration for shipping and storage and then re-extended for installation. The present invention further seeks to provide a method for manufacturing such a duct that is simple, fast, and efficient.
[0008] There is thus provided, a semi-rigid, flexible, duct for gas transport and in particular, to serve as a clothes dryer exhaust transition duct, having an axis, including a pair of coaxial sleeves, including an inner sleeve and an outer sleeve disposed parallel to and about the inner sleeve, and a resilient helical element disposed between them;
wherein each of the inner sleeve and the outer sleeve includes a first layer having metallic properties and one or both of which further include a second, plastic layer bonded to the first layer having metallic properties; wherein the helical element imparts helical corrugations to the inner sleeve and the outer sleeve, such that the duct is axially extendible between a compacted configuration suitable for storage and for shipping and an extended configuration suitable for installation in a gas transport arrangement; and wherein all the layers of both the inner sleeve and the outer sleeve are of a thickness predetermined to together render the duct substantially rigid when in the extended configuration and to together enable the duct to maintain its substantial rigidity upon extension from the compacted configuration.
[0012] When a predetermined length of the duct is in the extended configuration and is disposed horizontally and supported at a first end thereof, the duct is fabricated to bend under the influence of gravitational force such that a second unsupported end thereof is lower than the first supported end by no more than a predetermined percentage of the predetermined length. Further, when a predetermined length of the duct is in the extended configuration and is disposed horizontally and supported at both ends thereof, the duct is fabricated to bend under the influence of gravitational force such that the central portion thereof is also lower than the level of the supported ends by no more than a predetermined percentage of the predetermined length, which, for a 2 meter length of a duct with a diameter of approximately 10 centimeters, will be less than 1 centimeter for an extended duct that was not compacted and less than 5 centimeters for a duct that was extended from the compacted configuration. Additionally, when the duct is in the extended configuration after having been compressed to the compacted configuration, the inward-facing surface of the first layer having metallic properties of the inner sleeve is substantially smooth and featureless except for the helical corrugations.
[0013] Further, both the inner sleeve and the outer sleeve include a first layer having metallic properties and a second, plastic layer, forming thereby, respectively, an inner two-layer laminate and an outer two-layer laminate, which are fabricated of fire-resistant and puncture-resistant materials. In all of the two-layer laminates, the layers are bonded together with a fire-retardant adhesive and the inner two-layer laminate is also bonded to the outer two-layer laminate with a fire-retardant adhesive. Additionally, the first layers having metallic properties of the inner two-layer laminate and the outer two-layer laminate are fabricated of aluminum ribbon of predetermined thicknesses and the second, plastic layers of the inner two-layer laminate and the outer two-layer laminate are fabricated of polyester ribbon of predetermined thicknesses, respectively bonded together to form thereby, respectively, an inner two-layer laminated tape of predetermined thickness and an outer two-layer laminated tape of predetermined thickness, and wherein the inner two-layer laminate is an inner helical wrapping with a predetermined overlap of the inner two-layer laminated tape and the outer two-layer laminate is an outer helical wrapping with a predetermined overlap of the outer two-layer laminated tape. Further, in the inner sleeve, the second plastic layer is disposed parallel to and about the first layer having metallic properties and in the outer sleeve, the first layer having metallic properties is disposed parallel to and about the second plastic layer. The first layer having metallic properties of the inner two-layer laminate is fabricated of aluminum ribbon of a thickness in the range of 6 to 12 microns, and the first layer having metallic properties of the outer two-layer laminate is fabricated of aluminum ribbon of a thickness in the range of 24 to 35 microns. The second plastic layers of both the outer and inner two-layer laminates are fabricated of polyester ribbon of a thickness in the range of 10 to 14 microns.
[0014] Additionally, the resilient helical element is fabricated of a metal having spring-like resilience, such as a coiled bronze-coated steel wire of a diameter in the range of 0.9 to 1.3 millimeters.
[0015] Further, in accordance with a preferred embodiment of the invention, the resilient helical element is aligned with the inner helical wrapping so that the coiled bronze-coated steel wire is approximately centered over the overlap of the inner helical wrapping of the inner two-layer laminated tape and the outer helical wrapping of the outer two-layer laminated tape is aligned with the resilient helical element so that the overlap of the outer helical wrapping of the outer two-layer laminated tape is approximately centered over the spaces between the wires of the coiled bronze-coated steel wire of the resilient helical element.
[0016] In accordance with a further embodiment of the invention, the duct also includes an insulating sheath fabricated of fiberglass, disposed parallel to and about the outer sleeve, and an enclosing jacket disposed parallel thereto and thereabout. The enclosing jacket is a multi-layer jacket including a tubular, plastic inner wrapping and a two-layer laminate outer wrapping, including a plastic inner layer and an outer layer having metallic properties, bonded together with a fire-retardant adhesive, disposed parallel and about the tubular, plastic inner wrapping and bonded thereto with a fire-retardant adhesive. The plastic inner wrapping is fabricated of polyester ribbon of predetermined thickness, and the plastic inner layer of the two-layer laminate outer wrapping is fabricated of polyester ribbon of predetermined thickness and the outer layer having metallic properties of the two-layer laminate outer wrapping is fabricated of aluminum ribbon of predetermined thickness. The insulating sheath is fabricated of fiberglass of a thickness in the range of 25 to 50 millimeters. The plastic inner wrapping is fabricated of polyester ribbon of a thickness in the range of 10 to 14 microns. The plastic inner layer of the two-layer laminate outer wrapping is fabricated of polyester ribbon of a thickness in the range of 10 to 14 microns, and the outer layer having metallic properties of the two-layer laminate outer wrapping is fabricated of aluminum ribbon of a thickness in the range of 6 to 9 microns.
[0017] There is further provided, in accordance with the present invention, a method for manufacturing a semi-rigid, flexible, duct of a preselected diameter for gas transport, including the steps of:
a) providing a mandrel of preselected diameter for fabricating a duct therearound; b) combining a first aluminum continuous ribbon of predetermined thickness in the range of 6 to 12 microns with a first polyester continuous ribbon of predetermined thickness in the range of 10 to 14 microns to form a first two-layer laminated continuous tape; c) combining a second aluminum continuous ribbon of predetermined thickness in the range of 24 to 35 microns with a second polyester continuous ribbon of predetermined thickness in the range of 10 to 14 microns to form a second two-layer laminated continuous tape; d) helically wrapping the first two-layer laminated continuous tape with a predetermined overlap around the mandrel with the first aluminum ribbon facing inward toward the mandrel and the first polyester ribbon facing outward with respect to the mandrel to form an inner two-layer sleeve; e) helically coiling a bronze-coated steel wire of a thickness in the range of 0.9 to 1.3 millimeters around the inner two-layer sleeve; and f) helically wrapping the second two-layer laminated continuous tape with a predetermined overlap around the inner two-layer sleeve and the bronze-coated steel wire coil with the second polyester ribbon facing inward toward the mandrel and the second aluminum ribbon facing outward with respect to the mandrel to form an outer two-layer sleeve disposed parallel to and about the inner two-layer sleeve.
[0024] Additionally, the step b) of combining a first aluminum ribbon includes the sub-step of applying a fire-retardant adhesive between the first aluminum ribbon and the first polyester ribbon to bond them together; and the step of c) combining a second aluminum ribbon includes the sub-step of applying a fire-retardant adhesive between the second aluminum ribbon and the second polyester ribbon to bond them together. Further, the step of b) combining a first aluminum ribbon further includes the sub-step of coating the polyester face of the first two-layer laminated continuous tape with a fire-retardant adhesive; the step c) of combining a second aluminum ribbon further includes the sub-step of coating the polyester face of the second two-layer laminated continuous tape with a fire-retardant adhesive; and in the step d) of helically wrapping the second two-layer laminated continuous tape, the outer two-layer sleeve is bonded to the inner two-layer sleeve with the bronze-coated steel wire helically coiled therebetween.
[0025] Additionally in accordance with the method of the present invention, the step e) of helically coiling a bronze-coated steel wire includes the sub-step of aligning the coiled wire with the overlap in the wrapping of the inner two-layer sleeve so that the coiled wire is approximately centered over the overlap in the wrapping of the inner two-layer sleeve, and the step f) of helically wrapping the second continuous two-layer laminated tape includes the sub-step of aligning the wrapping of the second continuous two-layer laminated tape so that the overlap in the wrapping of the outer two-layer sleeve is approximately centered over the spaces between the coils of wire.
[0026] Further in accordance with the method of the present invention, the steps d), e), and f) of helically wrapping the first two-layer laminated continuous tape, helically coiling the bronze-coated steel wire, and helically wrapping the second two-layer laminated continuous tape are performed by rotating the mandrel as the first two-layer laminated continuous tape, the bronze-coated steel wire, and the second two-layer laminated continuous tape are respectively deposited thereupon; and the steps d), e), and f) of helically wrapping the first two-layer laminated continuous tape, helically coiling the bronze-coated steel wire, and helically wrapping the second two-layer laminated continuous tape are performed continuously and simultaneously with predetermined phase differences, with respect to the rotation of the mandrel, therebetween. Namely, the steps d) and e) of helically wrapping the first two-layer laminated continuous tape and helically coiling the bronze-coated steel wire are performed continuously and simultaneously with a phase difference of 360 degrees, with respect to the rotation of the mandrel, therebetween; and the steps e) and f) of coiling the bronze-coated steel wire and helically wrapping the second two-layer laminated continuous tape are performed continuously and simultaneously with a phase difference of 120 degrees, with respect to the rotation of the mandrel, therebetween.
[0027] In accordance with an additional embodiment of the present invention, the method further includes, after the step f) of helically wrapping the second two-layer laminated tape, the steps of:
g) sheathing the outer two-layer sleeve with a fiberglass insulating sheath of a thickness in the range of 25 to 50 millimeters, disposed parallel thereto and thereabout; and h) enveloping the insulating sheath with an enclosing jacket.
Additionally, the step h) of enveloping includes the following sub-steps:
[0030] 1) providing a mandrel of preselected diameter for fabricating the enclosing jacket therearound;
2) combining a polyester continuous ribbon of predetermined thickness in the range of 10 to 14 microns with an aluminum continuous ribbon of predetermined thickness in the range of 6 to 9 microns to form a two-layer laminated continuous tape; 3) helically wrapping a polyester continuous ribbon of predetermined thickness in the range of 10 to 14 microns around the mandrel to form an inner plastic sleeve; and 4) helically wrapping the two-layer laminated continuous tape around the inner plastic sleeve with the polyester ribbon facing inward toward the mandrel and the aluminum ribbon facing outward with respect to the mandrel to form an outer two-layer sleeve disposed parallel to and about the inner plastic sleeve.
[0034] The sub-step 2) of combining includes the sub-sub-step of applying a fire-retardant adhesive between the polyester ribbon and the aluminum ribbon to bond them together, and the sub-step 3) of helically wrapping a polyester ribbon includes the sub-sub-step of coating the outer face of the inner plastic sleeve with a fire-retardant adhesive to bond it to the two-layer laminated tape.
[0035] Additionally, the sub-steps 3) and 4) of helically wrapping a polyester ribbon and helically wrapping the two-layer laminated tape are performed by rotating the mandrel as the polyester ribbon and the two-layer laminated tape are respectively deposited thereupon. Further, the sub-steps 3) and 4) of helically wrapping a polyester ribbon and helically wrapping the two-layer laminated tape are performed continuously and simultaneously with a predetermined phase difference, namely, of 360 degrees, with respect to the rotation of the mandrel, therebetween.
BRIEF DESCRIPTION OF THE DRAWINGS
[0036] The present invention will be more fully understood and appreciated from the following detailed description, taken in conjunction with the drawings, in which:
[0037] FIG. 1 is a side view of a segment of a duct, constructed and operative in accordance with an embodiment of the present invention;
[0038] FIG. 2 is a schematic axial cross-sectional view of the duct of FIG. 1 ;
[0039] FIG. 3 is a schematic oblique view of a segment of a duct that has been compressed;
[0040] FIG. 4 is a schematic oblique view of a duct similar to that shown in FIG. 1 , further including an insulating sheath, constructed and operative in accordance with a further embodiment of the present invention;
[0041] FIG. 5 is a schematic axial cross-sectional view of the duct of FIG. 4 ;
[0042] FIG. 6 is a schematic view of a duct, constructed and operative in accordance with an embodiment of the present invention, which is installed as an exhaust transition duct of a clothes dryer;
[0043] FIG. 7 is a schematic axial view of a duct such as that of FIG. 1 being fabricated according to the method of the present invention;
[0044] FIG. 8 is an enlarged detailed schematic cross-sectional view of a portion of the wall of a duct such as that of FIG. 1 ;
[0045] FIG. 9 is a schematic axial view of an enclosing jacket such as that of FIG. 5 being fabricated according to the method of the present invention;
[0046] FIG. 10 is a schematic representation of the vertical sag of the unsupported center of a segment of duct such as that of FIG. 1 supported at its ends;
[0047] FIG. 11 is a schematic representation of the vertical displacement from the horizontal of the unsupported end of a segment of duct such as that of FIG. 1 supported at its other end; and
[0048] FIG. 12 is a schematic representation of the fabrication of an insulated duct such as that of FIG. 5 .
DETAILED DESCRIPTION OF THE INVENTION
[0049] Referring now to the drawings, there are shown, in FIG. 1 , a side view of a segment of a duct, referred to generally as 100 , constructed and operative in accordance with a preferred embodiment of the present invention, and a schematic axial cross-sectional view thereof in FIG. 2 . Duct 100 , which is intended for use in a gas transport arrangement, is cylindrical, having an axis 150 , and is of multi-layer construction, as shown in detail in FIG. 2 . Duct 100 has inner and outer sleeves, referenced 220 and 230 , respectively, which are coaxial and are of a laminate construction, each preferably being formed of a helical wrapping of a two-layer laminated tape formed of two layers of ribbon, 222 , 224 , and 232 , 234 , respectively, bonded together with an adhesive layer 240 , 280 . Inner sleeve 220 has an internal layer of aluminum ribbon 222 and an external layer of polyester ribbon 224 bonded together with adhesive layer 240 to form a two-layer laminated tape which is helically wrapped around a mandrel ( 710 , see FIG. 7 , discussed hereinbelow) to form inner sleeve 220 . Coaxially coiled around inner sleeve 220 is a helical wire 250 , preferably of bronze-coated steel, disposed and encapsulated between inner sleeve 220 and outer sleeve 230 with a layer of adhesive 260 . Outer sleeve 230 is fabricated in a manner similar to inner sleeve 220 , but wherein, the helically wrapped two-layer laminated tape has an internal layer of polyester ribbon 234 and an external layer of aluminum ribbon 232 , bonded together with adhesive layer 280 . The helically coiled bronze-coated steel wire 250 imparts helical corrugations 160 to duct 100 , as can be seen in FIG. 1 .
[0050] Polyester ribbon layers 224 and 234 are both heat resistant and fire retardant and further are made thick enough to contribute to the rigidity and structural integrity of duct 100 together with aluminum ribbon layers 222 and 232 , which, being metallic, are fireproof as well. The adhesive employed in adhesive layers 240 , 260 , and 280 is also heat resistant and fire retardant. It should be noted that polyester ribbon layers 224 and 234 are also puncture resistant, which is a further advantage of the duct 100 of the present invention.
[0051] Duct 100 is manufactured fully extended by a continuous process, further described hereinbelow, and is then cut to a desired length. The corrugations 160 imparted thereto by helical wire 250 allow duct 100 to be axially compressed into a compact configuration convenient for storage or shipping. When duct 100 is compressed, as shown in FIG. 3 , aluminum layers 222 and 232 and polyester layers 224 and 234 naturally fold between the ridges (referenced 160 in FIG. 1 ) created by helical wire 250 . For example, a 2.4 meter length of 10 centimeter diameter duct fabricated in accordance with the present invention can be compressed to a length of approximately 15 centimeters, which is comparable to the compression of simple prior art ducts described hereinabove that do not have the advantages and improvements of the present invention.
[0052] A particular advantage of the unique, multilayered construction of the present invention is that duct 100 maintains its rigidity and structural integrity and functions like a totally rigid duct even after having been compressed to its compact configuration and re-extended to its original length. Referring now to FIG. 10 , there is shown, schematically, the vertical sag c of the unsupported center 210 of a horizontal segment of duct 200 spanning between two supports 215 a distance L apart. For example, for a length of duct that has been returned to its extended configuration after having been compressed, a 1.5 meter horizontal span of 10 centimeter diameter duct with no support in its center will substantially maintain its rigid shape and sag in the unsupported center by no more than 1 centimeter, while a similar 2 meter horizontal span of 10 centimeter diameter duct will sag in the unsupported center by no more than 5 centimeters. For a length of duct 100 that has not been compressed, a 1.5 meter horizontal span of 10 centimeter diameter duct that has no support in its center will maintain its rigid shape with negligible sag, while a 2 meter horizontal span of 10 centimeter diameter duct will sag in the unsupported center by no more than 1 centimeter. Referring now to FIG. 11 , there is shown, schematically, the vertical displacement y from the horizontal of one unsupported end 290 of a horizontal segment of duct 200 of length L, as a result of bending due to gravity, when the other end 295 has support 215 . Similarly, a vertically deployed segment of the duct of the present invention will maintain its rigidity, and not sag or collapse, even when returned to its extended configuration after having been compressed. As will be clear to those familiar with the art, these features represent a major improvement over the prior art, including solid aluminum corrugated tubes such as those employed in the invention of the Whitney patent (U.S. Pat. No. 5,281,187) discussed hereinabove.
[0053] Another advantage of the unique multilayered construction of the present invention is that when it is fully extended after compression, the inward-facing surface of the aluminum layer 222 of the inner sleeve 220 is substantially smooth and featureless except for the helical corrugations imparted by wire helix 250 . This reduces frictional resistance to air flow within the duct, and, for clothes dryer exhaust transition ducts, significantly impedes the accumulation of lint inside the duct, thereby greatly reducing the fire hazard cited hereinabove with respect to the prior art.
[0054] Referring again to FIG. 2 , in a preferred embodiment of the present invention in a typical product of the invention, duct 100 may have the following exemplary dimensions. The two-layer laminated tape of inner sleeve 220 has an inner aluminum ribbon layer 222 that is 7 microns thick and a polyester ribbon layer 224 that is 12 microns thick, so that, with the adhesive 240 , inner sleeve 220 has a thickness of 21 microns. The wire helix 250 is 0.9 mm diameter bronze-coated steel wire. The two-layer laminated tape of outer sleeve 230 has an outer aluminum ribbon layer 232 that is 25 microns thick and a polyester ribbon layer 234 that is 12 microns thick, so that, with the adhesive 280 , outer sleeve 230 has a thickness of 39 microns. The use of the thinner (7 microns) of aluminum ribbon layer 222 in inner sleeve 220 contributes to the above-mentioned smoothness of the inner surface of duct 100 . It should be noted that the above-mentioned dimensions are typical and are exemplary of a preferred embodiment of the present invention, and that the present invention is not limited thereto. It should further be noted that, with suitable dimensions for the other layers of the duct of the present invention, either polyester layer 224 of inner sleeve 220 or polyester layer 234 of outer sleeve 230 may be omitted without loss of the improvements in rigidity of the present invention, albeit at a cost of additional thickness of aluminum, resulting in additional weight and expense. As such, either of these alternative configurations should be considered as being included in the present invention, as well as alternative dimensions of the layers that can still provide the desired performance of duct 100 . Similarly, metallic layers or plastic layers fabricated of materials having properties comparable to those of the aluminum and polyester layers described hereinabove should also be considered as being included in the present invention.
[0055] Referring now to FIG. 4 . there is shown a schematic oblique view of a segment of a duct, referred to generally as 400 , A schematic axial cross-sectional view of duct 400 is shown in FIG. 5 . As shown in FIG. 5 , duct 400 is similar to that shown in FIG. 1 , but also includes an insulating layer 470 disposed parallel to and about outer sleeve 430 constructed and operative in accordance with a further preferred embodiment of the present invention. Additionally, insulating layer 470 has an enclosing jacket serving as a vapor barrier, referred to generally as 490 , disposed thereabout. Insulating layer 470 is typically fabricated of fiberglass, which provides the desired insulation and is fire resistant. Enclosing jacket 490 is formed of an inner helical wrapping of polyester ribbon 484 , bonded with a layer of heat and fire retardant adhesive 485 and an outer helical wrapping of a two-layer laminated tape having an inner layer of polyester ribbon 494 and an outer layer of aluminum ribbon 492 bonded together by a heat resistant and fire retardant adhesive 495 .
[0056] In a preferred embodiment of the present invention, insulating layer 470 and enclosing jacket 490 of duct 400 have the following dimensions. Depending on the application, insulating layer 470 typically may be either 25 or 50 millimeters in thickness. The wrapping of polyester ribbon 484 is 12 microns thick. The two-layer laminated tape of the outer helical wrapping has an inner polyester ribbon layer 494 that is 12 microns thick and an outer aluminum ribbon layer 492 that is 7 microns thick, so that, with the adhesive 495 , outer helical wrapping has a thickness of 21 microns. It should be noted that the above-mentioned dimensions are typical and are exemplary of a preferred embodiment of the present invention, and that the present invention is not limited thereto.
[0057] Enclosing jacket 490 is manufactured by a continuous process, similar to that of duct 100 , and is then cut to a desired length. Duct 400 is assembled from an insulating layer 470 cut to the desired length and an enclosing jacket 490 cut to the desired length, which are drawn onto a segment of uninsulated duct, similar to duct 100 , cut to the desired length.
[0058] Referring now to FIG. 6 , there is shown a schematic view of a duct 600 , constructed and operative in accordance with an embodiment of the present invention, installed as an exhaust transition duct of a clothes dryer 650 . Duct 600 is connected to dryer exhaust port 640 and has a vertical segment 660 and two right angle bends 670 connecting it to an outside exhaust port 680 , thereby allowing it to vent the exhaust gases of clothes dryer 650 . The features of the present invention discussed hereinabove, notably the rigidity and structural integrity and the reduced tendency to accumulate lint are particularly advantageous in applications such as this.
[0059] The advantageous properties of the duct of the present invention result both from its unique construction described hereinabove and from the method of manufacture thereof. Referring now to FIG. 7 , there is shown a schematic axial view of a duct, referred to generally as 700 , in accordance with the present invention being fabricated according to the method of the present invention. The size of the duct 700 being fabricated is determined by mandrel 710 which is rotated about its longitudinal axis 715 . Inner two-layer laminate tape 720 is helically wrapped with a predetermined overlap 828 ( FIG. 8 ) around mandrel 710 as it turns to produce the two-layer inner sleeve of duct 700 as a first step in forming duct 700 . Bronzed-coated steel wire 730 is helically coiled around the two-layer inner sleeve of duct 700 as mandrel 710 turns with the two-layer inner sleeve formed thereupon. Outer two-layer laminate tape 740 is helically wrapped with a predetermined overlap 848 ( FIG. 8 ) around the two-layer inner sleeve of duct 700 with bronzed-coated steel wire 730 coiled thereupon as mandrel 710 turns with the two-layer inner sleeve and the wire coil formed thereupon to produce the two-layer outer sleeve of duct 700 .
[0060] Referring now to FIG. 8 , there is shown an enlarged detailed schematic cross-sectional view of a portion of the wall of a duct, referred to generally as 800 , constructed in accordance with the present invention, being fabricated according to the method of the present invention. Inner two-layer laminate tape, referred to generally as 820 , is formed by combining an aluminum ribbon 822 with a polyester ribbon 824 by applying a fire-retardant adhesive 826 therebetween to bond them together. Similarly, outer two-layer laminate tape, referred to generally as 840 , is formed by combining a polyester ribbon 844 with an aluminum ribbon 842 by applying a fire-retardant adhesive 846 therebetween to bond them together. It should be noted that inner two-layer laminate tape 820 and outer two-layer laminate tape 840 are both prepared prior to their being helically wrapped around mandrel 710 ( FIG. 7 ) to fabricate duct 800 , and that inner two-layer laminate tape 820 is wrapped around the mandrel with the aluminum ribbon 822 side inward toward the mandrel and outer two-layer laminate tape 840 is wrapped around the mandrel with the polyester ribbon 844 side inward toward the mandrel. It should further be noted that inner two-layer laminate tape 820 and outer two-layer laminate tape 840 are each respectively helically wrapped with a predetermined partial overlap, 828 and 848 respectively, so that successive wrappings produce continuous inner and outer two-layer sleeves. Additionally, it should be noted that the wires of wire coil 830 are aligned approximately centered above the overlap 828 in inner two-layer laminate tape 820 , and the overlap 848 in outer two-layer laminate tape 840 is aligned approximately centered above the spaces between the wires of wire coil 830 , which has been found to enhance the strength and rigidity of duct 800 . Prior to inner two-layer laminate tape 820 and outer two-layer laminate tape 840 being helically wrapped around the mandrel to fabricate duct 800 , the outer, polyester ribbon 824 side of inner two-layer laminate tape 820 and the inner, polyester ribbon 844 side of outer two-layer laminate tape 840 are coated with a fire-retardant adhesive, such as with a rolling adhesive applicator, thereby allowing them to be bonded together with an adhesive layer 836 which also encapsulates bronzed-coated steel wire coil 830 there between, when all are wound around mandrel 710 ( FIG. 7 ) to fabricate duct 800 .
[0061] Returning now to FIG. 7 , it can be seen that both inner two-layer laminate tape 720 and outer two-layer laminate tape 740 , as well as bronzed-coated steel wire 730 , are all continuously and simultaneously wrapped and coiled, respectively, around mandrel 710 as it rotates. The wrappings and the coiling, while occurring simultaneously, are performed with predetermined phase differences, with respect to the rotation of mandrel 710 , between them. Thus duct 700 is fabricated in one continuous operation. In an exemplary preferred embodiment of the present invention, the phase difference between the wrapping of inner two-layer laminate tape 720 and the coiling of bronzed-coated steel wire 730 is 360 degrees or one complete rotation of mandrel 710 , and the phase difference between the coiling of bronzed-coated steel wire 730 and the wrapping of outer two-layer laminate tape 740 is 120 degrees or one third of a complete rotation of mandrel 710 about axis 715 .
[0062] For the insulated duct 400 of FIGS. 4 and 5 , enclosing jacket 490 is fabricated by a process analogous to that used to fabricate duct 700 described hereinabove. Referring now to FIG. 9 , there is shown a schematic axial view of an enclosing jacket, referred to generally as 900 , in accordance with the present invention being fabricated according to the method of the present invention. A two-layer laminate tape 940 with an inner polyester ribbon layer and an outer aluminum ribbon layer bonded with a fire-retardant adhesive is formed. A continuous inner plastic sleeve is produced by helically wrapping a polyester ribbon 920 around a rotating mandrel 910 of the desired diameter, and a continuous outer two-layer sleeve is produced by helically wrapping the two-layer laminate tape 940 around the inner plastic sleeve as the mandrel rotates, with a fire-retardant adhesive layer applied therebetween. Further as described hereinabove, enclosing jacket 900 is produced in one continuous operation, with continuous inner plastic sleeve and outer two-layer sleeve both wrapped around mandrel 910 continuously and simultaneously, with only a specific phase difference, with respect to the rotation of mandrel 910 , between them. In a preferred embodiment of the present invention, the phase difference between the wrapping of the inner plastic sleeve and that of the outer two-layer sleeve is 360 degrees or one complete rotation of mandrel 910 about axis 915 . In additional embodiments of the present invention, an additional tape of open-mesh laid fiberglass scrim may be wrapped between polyester ribbon 920 and two-layer laminate tape 940 in enclosing jacket 900 (not pictured).
[0063] To produce insulated duct 400 , a piece of continuously produced uninsulated duct 700 is cut to the desired length, and a piece of continuously produced enclosing jacket 490 is cut to the desired length. As shown schematically in FIG. 12 , the desired length piece of enclosing jacket 490 , together with an insulating fiberglass sheath 470 of the desired length and suitable inner and outer diameters, are drawn over the desired length piece of uninsulated duct 700 to produce the insulated duct 400 shown in FIGS. 4 and 5 .
[0064] It will further be appreciated by persons skilled in the art that the scope of the present invention is not limited by what has been specifically shown and described hereinabove, merely by way of example. Rather, the scope of the present invention is defined solely by the claims, which follow.
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A semi-rigid, flexible, duct for gas transport and for clothes dryer exhaust transition, and a method for manufacture thereof, including a pair of coaxial sleeves, an inner sleeve and an outer sleeve disposed parallel to and about the inner sleeve, and a resilient helical element disposed between them; wherein each of the inner sleeve and the outer sleeve includes a first aluminum layer and a second polyester layer, wherein the helical element imparts helical corrugations to the sleeves such that the duct is axially extendible between a compacted configuration suitable for storage and shipping and an extended configuration suitable for installation in a gas transport arrangement, and wherein all the layers of the sleeves are of a thickness predetermined to together render the duct substantially rigid when in the extended configuration and to together enable the duct to maintain its substantial rigidity upon extension from the compacted configuration.
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BACKGROUND
The invention relates to a control method for an internal combustion engine, in particular a Diesel engine, comprising an exhaust gas post-treatment system and a system for recirculating exhaust gases to the intake, the engine changing from a regeneration mode operation with throttling to a normal mode without throttling.
To meet emission control standards, internal combustion engines are equipped with post-treatment systems which trap and convert certain chemical compounds contained in the exhaust gases. Some post-treatment systems use an internal regeneration phase during which the operation of the engine is changed in order to establish favorable thermal and chemical conditions in the post-treatment system. These specific conditions promote the conversion of the chemical compounds which have been trapped in the post-treatment system.
These favorable conditions are usually obtained by reducing the performance of the engine by partial closing of the air intake circuit, which increases, particularly, the temperature of the exhaust gases.
Once the regeneration phase has passed, the aim is to open the air intake circuit as quickly as possible to limit the over-consumption of fuel and the transient production of certain chemical compounds contained in the exhaust gases.
However, for reasons of efficiency, these regeneration programs use high degrees of intake duct closure which create a significant reduction of the noise of the air intake circuit for the whole duration of the process.
At the end of the regeneration, by rapidly opening the intake ducts, the noise suddenly becomes loud again without the driver having changed the acceleration signal of the vehicle, which disturbs the auditory comfort of the occupants and may monopolize their attention.
BRIEF SUMMARY
The invention aims to improve on prior art systems and proposes to remedy their disadvantages, particularly to limit the perceived noise contrast, particularly at stable engine speed, when returning to a normal operation of the engine after a regeneration phase.
One object of the present invention is to provide an engine control method of the type mentioned above comprising a step in which the engine is made to operate temporarily in intermediate mode by carrying out a partial throttling to limit the intake noise contrast, at the end of the regeneration mode operation of the engine.
According to the particular embodiments, the control method for an internal combustion engine includes one or more of the following features:
the engine is made to change from an intermediate mode operation with partial throttling to a normal mode without throttling when at least one signal is detected, which masks the intake noise contrast by the change in the engine noise occurring in connection with the detection of the signal; the engine is made to change from an intermediate mode operation with partial throttling to a normal mode without throttling when an acceleration signal is detected, which masks the intake noise contrast by the change in the engine noise due to the change in the acceleration; the opening speed of an intake flap is controlled when switching from the regeneration mode with throttling to the intermediate mode with partial throttling, which optimizes the duration of the intermediate mode; in a first opening phase of the intake flap, there is a rapid change to a first partial throttling value corresponding to a first intake noise attenuation value, which reduces the duration of the intermediate mode; in a second opening phase of the opening flap, the opening speed of the flap is limited according to at least one intake noise rate-of-increase signal; in a third phase, the partial throttling value is maintained until an acceleration signal of the vehicle is applied, which ensures that the occupants do not perceive the intake noise contrast; the opening speed of the intake flap is made to vary according to a logarithmic function so that the rate of variation of the intake noise is generally constant; during the intermediate mode, the cross section of flow of the gases in the EGR system is reduced to lessen the contrast of the total noise emitted by the intake circuit, which improves the reduction of the total intake noise contrast; the engine is changed from an intermediate mode operation to a normal mode after a timed period, which ensures that it will be possible to return to the more economical normal mode after a certain preset period; and the timed period is adjusted according to an additional consumption value and/or a value for the production of certain chemical compounds during the intermediate mode.
BRIEF DESCRIPTION OF THE DRAWINGS
Other features and advantages of the invention will emerge clearly on reading the following description of the non-limiting embodiment of the invention, in connection with the attached drawings, in which:
FIG. 1 is a structural diagram of an engine on which the invention is used;
FIG. 2 is a graph showing the intake noise attenuation value obtained according to the closure of the intake flap;
FIG. 3 shows the intake noise variations with time for several throttling parameters in the various operating modes of the engine according to a first embodiment; and
FIG. 4 shows the intake noise variations with time for several throttling parameters in the various operating modes of the engine according to a second embodiment.
DETAILED DESCRIPTION
In the description which follows, it is understood that “throttling” refers to the action of reducing the cross section of flow of a gas which is introduced into a duct, for example an air intake duct in the engine. Moreover, “regeneration mode” refers to the operating mode of the engine in which an internal regeneration of the post-treatment systems is carried out with a throttling. A “normal mode” refers to an operating mode of the engine in which no regeneration and no throttling are carried out. Finally, an “intermediate mode” refers to an operating mode of the engine in which a partial throttling is carried out.
FIG. 1 illustrates the structure of an engine 1 on which the invention is used.
The engine 1 comprises an air intake circuit 2 and an exhaust circuit 3 . The intake circuit 2 has an air intake port 4 , through which enters the air which is brought to an air filter 6 through an intake duct upstream of the air filter 5 . The air continues its journey, through a duct upstream of a compressor 7 , to a compressor 8 , driven by a turbocharger 9 set in motion by exhaust gases. There the air is compressed and sent to an intercooler 11 via a duct upstream of the cooler 10 . After cooling, the air is brought through a duct located downstream of the cooler 12 to an air intake manifold 13 . The flow of air entering the manifold 13 is then adjusted by an intake flap 14 .
The air entering the engine 1 plays an active part in the internal combustion producing the exhaust gases which are discharged into the exhaust circuit 3 through an exhaust manifold 15 .
A first portion of the exhaust gases is recirculated to the intake to limit the emission of certain pollutants by an exhaust gas recirculation circuit 16 , called an “EGR circuit.” The quantity of exhaust gases recirculated is adjusted by a recirculation circuit valve 17 , called an “EGR valve.”
A second portion of the exhaust gases activates the turbo 9 then passes into an exhaust pipe 18 comprising an exhaust gas post-treatment system 19 .
The operation of the engine 1 creates a vibrational excitation which is propagated inside the air intake circuit 2 and which creates a noise called intake “roar.” At the time of the regeneration of the exhaust gas post-treatment systems 19 , when an air intake flap 14 closes at least partially the cross section of the circuit 2 , the propagation of the vibrational excitation coming from upstream is attenuated downstream of the flap 14 .
As illustrated in FIG. 2 , the attenuation of the level of intake roar increases with the throttling at the intake. More particularly, it can be seen on this graph that the level of attenuation of the intake noise follows an exponential curve according to the degree of closure of the intake flap 14 . It is therefore particularly advantageous to move this flap 14 according to a logarithmic speed setting in order that the rate of increase of the roar is linear.
This throttling also lessens noises of a lower intensity, downstream of the intake flap 14 , such as, for example, the vibrations and the noise produced by the components of the intake circuit 2 and the air filter 6 .
In the remainder of the description of the invention, intake noise will be mentioned to refer to the roar as well as the vibrations and the noise produced by the components of the intake circuit 2 , and generally any vibrational excitation which is propagated in the intake circuit 2 .
At the end of regeneration, the flap 14 opens the intake circuit 2 and the intake noise level noticeably increases. This increase is all the more disadvantageous as the circuit 2 is opened as quickly as possible to return to the normal mode and thus limit the over-consumption and the emission of certain pollutants. The transition is then clearly drawn to the attention of the occupants at the end of the regeneration phase, affecting their auditory comfort.
According to the invention, the engine is then put temporarily into an intermediate operating mode at the end of regeneration mode before returning to a normal mode without throttling. This intermediate mode limits the intake noise contrast. The intermediate mode next changes to the normal mode, when an acceleration signal is changed. This signal change can be either an acceleration signal or a deceleration signal.
The intermediate mode can also change to the normal mode when a manual or automatic transmission gear shift signal is detected.
It is also possible to use other signals corresponding to changes of sound levels, such as the radio volume or a fan speed for example.
In addition to the reduction of the intake noise contrast, the intermediate mode limits the over-consumption and the emission of certain pollutants compared to the regeneration mode. However, this intermediate mode remains less advantageous in terms of consumption and the production of certain chemical compounds than the normal mode. The aim is therefore to change to the normal mode as soon as possible, when the conditions ensure that the occupants will not be bothered by a high noise contrast.
FIG. 3 illustrates the intake noise variations with time for several throttling parameters in the various operating modes of the engine 1 , according to a first embodiment. The readings are carried out with a stable engine speed and load on the engine 1 .
When the engine 1 is operating in normal mode, without throttling, the intake noise level is high, and rises to a value H. In regeneration mode, the intake noise level only rises to a value B. A phase during which the engine is operating in an intermediate mode, during which the throttling is partial, is inserted between the end of regeneration mode and the change to normal mode. During this intermediate mode, the noise level gradually returns from the low value B to the high value H.
In a first period following the end of the regeneration mode, the noise level varies rapidly to return to a value I 1 of which the noise difference from B cannot be heard by the occupants, or, in other words, the value I 1 is a threshold value above which the rate of variation of the noise level must be limited so that the noise is not perceptible by the occupants. To do that, the intake circuit 2 is rapidly opened. For example, this value can be a value 10 dB less than the value H. This limits the duration for which the engine is operating at high levels of over-consumption, at the same time ensuring that the occupants cannot perceive, by ear, the end of the regeneration mode.
In a second period, the noise level is gradually raised from this value I 1 by the appropriate movement of the flap 14 . The speed of movement of the flap 14 is limited to a maximum speed, above which the occupant starts to perceive a rapid variation of the intake noise level.
This second period lasts until an acceleration signal of the vehicle is detected, from which the noise level increases rapidly by accelerating the movement of the flap 14 . Thus the intake noise contrast is successfully masked, by the change in noise perceived by the occupant when the acceleration signal of the vehicle changes.
According to a second embodiment, illustrated in FIG. 4 , the intermediate mode in which the engine 1 is operating between the regeneration mode and the normal mode comprises additional steps compared with the first embodiment. The readings are carried out with a stable engine speed and load on the engine 1 .
In a first period following the end of the regeneration mode, the noise level varies rapidly to return to the value I 1 . The value I 1 is a threshold value above which the rate of variation of the noise level must be limited so that the noise is not perceptible by the occupants. To do that, the intake circuit 2 is opened rapidly. For example, this value can be a value 10 dB less than the value H. This limits the duration for which the engine is operating at high levels of over-consumption, at the same time ensuring that the occupants do not perceive, by ear, the end of the regeneration mode.
In a second period, the noise level is gradually raised from this value I 1 by the appropriate movement of the flap 14 up to a value I 2 , which is a second threshold value. This value I 2 is, for example, a noise level associated with a limited adjustment of the combustion above which the over-consumption and the production of chemical compounds compared with the normal mode is acceptable.
In a third period, the movement of the intake flap 14 is blocked, so that the intake noise level remains constant and equal to 12.
This third period continues until the detection of an acceleration signal of the vehicle, from which the noise level increases rapidly by increasing the speed of movement of the flap 14 . Thus the intake noise contrast is successfully masked by the change in noise perceived by the occupant when the acceleration signal of the vehicle changes.
It is apparent from the foregoing that the system according to this second embodiment has many advantages, provided that the difference between the high H and low B noise levels is very great and that the rate of variation of the intake noise is small, which results in a period in which the engine remains in the intermediate mode for a very long time.
According to a third embodiment, during the intermediate mode, the throttling carried out at the intake flap 14 results in an adjustment of the opening signal of the EGR valve 17 of the recirculation circuit 16 .
In regeneration mode, the opening of the EGR valve 17 is smaller that its opening in normal mode. When this EGR valve 17 is open, pulses from the exhaust are partially transmitted to the intake circuit 2 . It follows that for certain operating phases of the engine 1 , the EGR circuit 16 plays an active part in the intake noise contrast when the regeneration mode changes to the normal mode.
When the engine is operating in intermediate mode, with partial throttling of the intake flap 14 , the proportion of air in the air/fuel mixture which plays an active part in the combustion is lower. The EGR valve 17 then has a smaller opening compared with the normal mode operation, with the aim of adjusting the proportions of the air/fuel mixture and limiting the exhaust emission of certain chemical compounds.
In this intermediate mode, the EGR valve 17 is in a position of partial throttling which lessens the contribution of the EGR circuit to the intake noise contrast when the regeneration mode changes to the normal mode.
What is more, according to the invention, it is understood that it is not limited to cases in which the EGR gases are taken from the exhaust manifold. For example, it is possible to take the gases for the EGR system downstream of an exhaust gas post-treatment system.
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A control method for an internal combustion engine including an exhaust gases post-processing system and a system for recirculating the exhaust gases towards the intake, wherein the engine can be switched from a regeneration operation mode with throttling to a nominal mode without throttling. At the end of the engine operation in the regeneration mode, the engine is temporarily operated in an intermediate mode with partial throttling for limiting the contrast of the intake noise.
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[0001] This application claims the benefit of priority European patent application no. 03 026 546.6-2114 filed Nov. 18, 2003, which is incorporated herein by reference in its entirety for all purposes.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to a novel method for the preparation of atorvastatin adsorbates and hydrates or solvates thereof, respectively. In an especially preferred embodiment the atorvastatin adsorbates according to the present invention comprise the active pharmaceutical ingredient in a finely dispersed amorphous form. According to the invention it is especially preferred that the active pharmaceutical ingredient is an alkaline earth metal salt, especially a hemicalcium salt as well as hydrate forms thereof.
[0003] Further, the invention relates to atorvastatin adsorbates and hydrates or solvates thereof, respectively, which are obtainable according to the afore-mentioned method.
[0004] Finally, the invention also relates to pharmaceutical formulations for the preparation of which the afore-mentioned atorvastatin adsorbates are used. Preferred drug forms according to the invention are tablets, capsules, pellets and granulates which are produced by usual pharmaceutically acceptable adjuvants in a manner known in itself. Tablets which rapidly release the active pharmaceutical ingredient and which are produced by direct pressing of the atorvastatin adsorbates according to the invention are especially preferred according to the invention.
[0005] The active pharmaceutical ingredient known as the INN atorvastatin is also known by the chemist as calcium salt of [R-(R*,R*)]-2-(4-fluorophenyl)-β,δ-dihydroxy-5-(1-methylethyl)-3-phenylphenylamino)carbonyl]-1H-pyrrol-1-heptanoic acid. This active pharmaceutical ingredient is an excellent inhibitor of the enzyme 3-hydroxy-3-methylglutaryl-(coenzyme A)-reductase I, also known by the acronyme HMG-CoA-reductase; thus it is usable as hypolipidemic and hypocholesterolemic active pharmaceutical ingredient for the therapy of lipidic metabolic disorders.
[0006] Thus HMG-CoA-reductase inhibitors are used successfully for preventing and for treating coronary heart diseases and other diseases being based on arteriosclerotic vascular changes. Thereby a significant lipid reduction, especially of the cholesterol, into the plasma can be achieved by various action modes (see e.g. Milestones in Drug Therapy/HMG-CoA-Reductase Inhibitors, Ed. G. Schmitz and M. Torzewski, Birkhauser Verlag Basel-Boston-Berlin [2002]).
[0007] The chemical structure of the atorvastatin was described in its racemic form for the first time in EP 247 633. The hemicalcium salt of the active [R-(R*,R*)] form used as active pharmaceutical ingredient was disclosed for the first time in EP 409 281 and was described as solid; but this document does not include a disclosure relating to a possible crystallinity of the product.
[0008] The production of the atorvastatin and important intermediates such as the lactone precursor of the atorvastatin is mentioned in various patent specifications, e.g. in EP 330 172, EP 553 213, EP 687 263, EP 915 866, EP 1 054 860, WO 99/57109, WO 01/72706, WO 02/55519.
[0009] It is known from the state of the art that atorvastatin in form of its hemicalcium salt does not only exist as amorphous solid, as described already by EP 409 281, but can also be obtained in more than 30 crystalline polymorphous forms.
[0010] Thus WO 97/03958 as well as WO 97/03959 filed at the same time describe the crystalline forms III as well as I, II and IV of the hemicalcium salt of the atorvastatin. While the form III is obtained by incubation of the form II for 11 days in an atmosphere having a moisture content of 95%, the forms I, II and IV can all be obtained from methanol or from methanol-water mixtures in various mixing ratios and at different temperatures. Very often the desired polymorphous form according to these documents can indeed only be obtained by a massive use of seed crystals.
[0011] WO 01/36384 discloses the polymorphous form V of the atorvastatin in form of its hemicalcium salt which is also obtained from a methanol-water mixture.
[0012] Also, WO 02/57229 describes a polymorphous form V of the atorvastatin obtained by stirring a suspension of raw atorvastatin hemicalcium in a mixture of water and absolute ethanol in the ratio of 14:3. However, according to the characterizations disclosed by the documents these two forms are different.
[0013] WO 02/41834 describes the polymorphous form VII of the atorvastatin in form of its hemicalcium salt which can be obtained by stirring a suspension of the polymorphous form V or the polymorphous form I of the atorvastatin in form of its hemicalcium salt in absolute ethanol at room temperature.
[0014] WO 02/43732 discloses the polymorphous forms VI, VIII, IX, X, XI and XII of the atorvastatin in form of its hemicalcium salt, wherein the form VI can be obtained from aqueous acetone, the form VIII can be obtained from ethanol or from n-butanol, the form IX can be obtained from ethanol or from n-butarol, the form X can be obtained from aqueous ethanol, the form XI can be obtained from methyl ethyl ketone and the form XII can be obtained from aqueous ethanol. In case of similar solvents it is found that the obtainment of a certain polymorphous form is dependent on minorly changed conditions such as different temperatures or a special water content.
[0015] WO 02/51804 uses a terminology (for describing the polymorphous forms of the atorvastatin) being different to the above patent documents. It describes the polymorphous forms X, A, B1, B2, C, D and E of the atorvastatin in form of its hemicalcium salt, wherein the form X can be obtained from methanol and methyl-t-butylether, the form A can be obtained from isopropanol containing traces of water, the form B1 can be obtained from an acetonitrile-THF mixture, the form B2 can be obtained from pure acetonitrile, the form C can be obtained from aqueous isopropanol, the form D can be obtained from ethanol and the form E can be obtained from methyl ethyl ketone by precipitating by peptone. Here it is also found that minor changes in the other conditions already lead to crystallization of another polymorphous form for the same solvents.
[0016] Finally, WO 03/04470 describes the polymorphous forms V, VI, VII, VIII, IX, X, XI, XII, Xm, XIV, XV, XVI, XVII, XVIII and XIX of the atorvastatin in form of its hemicalcium salt, wherein the form V characterized as trihydrate is obtained from aqueous acetonitrile, the form VI is obtained from aqueous DMF, the form VII characterized as sesquihydrate is obtained from aqueous acetone, the form VIII being a dihydrate is again obtained from aqueous DMF, and the form IX is again obtained from aqueous acetone. The form X being a trihydrate is obtainable from aqueous isopropanol, the form XI is again obtainable from aqueous acetonitrile, the form XII is obtainable from THF containing water, the form XIII is obtainable from aqueous methanol and the form XIV being a hexahydrate is again obtainable from aqueous isopropanol. The form XV being described as trihydrate arises from aqueous acetone, the form XVI being described as tetrahydrate-acetonitrile solvate arises from aqueous acetonitrile. The form XVIII being a solvate arises from a DMF-water-acetonitrile mixture and the form XIX also being a solvate arises from methyl-ethyl-ketone. Finally, the form XVII being a tetrahydrate is obtained by drying the form XVI for a long time. Also it will be apparent again from this disclosure that minor changes of the crystallization conditions can lead to other polymorphous forms for the use of the same solvent systems. Also it is found in this patent document, as described in the above cited disclosures, for a crystallization of the atorvastatin hemicalcium salt, that the formation of defined polymorphous forms is also strongly dependent on the starting polymorph, possibly also on seed crystals and on the different drying conditions.
[0017] In summary, it is found that the crystallization of atorvastatin hemicalcium in a defined polymorphous form is extraordinarily strongly dependent on minorly changed process parameters leading to a very costly process control since such a defined polymorph has to be absolutely guaranteed for a pharmaceutically active pharmaceutical ingredient to meet the regulatory requirements for medicaments and obviously also to ensure the constant quality of the medicament, and thus, the taking security for the patients.
[0018] A possibility to solve this problem and to reach a more advantageous isolation process is the use of amorphous atorvastatin hemicalcium. For obtaining the amorphous form several methods are described in prior art, e.g. in EP 839 132: from a solution of the active pharmaceutical ingredient in a THF-toluene mixture by removing the solvent, in EP 1 185 264: from a solution of the active pharmaceutical ingredient in THF by precipitating the product by heptane or according to EP 1 235 800 by “recrystallization” of the active pharmaceutical ingredient by lower alcohols.
[0019] The use of amorphous atorvastatin hemicalcium as active pharmaceutical ingredient in pharmaceutical formulations involves on the one hand the problem of the lower stability of the amorphous form in comparison to crystalline active pharmaceutical ingredient to surrounding conditions such as oxygen, light, heat, and residual humidity, as well as the higher sensitivity in relation to stability-reducing interactions with pharmaceutical adjuvants and additives. So it is e.g. known that atorvastatin hemicalcium in the presence of humidity and slightly acid-reacting substances very easily converts into the atorvastatin lactone which can lead to a non-acceptable active pharmaceutical ingredient decrease in the finished tablet. Mostly, to prevent the influence of such reactions in the finished drug alkalinizing additives such as special alkali and alkaline earth compounds, alkaline buffering systems (see, e.g., U.S. Pat. No. 5,180,589, U.S. Pat. No. 5,686,104, WO 00/35425 and WO 01/93859) or also the use of polymeric compounds having amido or amino groups (polyvinylpyrrolidone or cholestyramine, see WO 01/76566) for stabilization have been proposed. Also, a combination of both stabilization kinds (sodium hydroxide plus polyvinylpyrrolidone) has been used for analogous statin compounds (WO 98/57917).
[0020] A further problem of the use of amorphous atorvastatin hemicalcium as active pharmaceutical ingredient is the fact that, according to the experimental experiences of the inventors of the present application, there are during the precipitation process of the amorphous form often also heterogeneous products obtained: one part crystalline and another part amorphous, which leads to the precipitation process having to be repeated. But each additional production step poses the risk of a lost of substance of approx. 5% to 10%, being certainly not desired from an economic point of view for active pharmaceutical ingredients such as atorvastatin hemicalcium which has to be produced in a lengthy, costly and expensive synthesis series.
[0021] However, there is known from DE 10008506 A1 a method for producing an active pharmaceutical ingredient granulate for an analogous statin active pharmaceutical ingredient, namely cerivastatin, avoiding such a loss of substance, wherein an exclusively aqueous active pharmaceutical ingredient solution is directly granulated in the presence of a filler and a binder, and the so-obtained granulates are further processed after drying in tablets. But for the problem existing in the present case in relation to the active pharmaceutical ingredient atorvastatin hemicalcium, it is not a technically performable solution, because the active pharmaceutical ingredient is present in a maximum amount of 0.5% (w/w) in the granulates described by DE 10008506 A1. For therapeutic dosage of the atorvastatin hemicalcium the active pharmaceutical ingredient amount has to range between 20 mg and 80 mg. This would according to the disclosure of the DE 10008506 A1 lead to tablet weights between 4 and 16 g. The range acceptable for tablets being suitable for oral use, i.e. which have to be swallowed by the patient, ranges between 100 mg and 1 g.
[0022] Therefore, the known methods for producing pharmaceutical formulations of the atorvastatin hemicalcium are, insofar they can be performed, technically very costly, lengthy and expensive and do not solve the problem of a stable drug until now or do not solve it satisfactorily. The latter especially applies to the atorvastatin hemicalcium being preferred due to its better producibility and due to good dissolution properties and it has a high specific surface, i.e., especially amorphous or finely powdered. In such cases the stabilizations of prior art being described above are not sufficient.
[0023] Therefore, it is the object of the present invention to develop a simple and cheap method for producing stable atorvastatin powder systems which can be used directly for producing pharmaceutical formulations, wherein this method is however not limited to an especially preferred active pharmaceutical ingredient morphology, and avoids the afore-mentioned disadvantages.
SUMMARY OF THE INVENTION
[0024] Accordingly, the present invention provides a method for the preparation of atorvastatin adsorbates and solvates thereof, comprising the steps of starting from a solution of atorvastatin or one of its salts, hydrates, solvates, esters, lactones and tautomeric derivatives thereof in at least one organic solvent having a total water content of not more than 10 vol.-%, preferably not more than 5 vol.-%,
suspending therein an adsorber material selected from the group consisting of celluloses, cellulose derivatives, polyols, sugars, sugar derivatives, maltodextrins, cyclodextrins, starches, polydextroses or mixtures thereof, and removing the solvent by drying.
[0028] In a preferred embodiment of the invention the atorvastatin adsorbates comprise the active pharmaceutical ingredient in a finely dispersed amorphous form, especially as calcium salt. The amorphous atorvastatin according to the present invention can be both in water-free form and in form of solvates or hydrates, respectively.
[0029] Further, the invention relates to the atorvastatin adsorbates and solvates or hydrates thereof, respectively, which are obtainable by the afore-mentioned method. Further, the invention relates to pharmaceutical formulations comprising the novel atorvastatin adsorbates. The pharmaceutical formulations optionally comprise further adjuvants and can be converted into the desired administration form. Tablets rapidly releasing the active pharmaceutical ingredient and being produced by direct pressing are especially preferred.
DETAILED DESCRIPTION OF THE INVENTION
[0030] For the inventive method for the preparation of the atorvastatin adsorbates organic solvents are suitable for the solution comprising the pharmaceutically active pharmaceutical ingredient.
[0031] Especially, the organic solvents are selected from the group of the lower alkanols having 1 to 4 carbon atoms, the group of the ethers and the group of the aliphatic ketones and mixtures of the afore-mentioned solvents. Methanol, ethanol, isoproponol, n-propanol, acetone and other solvents such as ethyl acetate, methyl ethyl ketone, MTBE (methyl-tert-butylester) and mixtures of ethyl acetate and hexane as well as mixtures of the afore-mentioned solvents are especially preferred.
[0032] Pharmaceutically acceptable adjuvants which are suitable for rapid active pharmaceutical ingredient release such as celluloses and cellulose derivatives, especially microcrystalline cellulose, polyols, especially mannitol, sugars and sugar derivatives, especially lactose, maltodextrin, starches, cyclodextrins, polydextroses or mixtures of the afore-mentioned substances are according to the invention used as absorber materials. Microcrystalline cellulose, lactose and mannitol are preferred according to the invention.
[0033] According to the present invention the ratio of the pharmaceutical active pharmaceutical ingredient and adsorber material is in the range of 1:0.1 to 10, wherein a range of 1:1 to 1:2 is especially preferred.
[0034] For the preparation of the pharmaceutical formulations, while tablets being especially preferred, all common pharmaceutical adjuvants can be used. E.g. celluloses and cellulose derivatives (e.g. microcrystalline cellulose, native cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, methyl cellulose), sugars (e.g. lactose, fructose, saccharose, glucose, maltose), sugar alcohols (e.g. lactide, mannitol, sorbitol, xylitol), inorganic fillers (e.g. calcium phosphates and calcium sulfates) and starches (e.g. corn starch, potato starch, wheat starch, dextrins, pregelatinized starches) can be used as fillers. In addition, all further adjuvants such as lubricants, decomposition auxiliaries, wetting agents, alkaline additives, stabilizers as well as aromatics, colour pigments and colours being known by those skilled in the art due to their galenical basic knowledge can be used for producing the medicament formulations according to the invention.
[0035] The amount of binder in the whole mixture of the medicament preparation is preferably 0 to 20% (m/m), the amount of fillers and adjuvants in the whole mixture is 20 to 99%, preferably 50 to 99%.
[0036] Surprisingly stable adsorbates of atorvastatin, especially amorphous atorvastatin, are produced by the method according to the invention. These atorvastatin adsorbates are used as pharmaceutically active pharmaceutical ingredient in the preparations according to the invention. Preferably atorvastatin in form of its salts is used within the scope of this invention. Examples of the atorvastatin salts used according to the invention are the monosodium and the monopotassium salts as well as the magnesium and calcium salts as well as the hydrates and solvates thereof. Especially preferably are the atorvastatin hemicalcium salt and the hydrates and solvates thereof.
[0037] Further, the respective hydrates, solvates, esters, lactones and tautomeric derivatives of the atorvastatin which can especially arise within the scope of the production of the active pharmaceutical ingredient in solution can be used within the scope of this invention avoiding the isolation of the pure active pharmaceutical ingredient.
[0038] According to the invention there has been found a method starting from a solution of the atorvastatin or one of its salts, hydrates, solvates, esters, lactones and tautomeric derivatives in organic solvent and leading to active pharmaceutical ingredient absorbates which can directly be processed further.
[0039] In principle the active pharmaceutical ingredient solution of atorvastatin can be produced in an embodiment of the invention by dissolving the atorvastatin or one of its salts, hydrates, solvates, esters, lactones and tautomeric derivatives in a suitable organic solvent; however, it is advantageous to directly use the active pharmaceutical ingredient solution anyway arising within the scope of the synthesis without isolation of the atorvastatin.
[0040] For example the atorvastatin can be produced according to the EP 409 281 A1, Example 10, done then without the recrystallization step by dissolving in ethyl acetate and precipitating by hexane, and instead the adsorber material is suspended in the active pharmaceutical ingredient solution, and the solvent is later removed by drying. Then the kind of the organic solvent results in the individual case from the final synthesis step of the active pharmaceutical ingredient production.
[0041] To this organic active pharmaceutical ingredient solution a pharmaceutically acceptable adjuvant is added which is not soluble or low soluble therein as adsorber material, well wetted and the solvent is removed immediately thereafter by drying. The drying operation can be supported by temperature control and vacuum. It is advantageously performed so that a uniform distribution is done by suitable mechanical influence (rotating, staggering, stirring motion). The solvent can be recovered by working in closed system and employed again for the following process. It is a property of the invention that a precipitation and isolation of the atorvastatin is lapsed. Atorvastatin containing adsorbates produced according to the method described can be employed directly for subsequent processing to drug forms such as tablets, capsules, pellets or granulates, preferably for subsequent processing by means of a direct compression method.
[0042] Optionally the adsorbates or drug forms so obtained can further be provided with coatings of pharmaceutical polymethacrylates such as films of Eudragit®, methyl cellulose, ethyl celluloses, hydroxypropyl methyl celluloses, cellulose acetate phthalates and/or shellac for special uses to achieve a special use purpose, e.g. controlled release of active pharmaceutical ingredient, taste covering. For this purpose, there exist sufficient technical possibilities which are at the disposal for those skilled in the pharmaceutical art.
[0043] Surprisingly, it was found that the adsorbates produced according to the method of the invention bind the active pharmaceutical ingredient without forming crystal structures typical for active pharmaceutical ingredients. This could be shown by means of x-ray diffraction measurements. Additionally, comparing stability studies show that the preferred atorvastatin adsorbates have a better stability and a faster dissolution rate than the pure amorphous active pharmaceutical ingredient. Special adsorber materials, e.g. on basis of silica have stronger binding properties, and therefore another release behaviour for the adsorbed atorvastatin.
[0044] Particularly, the mentioned properties are also maintained when the atorvastatin adsorbates are processed to drug forms such as tablets.
BRIEF DESCRIPTION OF THE DRAWINGS
[0045] The invention is further described by the following non-limiting examples which refer to the accompanying FIGS. 1 to 11 , short articulars of which are given below.
[0046] FIG. 1 a powder x-ray diffraction diagram of an atorvastatin-microcrystalline cellulose adsorbate according to the invention (in the ratio of 1:1) in the upper curve as well as microcrystalline cellulose alone in the lower curve as comparison,
[0047] FIG. 2 a powder x-ray diffraction diagram of an atorvastatin-mannitol adsorbate according to the invention (in the ratio of 1:1) in the upper curve as well as mannitol alone in the lower curve as comparison,
[0048] FIG. 3 a powder x-ray diffraction diagram of an atorvastatin-lactose adsorbate according to the invention (in the ratio of 1:1) in the upper curve as well as lactose alone in the lower curve as comparison,
[0049] FIG. 4 a powder x-ray diffraction diagram of an atorvastatin-microcrystalline cellulose adsorbate according to the invention (in the ratio of 1:1.5) in the upper curve as well as microcrystalline cellulose alone in the lower curve as comparison,
[0050] FIG. 5 a powder x-ray diffraction diagram of an atorvastatin-mannitol adsorbate according to the invention (in the ratio of 1:1) in the upper curve as well as mannitol alone in the lower curve as comparison,
[0051] FIG. 6 a powder x-ray diffraction diagram of an atorvastatin-microcrystalline cellulose adsorbate according to the invention (in the ratio of 1:2) in the upper curve as well as microcrystalline cellulose alone in the lower curve as comparison,
[0052] FIG. 7 a powder x-ray diffraction diagram of crystalline atorvastatin (so-called form I, cf. WO 97/03959 A1) in powder mixture ratio with microcrystalline cellulose of 1:1 as well as microcrystalline cellulose alone in the lower curve as comparison,
[0053] FIG. 8 a powder x-ray diffraction diagram of crystalline atorvastatin (so-called form V, cf. WO 01/36384 A1) in powder mixture ratio with microcrystalline cellulose of 1:1 as well as microcrystalline cellulose alone in the lower curve as comparison.
[0054] FIG. 9 an FTIR spectrum of an atorvastatin-microcrystalline cellulose adsorbate according to the invention (in the ratio of 1:1),
[0055] FIG. 10 an FTIR spectrum of an atorvastatin-mannitol adsorbate according to the invention (in the ratio of 1:1), and
[0056] FIG. 11 an FTIR spectrum of a atorvastatin-lactose adsorbate according to the invention (in the ratio of 1:1).
EXAMPLES 1 TO 6
[0057] Used industrial equipment for the analytic studies:
[0000] HPLC Measurements:
[0058] All HPLC measurements were performed with an Agilent 100-HPLC.
Column used: Inertril ODS 2.5μ (150 × 4.6 mm) Mobile phase: 55% of 0.05 M sodium acetate 54% of acetonitrile pH: 4.0 (adjustment by acetic acid) Flow rate: 1 ml min −1 Detector: UV at 246 nm Injection volume: 20 ml Retention time atorvastatin: approx. 15 min Analysis duration: 60 min
X-Ray Measurements:
[0059] All powder x-ray diffraction diagrams were measured as follows:
Appliance: STADI P transmission diffractometer Cu-Ka l radiation (l = 1,54056 Å), U = 40 kV, I = 35 mA Primary ray monochromatic illuminator (crooked Ge 111) Detector: Linear position sensitive Width of slit: 1 mm Linear PSD: 2θ = 2° to 34°, 25 s/0.2° stepwise, increment Δ2θ = 0.02 Sample: Powder in mylar film
[0060] IP Spectra:
Appliance: GENESIS II FTIR spectrometer Measuring method: KBr pressed part having 1% of test substance
[0061] The spectra are shown as transmission values (in %) in dependence on the wave number (cm −1 ).
EXAMPLE 1
Atorvastatin-Microcrvstalline Cellulose Adsorbate
[0062] To a solution of heterogeneous atorvastatin hemicalcium in acetone (0.15 g/mL) are added 0.15 g/mL of microcrystalline cellulose (CelphereSCP-100′) and uniformly suspended. Then, the solvent is dried up under permanent motion and vacuum (rotary evaporator or asymmetric moved dryer) at 25° C. Finally, the mixture is post-dried at 35° C. for a short time for removing residual solvent.
[0063] Active pharmaceutical ingredient amount of the adsorbate by means of HPLC: 49.6% (theoretically 50%)
Powder x-ray diffraction diagram: FIG. 1
[0065] Impurity profile: Sum of all the impurities: HPLC, in %:
Start 15 days (70° C./75% relative humidity) Sample (adsorbate) 0.76 1.11 Comparison (amorphous 1.07 1.92 atorvastatin calcium) Tablet 0.77 1.07
[0066] Atorvastatin tablets were produced from the adsorbate by direct pressing according to following composition:
Atorvastatin-microcrystalline cellulose adsorbate 80 mg Microcrystalline cellulose (CelphereSCP-100 ®) 408 mg Adjuvants (Croscarmellose sodium, sodium laurylsulfate, 72 mg silica, magnesium stearate) in the usual amounts
[0067] The used amounts of the further adjuvants are known by those skilled in the art due to their basic knowledge and can be taken from standard works for formulating tablets, e.g. Ritschel et al., die Tablette, Editio Cantor—Aulendorf, 2. Auflage [2002].
[0068] Properties of the mixture ready for pressing and the tablet:
Compressibility and flowability: good Medium hardness 142 N Attrition: 0.06% (determined according to Ph. Eur.) Decay period: 40 sec. (determined according to Ph. Eur.) Release: 100% after 5 min. (Ph. Eur., 1000 mL water, 37° C., paddle 75 rpm)
[0069] The so-obtained tablets can be provided with a coating, if required.
EXAMPLE 2
Atorvastatin-Mannitol Adsorbate
[0070] To a solution of heterogeneous atorvastatin hemicalcium in acetone (0.15 g/mL) are added 0.15 g/mL of mannitol (Mannogern®) and uniformly suspended. Then the solvent is dried up under permanent motion and vacuum (rotary evaporator or asymmetric moved dryer) at 25° C. Finally the mixture is post-dried at 35° C. for a short time for removing residual solvent.
[0071] Active pharmaceutical ingredient amount of the adsorbate by means of HPLC: 49.85% (theoretically 50%)
Powder x-ray diffraction diagram: FIG. 2
[0073] Impurity profile (Sum of all the impurities, HPLC, in %):
Start 15 days (70° C./75% relative humidity) Sample (adsorbate) 0.91 1.40 Comparison (amorphous 1.07 1.92 atorvastatin calcium) Tablet 0.85 1.01
[0074] Atorvastatin tablets were produced from the adsorbate by direct pressing according to following composition:
Atorvastatin-mannitol adsorbate 80 mg Mannitol 408 mg Adjuvants (as in Ex. 1) 72 mg
[0075] Properties of the mixture ready for pressing and the tablets:
Compressibility and flowability: satisfactory till good Medium hardness 153 N Attrition: 0.18% (determined according to Ph. Eur.) Decay period: 65 sec. (determined according to Ph. Eur.) Release: 100% after 7 min. (Ph. Eur., 1000 mL water, 37° C., paddle 75 rpm)
[0076] The so-obtained tablets can be provided with a coating, if required.
EXAMPLE 3
Atorvastatin-Lactose Adsorbate
[0077] To a solution of heterogeneous atorvastatin hemicalcium in acetone (0.15 g/mL) are added 0.15 g/mL of lactose (Lactopress® Anhydrous) and uniformly suspended. Then the solvent is dried up under permanent motion and vacuum (rotary evaporator or asymmetric moved dryer) at 25° C. Finally, the mixture is post-dried at 35° C. for a short time for removing residual solvent.
[0078] Active pharmaceutical ingredient amount of the adsorbate by means of HPLC: 51.18% (theoretically 50%)
Powder x-ray diffraction diagram: FIG. 3
[0080] Impurity profile (Sum of all the impurities, HPLC, in %):
Start 15 days (70° C./75% relative humidity) Sample (adsorbate) 0.80 1.03 Comparison (amorphous 1.07 1.92 atorvastatin calcium) Tablet 0.79 1.05
[0081] Atorvastatin tablets were produced from the adsorbate by direct pressing according to following composition:
Atorvastatin-lactose adsorbate 80 mg Lactose 408 mg Adjuvants (as in Ex. 1) 72 mg
[0082] Properties of the mixture ready for pressing and the tablets:
Compressibility and flowability: satisfactory till good Medium hardness 138 N Attrition: 0.18% (determined according to Ph. Eur.) Decay period: 80 sec. (determined according to Ph. Eur.) Release: 100% after 8 min. (Ph. Eur., 1000 mL water, 37° C., paddle 75 rpm)
[0083] The so-obtained tablets can be provided with a coating, if required.
EXAMPLE 4
Atorvastatin-Microcrystalline Cellulose Adsorbate
[0084] To a solution of heterogeneous atorvastatin hemicalcium in ethanol (0.15 g/mL) are added 0.225 g/mL of microcrystalline cellulose (ratio of active pharmaceutical ingredient: adsorbate 2:3) and uniformly suspended. Then the solvent is dried up under permanent motion and vacuum (rotary evaporator or asymmetric moved dryer) at 25° C. Finally, the mixture is post-dried at 35° C. for a short time for removing residual solvent.
[0085] Active pharmaceutical ingredient amount of the adsorbate by means of HPLC: 40.3% (theoretically 40%)
Powder x-ray diffraction diagram: FIG. 4
[0087] Impurity profile (Sum of all the impurities, HPLC, in %):
Start 15 days (70° C./75% relative humidity) Sample (adsorbate) 0.83 1.04 Comparison (amorphous 1.07 1.92 atorvastatin calcium)
EXAMPLE 5
Atorvastatin-Mannitol Adsorbate
[0088] To a solution of heterogeneous atorvastatin hemicalcium in ethanol (0.15 g/mL) are added 0.15 g/mL of mannitol (1:1 mixture) and uniformly suspended. Then the solvent is dried up under permanent motion and vacuum (rotary evaporator or asymmetric moved dryer) at 25° C. Finally, the mixture is post-dried at 35° C. for a short time for removing residual solvent.
[0089] Active pharmaceutical ingredient amount of the adsorbate by means of HPLC: 50.4% (theoretically 50%)
Powder x-ray diffraction diagram: FIG. 5
[0091] Impurity profile (Sum of all the impurities, HPLC, in %):
Start 15 days (70° C./75% relative humidity) Sample (adsorbate) 0.72 1.05 comparison (amorphous 1.07 1.92 atorvastatin calcium)
EXAMPLE 6
Atorvastatin-Microcrystalline Cellulose Adsorbate
[0092] To a solution of heterogeneous atorvastatin hemicalcium in ethanol (0.15 g/mL) are added 0.30 g/mL of microcrystalline cellulose (ratio of active pharmaceutical ingredient:adsorbate 1:2) and uniformly suspended. Then the solvent is dried up under permanent motion and vacuum (rotary evaporator or asymmetric moved dryer) at 25° C. Finally, the mixture is post-dried at 35° C. for a short time for removing residual solvent.
[0093] Active pharmaceutical ingredient amount of the adsorbate by means of HPLC: 33.4% (theoretically 33.3%)
Powder x-ray diffraction diagram: FIG. 6
[0095] Impurity profile (Sum of all the impurities, HPLC, in %):
Start 15 days (70° C./75% relative humidity) Sample (adsorbate) 0.91 1.09 comparison (amorphous 1.07 1.92 atorvastatin calcium)
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The invention relates to a method for the preparation of atorvastatin adsorbates and solvates thereof, wherein one starts from a solution comprising the pharmaceutical active pharmaceutical ingredient substantially dissolved therein, one suspenses an adsorber material therein selected from the group of the celluloses, cellulose derivatives, polyols, sugars, sugar derivatives, maltodextrins, cyclodextrins, starches, polydextroses or mixtures thereof, and one removes the solvent by drying. Also, the invention relates to atorvastatin adsorbates obtainable according to this method as well as pharmaceutical formulations comprising them.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention is directed to a temporary aqueous aerosol paint composition and a method for preparing the inventive composition. In particular, the aqueous aerosol paint composition of the present invention may be utilized in temporary marking applications such as, for example, marking the location of underground utility lines, as is common in the construction industry.
[0003] 2. Description of the Related Art
[0004] Aerosol paints are utilized in a variety of applications, including those typically associated with standard (i.e. non-aerosol) oil or water based paints. This is a result of the numerous advantages of an aerosol delivery system. For example, the application of an aerosol paint often requires less skill than is typically required to properly apply a standard oil or water based paint. In addition, the use of an aerosol paint eliminates the need for cleaning paint brushes, paint rollers, paint trays, etc., as is required after the application of standard paints. Also, in certain instances, aerosol paint may be readily applied to surfaces which may be awkward and/or difficult to access, thereby hindering the application of standard paints.
[0005] Due to the numerous advantages of aerosol paints, their use has become widespread for both home and commercial applications. One particular area of widespread commercial usage of aerosol paints is in the construction industry, and in particular, the non-permanent identification of various structures and/or materials on or around a construction site, for example, site boundaries and/or locations specified by a surveyor, identification of the location of underground utility lines and/or other underground structures, identification of building materials, etc.
[0006] Historically, the aerosol paints utilized in the construction industry and, in fact, aerosol paints in general, comprise a mixture of volatile organic solvents, as well as, typically, an equally volatile aerosol propellant. While this combination of volatile compounds results in a stable and usable aerosol paint composition, the hazardous aspects of such volatile compounds are now all too well known. To begin, such compositions are typically flammable, due to the concentration of highly volatile compounds, and as such, these compositions are dangerous to store, transport, and handle, and the potential of a fire, or worse, an explosion, due to mishandling is a constant concern. In addition, it is also now well documented that exposure to such volatile organic compounds, even in limited amounts, presents a health hazard to the persons who are exposed to them. This exposure hazard exists for persons who are directly applying such volatile compositions as well as those who may simply be present in the general vicinity in which they are being applied. Aside from the potential fire, explosion, and health hazards presented by such volatile aerosol paint compositions, such compositions are also believed to be a factor in the further depletion of the ozone layer and thus, they are believed to contribute to the phenomenon now commonly known as “global warming,” which, if left uncontrolled, is believed to pose a potentially devastating threat to the very existence of our planet.
[0007] Attempts to address the negative aspects of such volatile aerosol paint compositions, as outlined above, have resulted in the development of formulations which reduce and/or eliminate the reliance on volatile compounds in aerosol paint compositions, with varying degrees of success. For instance, although a number of aerosol paint compositions have been formulated which no longer require a volatile organic solvent, many of these formulations still utilize a volatile organic propellent, thereby still presenting the hazards presented above, albeit to a somewhat lesser degree. In addition, these formulations are reportedly prone to foaming problems upon application, due to entrapment of the volatile organic propellent in the non-volatile paint component. Also, many of these formulations are known to be unstable even after only a short period of time.
[0008] Further attempts to improve aerosol paint formulations include the use of essentially non-volatile compounds in both the paint component and the propellant component, however, many of these formulations still reportedly exhibit excessive foaming so as to limit their widespread commercial usage. In addition, these later formulations still typically contain other harmful organic compounds and, as such, they continue to present a health hazard to persons who directly apply them or are otherwise exposed to them.
[0009] In addition, the currently known and purportedly “temporary” aerosol marking paints utilized in the construction industry today are formulated such that they typically remain visible from between several months to and more than a year after application, depending upon the type of surface or material on which they are applied, and the climatic conditions in the region of application. Aside from the obvious eyesore such lingering markings present, a more serious issue is the safety hazard created due to potential confusion in determining exactly what the various and often overlapping markings are supposed to indicate. As should be appreciated, the potential of a construction crew digging or drilling in an area where underground gas, electric, water, and/or sewer lines are not clearly identified presents a serious risk to the health and well being of the crew, as well as the persons in the immediate and surrounding areas.
[0010] As such, it would be beneficial to provide an aerosol paint composition which minimizes and/or eliminates the negative attributes identified above, yet is formulated for ease of handling and consistency of application. More in particular, such an aerosol paint composition would preferably comprise an aqueous paint component, including an aqueous solvent, as well as an aqueous propellant component. It would be further beneficial for such an aqueous aerosol paint composition to comprise compounds which minimize and/or eliminate the hazards presented to users and the environment relative to the various volatile and non-volatile organic compounds typically included in aerosol paint compositions, as discussed above. Preferably, any such aqueous aerosol paint composition would be formulated to provide a highly visible marking in a variety of flourescent colors such that various structures and/or materials on or around a construction site may be clearly marked so as to eliminate confusion. Yet another benefit would be for such an aqueous aerosol paint composition to naturally and essentially completely degrade within weeks rather than months of application. A further advantage would be achieved by providing a simple and cost effective method for preparing and packaging such a temporary aqueous aerosol paint composition to permit widespread usage within the construction industry and elsewhere.
SUMMARY OF THE INVENTION
[0011] The present invention is directed to a temporary and completely aqueous aerosol paint composition for use in any temporary marking application such as, by way of example only, marking the location of buried utility lines or other structures and/or materials, as is common in the construction industry. More in particular, the inventive composition of the present invention comprises an aqueous paint component and an aqueous propellant component.
[0012] To begin, the aqueous paint component of the present invention comprises an aqueous solvent. The aqueous solvent may comprise between generally about 50% to 90% by weight of the aqueous paint component. In one embodiment, the aqueous solvent comprises an amount of water. In one further embodiment, the aqueous solvent comprises an amount of filtered water which has been filtered specifically to remove chlorine and/or iron and/or ions thereof.
[0013] The aqueous paint component of the present invention also includes a polymeric resin, which may comprise between generally about 5% to 10% by weight of the aqueous paint component. In one embodiment, the polymeric resin comprises a polymeric compound dispersion and, in at least one further embodiment, the polymeric resin comprises a polyvinyl acetate dispersion.
[0014] Additionally, the composition of the present invention includes at least one pigment compound, and in at least one embodiment, a colored pigment compound. Another embodiment of the present invention comprises a flourescent colored pigment compound. At least one other embodiment comprises a plurality of colored pigment compounds, while yet another embodiment comprises a white pigment compound. The aqueous paint component of the present invention includes at least one pigment compound in an amount between generally about 5% to 25% by weight.
[0015] Also, the aqueous paint component comprises at least one filler compound. Similar to the pigment compounds, however, at least one embodiment of the aqueous paint component comprises a plurality of filler compounds. One embodiment of the present invention includes the at least one filler compound in an amount between generally about 1% to 10% by weight of the aqueous paint component.
[0016] The aqueous paint component of the present invention may also comprise a number of additional compounds including, but not limited to, an anti-foaming agent, a dispersant, a surfactant, a bactericide, and/or a light stabilizer. For example, at least one embodiment the aqueous paint component includes an anti-foaming agent which may comprise between generally about 0.10% to 0.50% by weight of the aqueous paint component. At least one other embodiment of the aqueous paint component includes a dispersant comprising between generally about 0.10% to 1.00% by weight, and yet one other embodiment may include a surfactant comprising an amount between generally about 0.05% to 1.00% by weight, while still another embodiment includes a bactericide which may comprise between generally about 0.01% to 0.10% by weight of the aqueous paint component.
[0017] In the embodiments of the present invention comprising at least one flourescent colored pigment compound, the aqueous paint component also preferably includes an amount of a light stabilizer. In one embodiment, the present invention includes a light stabilizer comprising generally about 0.6% by weight of the aqueous paint component.
[0018] The present invention also comprises a method for preparing an temporary aqueous aerosol paint composition, in accordance with the composition presented above. The method of the present invention comprises charging a reaction vessel with an initial amount of an aqueous solvent which, as indicated above, comprises water in at least one embodiment. The method of the present invention also includes setting a primary mixing cycle for the contents of the reaction vessel. More in particular, setting the primary mixing cycle includes adjusting the mixing speed to a predetermined primary mixing speed, which may be expressed in revolutions per minute (rpm) of the mixing blade, and maintaining this predetermined primary mixing speed for a predetermined primary mixing time.
[0019] Additionally, the method of the present invention comprises adding at least one pigment compound to the reaction vessel, however, at least one embodiment includes adding a plurality of pigment compounds to the reaction vessel. The method also includes adding an additional amount of the aqueous solvent to the reaction vessel, and setting a high velocity mixing cycle for the contents of the reaction vessel (i.e. adjusting and maintaining the mixing speed at a predetermined high velocity mixing speed for a predetermined high velocity mixing time).
[0020] The method of the present invention also includes adding at least one filler compound to the reaction vessel. In at least one embodiment, the method of the present invention comprises adding a plurality of filler compounds to the reaction vessel. The method also includes setting a first low velocity mixing cycle for the contents of the reaction vessel, which is set in a similar manner to that described above with respect to the primary and high velocity mixing cycles.
[0021] One preferred embodiment of the method of the present invention further comprises adding a polymeric resin to the reaction vessel, and setting a second low velocity mixing cycle for the contents of the reaction vessel, once again, in a similar manner to that described above with respect to the primary and high velocity mixing cycles. In addition, the method of the present invention includes adding a final amount of the aqueous solvent to the reaction vessel.
[0022] It is understood to be within the scope of the method of the present invention to comprise adding one or more additional compounds to the reaction vessel including, by way of example only, an anti-foaming agent, a dispersant, a surfactant, a bactericide and/or a light stabilizer.
[0023] These and other objects, features and advantages of the present invention will become more clear as the detailed description are taken into consideration.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0024] While this invention is susceptible of embodiment in many different forms, there is described in detail herein at least one specific embodiment, with the understanding that the present disclosure is to be considered as an exemplification of the principles of the invention and is not intended to limit the invention to this one specific embodiment.
[0025] As previously indicated, the present invention is directed to a temporary aqueous aerosol paint composition and a method for preparing the inventive composition more in particular, the present invention is directed to an aqueous aerosol paint composition which may be utilized for temporary marking of a variety of items. At least one embodiment of the composition of the present invention may be utilized to temporarily, yet positively, identify a variety of structures and/or materials on or around a construction site including, by way of example only, site boundaries and/or locations specified by a surveyor, locations of underground utility lines and/or other underground structures, various building materials, etc.
[0026] The temporary aqueous aerosol paint composition of the present invention comprises an aqueous paint component as well as an aqueous propellant component. The temporary aqueous paint component may comprise between generally about 60% to 80% by weight of the inventive composition, while the aqueous propellant component comprises between generally about 20% to 40% by weight of the aqueous aerosol paint composition.
[0027] The aqueous aerosol paint component of the present invention comprises an aqueous solvent, the aqueous solvent comprising between generally about 50% to 90% by weight of the aqueous paint component. In one preferred embodiment, the aqueous solvent comprises between generally about 70% to 80% by weight of the aqueous paint component, while in one other preferred embodiment, the aqueous solvent comprises between generally about 60% to 65% by weight.
[0028] In at least one embodiment of the present invention the aqueous solvent may comprise an amount of water, however, it is understood that other aqueous solvents may be utilized and that compositions comprising such other aqueous solvents are also included within the scope and intent of the present invention. In one preferred embodiment, the aqueous solvent of the present invention comprises an amount of filtered water and, more specifically, an amount of filtered water which has been filtered to remove chlorine and/or iron and/or ions thereof.
[0029] In addition to the aqueous solvent, the aqueous aerosol paint component of the present invention comprises a polymeric resin. Such polymeric resins are typically provided as a carrier for one or more paint pigment compounds and, more importantly, as a film forming agent which acts as an adhesive interface between the pigment compounds and a surface on which the paint composition is applied. In the present inventive composition, the polymeric resin may comprise a polymeric compound dispersion and, in particular, an aqueous polymeric compound dispersion. In one preferred embodiment, the polymeric compound dispersion comprises a short chain polymer, such as polyvinyl acetate, so as to facilitate the inhibition of unwanted interaction between the polymeric resin with the other compounds of the aqueous aerosol paint component of the present invention. More in particular, the polyvinyl acetate dispersion of one preferred embodiment of the present invention comprises an aqueous dispersion of a short chain homopolymer of vinyl acetate without a plasticizer, such as Mowilith D-50, a polyvinyl acetate dispersion manufactured by Clariant Mexico, S.A. de C.V.
[0030] The aqueous paint component of the inventive composition of the present invention comprises the polymeric resin in an amount of between generally about 5% to 10% by weight of the aqueous paint component and, in one preferred embodiment of the present invention, the aqueous paint component comprises generally about 6% by weight of a polyvinyl acetate dispersion.
[0031] Also as indicated above, the aqueous paint component of the present invention further comprises at least one pigment compound. The at least one pigment compound is structured to at least partially define a color of the temporary aerosol paint composition, and more in particular, a color of the composition after applying to a surface and curing. In one preferred embodiment, the at least one paint pigment compound is structured to at least partially define a flourescent color, while in at least one other preferred embodiment, the at least one pigment compound is structured to at least partially define a white color. A further preferred embodiment of the present invention comprises an aqueous paint component having a plurality of pigment compounds to at least partially define a color of the temporary aerosol paint composition.
[0032] One preferred embodiment of the present invention comprises a benzoguanamine/formaldehyde condensate with organic dyes, such as one of the Fiesta Daylight Flourescent Colours, manufactured by Swada (Limited) London, as the at least one pigment compound. These pigment compounds may be utilized to at least partially define such flourescent colors as pink, red, orange, green, blue, and yellow, just to name a few. At least one embodiment of the present invention comprises one of the flourescent pigments comprising a formaldehyde-melamine-p-toluenesulfonamide copolymer, such as is manufactured by the Sinloihi Co. Ltd. of Japan.
[0033] Alternatively, the aqueous paint component of the present invention may comprise at least one white pigment compound comprising titanium dioxide such as, by way of example only, Tronox CR-828, as manufactured by the Kerr-McGee Chemical Corporation.
[0034] The at least one pigment compound of the aqueous component of the present invention comprises between generally about %5 to 25% by weight. Tables I through VII below contain exemplary formulations of the inventive composition of the present invention for a number of color variations, including generally the amount of specific pigment compounds in each.
[0035] The aqueous paint component of the present invention further comprises at least one filler compound, however, one preferred embodiment comprises a plurality of filler compounds. In one embodiment, the at least one filler compound of the aqueous paint component comprises an aluminum silicate compound. Aluminum silicate compounds including, but not limited to, kaolin or kaolinite have been included in paint compositions to enhance viscosity, i.e. to increase the viscosity of the paint composition, so as to limit running upon application to a surface. In at least one other embodiment, the at least one filler compound comprises a calcium carbonate compound. Such calcium carbonate compounds have been utilized in paint formulations to limit adsorption by porous surfaces such as may be encountered, for example, when marking the location of underground utility lines and/or other underground structures on overlying concrete, asphalt, gravel, grass, and/or dirt. As indicated above, however, one preferred embodiment of the present invention comprises a plurality of filler compounds such as, for example, an aluminum silicate compound and a calcium carbonate compound.
[0036] At least one embodiment of the aqueous paint component of the present invention comprises the at least one filler compound in an amount of between generally about 1% to 10% by weight. In one preferred embodiment, the aqueous paint component of the present invention comprises a plurality of filler compounds each in an amount of between generally about 1% to 10% by weight. More in particular, one preferred embodiment of the aqueous paint component comprises an aluminum silicate compound in an amount of generally about 1.7% by weight and a calcium carbonate compound in an amount of generally about 2.1% by weight. One other preferred embodiment of the aqueous paint component of the present invention comprises an aluminum silicate compound in an amount of generally about 5.1% by weight and a calcium carbonate compound in an amount of generally about 6.4% by weight. Once again, Tables I through VII below contain exemplary formulations of the inventive composition of the present invention for a number of color variations, including generally the amount of specific filler compounds in each.
[0037] One further embodiment of the aqueous paint component of the present invention comprises a dispersant. In particular, the aqueous paint component may comprise a dispersant structured to balance the ionic forces between the various compounds comprising the aqueous paint component, so as to enhance the stability of these compounds in an aqueous medium. The aqueous paint component of the present invention comprises the dispersant in an amount of between generally about 0.10% to 1.00% by weight. More specifically, one preferred embodiment of the aqueous paint component comprises the dispersant in an amount of generally about 0.5% by weight, while one other preferred embodiment comprises generally about 0.25% by weight. In one preferred embodiment, the dispersant comprises a non-ionic surfactant such as, by way of example only, Crisanol NF-100, manufactured by Christianson S.A. de C.V., or a mixture of Brimopol S 904 and Brimopol S 9010, each manufactured by Polaquimia, S.A. de C.V.
[0038] The aqueous paint component of the present invention may also comprise an anti-foaming agent. In particular, at least one embodiment of the aqueous paint component of the present invention comprises between generally about 0.10% and 0.50% by weight of the anti-foaming agent. The anti-foaming agent is included in the aqueous paint component to facilitate the release of the minimal amount of volatile compounds present in the aqueous paint component during application and cure, so as to minimize irregularities in the surface of the cured paint film due to the release of such volatile compounds. One preferred embodiment comprises between generally about 0.20% and 0.25% by weight of the anti-foaming agent in the aqueous paint component. In at least one embodiment, the anti-foaming agent comprises an emulsion such as, by way of example only, Antifoam H-10 Emulsion, manufactured by Dow Corning Corporation, although it is understood that anti-foaming agents exhibiting similar properties may be utilized.
[0039] In yet another embodiment of the temporary aqueous aerosol paint composition of the present invention, the aqueous paint component also comprises a surfactant. Similar to the dispersant described above, the surfactant may be included to enhance the stability of the aqueous paint component by “balancing” the various interactive forces between the different compounds. At least one embodiment of the present invention utilizes an alcohol based compound as the surfactant, such as, by way of example only, the ester alcohol compound Texanol as manufactured by the Eastman Chemical Company. The aqueous paint component of the inventive composition of the present invention may comprise the surfactant between generally about 0.1% to 1.0% by weight. More specifically, one preferred embodiment of the aqueous paint component of the present invention comprises generally about 0.85% by weight of the surfactant, while one other preferred embodiment comprises generally about 0.10% by weight of the surfactant.
[0040] The aqueous paint component of the present invention may also comprise a bactericide, to minimize spoilage of the aqueous paint component by the various bacterium to which it may be exposed. The aqueous paint component preferably comprises an aqueous based broad spectrum bactericide, and in one preferred embodiment, the bactericide comprises 1,3-dihydroxymethyl-5,5-dimethylhydantoin and 1-hydroxymethyl-5,5-dimethylhydantoin, such as, for example, Troysan 395, manufactured by Troy Chemical Company. A preferred embodiment of the aqueous paint component comprises the bactericide in an amount of generally about 0.03% by weight.
[0041] A further embodiment of the aqueous paint component of the present invention may comprise a light stabilizer. More in particular, the aqueous paint component comprises a light stabilizer in formulations also comprising one or more colored pigment compounds, to prevent premature degradation of the paint composition following application and cure. The type and amount of light stabilizer which the aqueous paint component comprises is important to achieve the desired “temporary” aspect of the inventive composition of the present invention. Specifically, utilization of the incorrect type and/or amount of the light stabilizer will result in a paint composition which either degrades too quickly or too slowly, following application and cure, via exposure to the ultra-violet rays of the sun.
[0042] The light stabilizer utilized in the present invention may comprise, in one preferred embodiment, a combination of polymeric benzotriazole compounds such as, by way of example only, Tinuvin 5151, manufactured by Ciba Specialty Chemicals Corporation U.S.A. Further, the aqueous paint component of the inventive composition of the present invention may comprise the light stabilizer in an amount of generally about 0.6% by weight, in one preferred embodiment. As illustrated below in the exemplary formulations of Tables I through VII, the light stabilizer is only included in the formulations comprises one or more colored pigment compounds.
[0043] In addition to the aqueous paint component, the temporary aqueous aerosol paint composition of the present invention also comprises an aqueous propellant component. The aqueous propellant component may comprise between generally about 10% to 40% by weight of the temporary aqueous aerosol paint composition. One preferred embodiment of the aqueous propellant component comprises an aqueous dimethyl ether compound and, in this preferred embodiment, the aqueous propellent component comprises generally about 25% by weight of the temporary aqueous aerosol paint composition. In at least one embodiment, the aqueous propellant component of the present invention comprises the aqueous dimethyl ether compound Dymel, manufactured by DuPont Fluoroproducts.
[0044] The following tables, Tables I through VII, provide exemplary formulations of one preferred embodiment of the aqueous paint component of the composition of the present invention for several possible color variations. These exemplary formulations list generally the amount of each specific compound in each embodiment. The weight percentages indicated in the following tables are for illustrative purposes only, and are not intended to imply exact values for purposes of limiting the scope of the present invention, rather they are presented to illustrate the combinations and amounts of the aforementioned compounds which various embodiments of the aqueous paint component of the present invention may comprise.
TABLE I FLOURESCENT PINK AQUEOUS PAINT COMPONENT Compound Weight Percent water 72% polyvinyl acetate dispersion 6% flourescent pink pigment compound 15% aluminum silicate compound 2% calcium carbonate compound 2% dispersant 0.5% anti-foaming agent 0.25% surfactant 0.8% bactericide 0.03% light stabilizer 0.6%
[0045]
TABLE II
FLOURESCENT RED AQUEOUS PAINT COMPONENT
Compound
Weight Percent
water
72%
polyvinyl acetate dispersion
6%
flourescent red pigment compound
10%
organic red pigment compound
5%
aluminum silicate compound
2%
calcium carbonate compound
2%
dispersant
0.5%
anti-foaming agent
0.25%
surfactant
0.8%
bactericide
0.03%
light stabilizer
0.6%
[0046]
TABLE III
FLOURESCENT ORANGE AQUEOUS PAINT COMPONENT
Compound
Weight Percent
water
73%
polyvinyl acetate dispersion
6%
flourescent orange pigment compound
14%
aluminum silicate compound
2%
calcium carbonate compound
2%
dispersant
0.5%
anti-foaming agent
0.25%
surfactant
0.8%
bactericide
0.03%
light stabilizer
0.6%
[0047]
TABLE IV
FLOURESCENT GREEN AQUEOUS PAINT COMPONENT
Compound
Weight Percent
water
71%
polyvinyl acetate dispersion
6%
flourescent green pigment compound
16%
aluminum silicate compound
2%
calcium carbonate compound
2%
dispersant
0.5%
anti-foaming agent
0.25%
surfactant
0.8%
bactericide
0.03%
light stabilizer
0.6%
[0048]
TABLE V
FLOURESCENT BLUE AQUEOUS PAINT COMPONENT
Compound
Weight Percent
water
78%
polyvinyl acetate dispersion
6%
flourescent blue pigment compound
9%
aluminum silicate compound
2%
calcium carbonate compound
2%
dispersant
0.5%
anti-foaming agent
0.25%
surfactant
0.8%
bactericide
0.03%
light stabilizer
0.6%
[0049]
TABLE VI
FLOURESCENT YELLOW AQUEOUS PAINT COMPONENT
Compound
Weight Percent
water
70%
polyvinyl acetate dispersion
6%
flourescent yellow pigment compound
17%
aluminum silicate compound
2%
calcium carbonate compound
2%
dispersant
0.5%
anti-foaming agent
0.25%
surfactant
0.8%
bactericide
0.03%
light stabilizer
0.6%
[0050]
TABLE VII
WHITE AQUEOUS PAINT COMPONENT
Compound
Weight Percent
water
63%
polyvinyl acetate dispersion
6%
white pigment compound
18%
aluminum silicate compound
5%
calcium carbonate compound
6%
dispersant
0.25%
anti-foaming agent
0.23%
surfactant
0.1%
bactericide
0.03%
[0051] The present invention also comprises a method for preparing a temporary aqueous aerosol paint composition, such as the composition described above. More in particular, the present invention encompasses a method for preparing an aqueous paint component of a temporary aqueous aerosol paint composition, as described above.
[0052] The method of the present invention comprises charging a reaction vessel with an initial amount of an aqueous solvent. The reaction vessel may comprise any number of configurations with respect to volume and geometry, provided that the reaction vessel includes means for thoroughly mixing the contents of the reaction vessel, i.e. the compounds comprising the aqueous paint component, at each predetermined mixing speed indicated below. In addition, the reaction vessel includes means for controlling the temperature of the contents of the reaction vessel as required, also as indicated below. As will be appreciated, the actual quantity of the temporary aqueous aerosol paint composition which may be prepared utilizing the present inventive method may be easily adjusted by modifying the amounts of the various compounds relative to the final amount desired, and providing a reaction vessel suited to thorough mixing and temperature control of this actual quantity.
[0053] In the method of the present invention, the aqueous solvent may comprise an amount of water, and in one preferred embodiment, an amount of filtered water. As described above, the amount of filtered water may be filtered to remove chlorine, and/or iron and/or ions thereof. Charging the reaction vessel with the initial amount of aqueous solvent comprises adding an amount of aqueous solvent to the reaction vessel which is generally about 20% by weight of a total amount of aqueous solvent to be added.
[0054] The method of the present invention further comprises setting a primary mixing cycle for the contents of the reaction vessel. Specifically, setting the primary mixing cycle comprises adjusting a mixing speed for the contents of the reaction vessel to approximately 1,800 revolutions per minute (rpm), and maintaining the mixing speed at approximately 1,800 rpm for generally about 10 to 15 minutes.
[0055] Additionally, the method of the present invention also comprises adding at least one pigment compound to the reaction vessel. The at least one pigment compound may comprise, for example, any of the pigment compounds described above, and in an amount of between generally about 5% to 25% by weight of the aqueous paint component. One embodiment of the present method comprises adding the at least one pigment compound to the reaction vessel during the primary mixing cycle, preferably, just after setting the primary mixing cycle. In addition, the at least one pigment compound is preferably added slowly, thereby allowing the at least one pigment compound to mix thoroughly with the aqueous solvent. At least one embodiment of the present method further comprises adding a plurality of pigment compounds to the reaction vessel, the plurality of pigment compounds being of the type and generally in the amounts indicated above for pigment compounds.
[0056] The method of the present invention also comprises adding an additional amount of the aqueous solvent to the reaction vessel. In one preferred embodiment, the method comprises adding an additional amount of the aqueous solvent wherein the additional amount is generally about 10% by weight of the total amount of aqueous solvent to be added.
[0057] In addition, the method for preparing an aqueous paint component of a temporary aqueous aerosol paint composition further comprises adding a dispersant to the reaction vessel. In one preferred embodiment, the dispersant comprises a non-ionic surfactant as described above, and in an amount of between generally about 0.10% to 1.00% by weight of the aqueous paint component in the reaction vessel.
[0058] The method of the present invention further comprises setting a high velocity mixing cycle for the contents of the reaction vessel. More in particular, setting the high velocity mixing cycle comprises adjusting a mixing speed for the contents of the reaction vessel to approximately 2,300 rpm, and maintaining the mixing speed at approximately 2,300 rpm for generally about 60 minutes. In addition, the method comprises controlling a temperature of the contents of the reaction vessel at approximately, but not exceeding, thirty degrees Celsius (30° C.), during at least the high velocity mixing cycle.
[0059] One embodiment of the present method comprises adding at least one filler compound to the reaction vessel. The at least one filler compound may be added in accordance with the amount previously described, being between generally about 1% to 10% by weight of the aqueous paint component. Further, adding the at least one filler compound to the reaction vessel may comprise adding one of the filler compounds disclosed above, specifically, an aluminum silicate compound or a calcium carbonate compound.
[0060] In one preferred embodiment, the method of the present invention comprises adding a plurality of filler compounds to the reaction vessel, each comprising between generally about 1% to 10% by weight of the aqueous paint component. Specifically, one preferred embodiment of the present method comprises adding an aluminum silicate compound and a calcium carbonate compound, each in an amount of generally about 2% by weight of the aqueous paint component. In one other preferred embodiment, the present method comprises adding an aluminum silicate compound in an amount of generally about 5% by weight of the aqueous paint component and a calcium carbonate compound in an amount of generally about 6% by weight.
[0061] The method of the present invention further comprises setting a first low velocity mixing cycle for the contents of the reaction vessel. More in particular, setting the first low velocity mixing cycle comprises adjusting a mixing speed for the contents of the reaction vessel to approximately 800 rpm, and maintaining the mixing speed at approximately 800 rpm for generally about 5 to 10 minutes. In one preferred embodiment, the present method further comprises adding an anti-foaming agent to the reaction vessel in an amount of between generally about 0.10% and 0.50% by weight of the aqueous paint component. One further preferred embodiment comprises adding an amount of a surfactant to the reaction vessel in an amount of between generally about 0.05% to 1.00% by weight of the aqueous paint component. In at least one embodiment of the present method, the anti-foaming agent may comprise an emulsion, and the surfactant may comprise an alcohol based compound, as disclosed above. Preferably, the anti-foaming agent and the surfactant are added to the reaction vessel as the mixing speed is being reduced from the high velocity mixing speed to the first low velocity mixing speed.
[0062] At least one embodiment of the present method for preparing an aqueous paint component of a temporary aqueous aerosol paint composition comprises adding a bactericide to the reaction vessel. In at least one embodiment, the bactericide comprises an aqueous based broad spectrum bactericide as described above, in an amount of between generally about 0.10% to 1.00% by weight of the aqueous paint component in the reaction vessel. In one preferred embodiment, adding the bactericide comprises adding the bactericide in an amount of generally about 0.03% by weight of the aqueous paint component.
[0063] The method of the present invention may also comprise adding an amount of a light stabilizer to the reaction vessel. The light stabilizer may comprise a polymeric benzotriazole, as indicated above. One preferred embodiment of the method of the present invention comprises adding the light stabilizer in an amount of generally about 0.6% by weight of the aqueous paint component.
[0064] The present method for preparing an aqueous paint component of a temporary aqueous aerosol paint composition further comprises adding a polymeric resin to the reaction vessel, the polymeric resin comprising between generally about 5% to 10% by weight of the aqueous paint component. One preferred embodiment of the present invention comprises adding the polymeric resin to the reaction vessel in an amount of generally about 6% by weight of the aqueous paint component. In addition, in a preferred embodiment, the polymeric resin comprises an aqueous polymeric compound dispersion and, more specifically, a polyvinyl acetate dispersion, as previously disclosed.
[0065] The method of the present invention further comprises setting a second low velocity mixing cycle for the contents of the reaction vessel. More in particular, setting the first low velocity mixing cycle comprises adjusting a mixing speed for the contents of the reaction vessel to approximately 600 rpm, and maintaining the mixing speed at approximately 600 rpm for generally about 10 to 15 minutes.
[0066] Additionally, the method of the present invention comprises adding a final amount of aqueous solvent to the reaction vessel, the final amount of aqueous solvent comprising generally about 70% by weight of the total amount of aqueous solvent added to the reaction vessel.
[0067] The present invention further comprises a method for charging an aerosol can with a temporary aqueous paint composition, such as disclosed above, thereby permitting a ready means for applying the inventive composition as required. One preferred embodiment comprises charging an aerosol can specifically designed for inverted application of the aqueous aerosol paint composition of the present invention.
[0068] Specifically, the method comprises charging the aerosol can with an amount of an aqueous paint component, such as may be prepared via the method disclosed herein. In one preferred embodiment, the method comprises charging the aerosol can with an amount of the aqueous paint component comprising generally about 75% by weight of the aqueous aerosol paint composition. The method may further comprise installing a valve on the can to permit controlled application of the contents therefrom. Also, the present method comprises charging the aerosol can with an amount of an aqueous propellant. In a preferred embodiment, the method includes charging the aerosol can with an aqueous dimethyl ether compound in an amount of generally about 25% by weight of the aqueous paint composition, such as the inventive temporary aqueous aerosol paint composition disclosed herein.
[0069] Since many modifications, variations and changes in detail can be made to the described preferred embodiment of the invention, it is intended that all matters in the foregoing description be interpreted as illustrative and not in a limiting sense. Thus, the scope of the invention should be determined by the appended claims and their legal equivalents.
[0070] Now that the invention has been described,
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A temporary aqueous aerosol paint composition comprising an aqueous paint component, including an aqueous solvent, and an aqueous propellant component. At least one embodiment of the temporary aerosol paint composition includes an amount of water, and more particularly, an amount of filtered water, as the aqueous solvent. In addition, the temporary aerosol paint composition may include an amount of an aqueous dimethyl ether compound as the aqueous propellant component. The temporary aerosol paint composition is formulated to minimize and/or eliminate the hazards presented by the various volatile and non-volatile organic compounds present in known aerosol paint compositions, by eliminating or minimizing the inclusion of such organic compounds. Any one of a number of pigment compounds may be utilized in the temporary aqueous aerosol paint composition, including flourescent colored pigment compounds, thereby permitting use in a variety of applications. A simplified method for preparing a temporary aqueous aerosol paint composition includes adding the various compounds to a reaction vessel in which a plurality of mixing cycles are accomplished.
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RELATED APPLICATIONS
This case is a continuation-in-part of U.S. application Ser. No. 918,785, filed on June 26, 1978, now abandoned, which in turn was a continuation of U.S. Application Ser. No. 704,998, filed July 14, 1976 and now abandoned.
BACKGROUND OF THE INVENTION
The present invention relates to postal meters and more particularly to an electronic postal meter having an improved, noise-rejection input/output channel.
Electronic postal meters have been developed utilizing microprocessors as a part of the meter control unit. Data and instructions may be entered into the control unit for such meters through keyboard devices. The results of calculations, requests for more information and error messages may be presented to an operator on an output printer or on a CRT display unit. Units such as the keyboard, the printer and the CRT display, generally described as input/output devices may be located at some distance from the meter control unit and the meter mechanism controlled by that unit, requiring some form of communications channel between the input/output devices and the meter control unit. Heretofore, the communications channel consisted of direct electrical connections in the form of electrical cables or leads between the computer control and the input/output devices.
Postal meters are generally located in the vicinity of other electrical machines which, during operation, may produce extraneous electric fields. Such extraneous electric fields may induce noise voltages in nearby electrical apparatus and particularly in cables or leads. Where the apparatus operates with low signal voltages, as is the case for a microprocessor, induced noise voltages may cause the apparatus to misinterpret and erroneously act upon incoming information.
Moreover, postal meters are most likely to be found in business offices. Since many business offices are carpeted, users of postal meters may build up a static electric charge simply in walking to the meter. When the user touches the keyboard or other input unit, the static electrical discharge may temporarily cause a controlling microprocessor to malfunction or to misinterpret incoming data.
Shielded cables have been used to shield electrical connectors from extraneous electric fields. However, such shielded cables do not solve another problem; i.e., the effect of an electrical malfunction or voltage surge generated in an input/output device such as a keyboard. When a malfunction occurs or a voltage surge takes place in such a device, the voltage may be transmitted directly to the microprocessor control. Voltage surges may disrupt microprocessor operation or even destroy microprocessor circuitry.
Moreover, it is possible for a remote postal meter to be disconnected from one input/output device and reconnected to another. Where the meter and the control unit are directly connected, a faulty reconnection may cause damaging voltages to be applied to the meter.
SUMMARY OF THE INVENTION
The present invention is an improved, noise voltage-rejecting input/output channel which also isolates a postal meter control from surge voltages occurring at remotely-located input/output devices while providing improved security.
The invention is employed in a postal meter having a postage printer. The postal meter also includes a control means for generating the printer-setting signals and input/output means for providing information in the form of electrical signals to and for receiving information in the same form from the control means. The control means and the input/output means are linked by an improved input/output channel which includes means for converting electrical signals provided by one of the linked means to optical signals. The channel also includes means for transmitting the optical signals and means for converting the transmitted optical signals to an electrical format usuable by the other of the linked means.
In accordance with a further preferred embodiment of the invention, optical electric transducing means are provided with the secure housing of the postal meter at a location that is substantially inaccessible from the exterior of the secure housing, even by way of the port or the like in the housing through which the communication path to peripheral equipment extends. The optical-electric transducing means may be in the form of optical-electric coupling devices of conventional form, if the communication path to the peripheral equipment is by way of electric conductors, or it may be in the form of photo-electric devices positioned to receive radiation from optical fibers, if the optical fibers are employed as a communication path. Independently of the form of the communication path, however, the interior of the secure housing is configured to render it as difficult as possible to apply potentials, either intentionally or accidentally, to the electric circuit portions of the transition means. As a consequence, the accidental or intentional application of voltages which may cause damage to the electronic circuits within the housing, is inhibited, independently of the type of communication path employed, whereby voltages cannot be externally applied to the accompanying circuits or registers of the postal meter so as to damage the equipment or wipe out the data stored therein. The inaccessibility of the transducing means may be due to, for example, the placement of the transducing means as deep as possible within the secure housing, the providing of a circuitous route for the portion of the communication path within the secure housing, or the provision of a connector assembly at the port of the housing through which the communication path extends that inhibits the directing of conductors into the housing that could carry potentials detrimental to the electronic system.
DESCRIPTION OF THE DRAWINGS
While the specification concludes with claims particularly pointing out and distinctly claiming that which is regarded as the present invention, details of a preferred embodiment of the invention may be more readily ascertained from the following detailed description when read in conjunction with the accompanying drawings wherein:
FIG. 1 is a general block diagram of a system which may include the invention;
FIG. 2 is a more detailed block diagram of the system;
FIG. 3 is a detailed block diagram of the control means for the postal meter;
FIG. 4 is a perspective of the postal printing mechanism driven by the control means;
FIG. 5 is a detailed schematic diagram of the interface between the control means and the postal printing mechanism;
FIG. 6 is a schematic diagram of a preferred embodiment of the improved noise-rejecting input/output channel;
FIG. 7 is a simplified schematic illustration of a postal meter in accordance with a further embodiment of the invention;
FIG. 8 is a simplified cross sectional view of a modification of the postal meter of FIG. 7; and
FIG. 9 is an enlarged cross sectional view of a further modification of the arrangement of FIG. 7.
DETAILED DESCRIPTION
Referring now to FIG. 1, a postal meter 10 is linked to an input/output unit 12 through an input/output channel 14. Postal meter 10 is an electronic device in which the contents of the ascending and descending registers, among others, are stored electronically. Postal meter 10 accepts data and instructions sent to it through the input/output channel 14 from the input/output unit 12. In turn, postal meter 10 provides signals to the input/output unit 12 through channel 14 representing the results of calculations, requests for further instructions and error messages.
Input/output unit 12 may include a keyboard for entering data and instructions into the system and a printer or CRT display for presenting the results of calculations, instruction requests and error messages to an operator. While unit 12 is represented as a single device, the input and output sections of unit 12 obviously could be physically-independent units. Input/output channel 14, which will be described in more detail later, is highly immune to noise voltages generated outside the system and also acts to prevent the transmission of voltage surges from one of the units to the other.
Referring now to FIG. 2, the entire system is shown in block diagram form. A central processor unit 16 communicates with random access memory 18, output ports 19 and with a memory interface unit 20 which generally controls the flow of data and instruction between central processor unit 16, read-only memory 22 and a special-purpose, non-volatile random access memory 24. In a preferred embodiment of the invention, the components may be commercially-available solid-state chips. Central processor unit 16, random access memory 18 and read-only memory 22 may be one or more 4040, 4002 and 4001 chips, respectively, in a MSC-4 Micro Computer Set available from Intel Corporation of Santa Clara, California.
Output signals from the central processor unit 16 are transmitted through output ports 19, to meter setting elements 26, to an input multiplexer 28 and to the input/output channel 14.
Inputs to the control for postal meter 10 include both internal and external inputs. The external inputs are provided by input/output unit 12 through input/output channel 14 to a buffer system 34. Internal inputs representing the status of components of a meter setting mechanism are provided by a meter setting detector array 30 under the control of multiplexer 28. Multiplexer 28 is preferably in Intel 4003 chip. Selected outputs from detector 30 are applied to buffer system 34. Additional internal inputs are provided by an interrupt generator circuit 32 which applies an interrupt signal to the central processor unit 16. The outputs of interrupt generator circuit 32 are applied to buffer system 34. Outputs from buffer system 34 are applied to the memory interface unit 20.
The central processor unit 16 performs calculations using data provided through the input buffer system 34 and instructions stored in read-only memory 22. Read-only memory 22 serves as a program store for the routines and subroutines employed within the meter 10. Random access memory 18 provides a working memory for the central processor unit 16. Non-volatile random access memory 24 is a special purpose memory for operating on and storing the contents of certain critical registers within the postal meter 10. These registers include the ascending register which contains the accumulated total of all postage processed through the meter 10 and the descending register which stores the amount of funds remaining to be used in the meter 10. Non-volatile memory 24 is powered with a battery back-up unit to permit the contents of memory 24 to be saved in the event of a loss of power in the meter 10. The memory interface chip 20 which controls input/output from non-volatile random access memory 24 may be a 4289 chip available from Intel Corporation while memory 24 may be conventional RAM chip such as a MC 14552 (Motorola).
Further details as to the organization of the postal meter 10 appear in the description relating to FIG. 3. The operations of central processor unit 16 are timed by a clock circuit 36 which supplies two trains of non-overlapping clock pulses 01 and 02 and a reset signal. These signals are applied to the central processor unit 16, to memory interface unit 20 and to a number of random access memory units 38, 40, 42.
Outputs from an output port 37 associated with random access memory unit 38 are applied to a pair of coil select circuits 44, 46 which are used in setting the one type of postal printing device. The coil select circuits 44 and 46 are connected to a motor select circuit 48 which, under the control of outputs from an output port 39 associated with random access memory unit 40, determines which of the two motors will be energized. Details of the coil select circuits 44 and 46 and the motor select circuit 48 are provided in a following section of this specification. Another output from output port 39 controls a test switch 50, which is part of the interrupt generator circuit 32.
The interrupt generator circuit 32 includes a power sense circuit 52, a meter locked detector 54 and a print detector 56. The power sense circuit 52 monitors the output of the power supply for the postal meter and generates an interrupt signal whenever the onset of a power failure is detected. This interrupt signal triggers a computer routine in which the contents of the ascending and descending registers are updated in the non-volatile random access memory 24 before the meter shuts down.
The print detector circuit 56 includes photoelectric devices for sensing the completion of a mechanical printng operation by the meter. This information is used for resetting the computer to enable calculation of new postal values. The meter locked detector 54 includes photoelectric devices which sense whether the meter, itself a relatively small unit, remains attached to its original, relatively large base. If the meter is removed from the base for any reason, an output from meter locked detector 54 causes an interrupt signal to be generated. This interrupt signal is employed to disable the meter. The outputs of power sense circuit 52, meter locked detector circuit 54 and print detector circuit 56 are applied both to a NAND circuit 58 and to a logic buffer 60.
In a preferred embodiment, postal meter 10 employs negative logic; that is, a binary "1" is represented by a negative voltage such as -15 volts whereas a binary "0" is represented by a more positive voltage such as ground or zero volts. When any of the outputs of the circuits 52, 54, 56 goes to a binary 1 level, the output of NOR circuit 58 switches to produce an interrupt pulse at an input to the central processor unit 16. Since the response of the central processor unit 16 will be different for different ones of the interrupt signals, the interrupt signals must be applied as an internal input in the system through the logic buffer 60. Interrupt signals appearing on the output of buffer 60 are applied to memory interface unit 20 which, in response to a command from the central processor unit 16, transfers the interrupt signal to the processor for decoding.
The memory interface unit 20 provides outputs to a first decoder circuit 62 and a second decoder circuit 64. One input to the second decoder circuit 64 is provided by the first decoder circuit 62. The decoder circuit 62 and 64 are used in selecting whether non-volatile random access memory 24, one of several read-only memory units 66, 68, 70, 72 or one of a number of input logic buffers 60, 74, 76 is to be enabled.
A single input to buffer 76 is provided from the input/output channel 14. Outputs to the input/output channel 14 are provided by output port 39 associated with random access memory 40. Logic buffer 74 receives signals from meter setting detector array 30. There are more detectors in the detector array 30 than logic buffer 74 can accommodate at one time. A shift register input multiplexer 28 operating under the control of signals provided through the output port 41 associated with random access memory 42 multiplexes the inputs from detector array 30 to logic buffer 74. Multiplexer 28 may be a 4003 device available from Intel Corporation.
The postal meter described above represents one embodiment of a meter for controlling a postal printing mechanism now to be described with reference to FIG. 4. In a preferred embodiment, the mechanism is used to set print wheels contained within a print drum 78 of a modified Model 5300 postage meter manufactured by Pitney Bowes, Inc., Stamford, Conn. The basic Model 5300 postage meter is a mechanical device with mechanical registers and actuator assemblies. The modified meter contains only the print drum 78 and a set 80 of print wheel driving racks 80a, 80b, 80c, 80d. All mechanical registers and actuator assemblies have been removed.
The print wheels (not shown) within print drum 78 are set by a mechanism driven by a first stepping motor 82 and a second stepping motor 84. Signals for controlling the operation of the stepping motors 82 and 84 are provided through the output ports 37 and 39 of the control system. Further details of the connections between the output ports 37 and 39 and the coils for the stepping motors 82 and 84 are provided later in the specification.
The stepping motor 82 drives the set 80 of postal wheel driving racks through a gearing assembly including upper and lower nested shafts. Only the upper set of nested shafts of 86a, 86b is shown. The angular settings of the nested shafts are controlled by a master gear 88 which may be driven in either a clockwise or counterclockwise direction by the stepping motor 82.
The print drum 78 has four independently-positioned print wheels (not shown) which provide a postage impression to the maximum sum of $99.99. Each print wheel provides a separate digital sum and can be set from "0" to "9". The print wheels are sequentially set by the meter setting mechanism by means of the four driving racks 80a, 80b, 80c, 80d which are slidable within a print drum shaft 90 in the directions indicated by the double-headed arrows 92.
The settings of the upper racks 80a, 80b are controlled by pinion gears 94a, and 94b, respectively. The settings of the lower racks 80c and 80d are controlled by a similar set of pinion gears, not shown in the drawings.
The pinion gear 94a is connected to the inner shaft 86a while the pinion gear 94b is connected to the concentric outer shaft 86b. The pinion gears which control the settings of driving racks 80c, 80d are similarly attached to the lower set of nested shafts, not shown. The angular positions of the nested shafts are controlled by shaft-mounted spur gears, of which only the upper spur gears 96a, 96b are shown.
The master gear 88 can be shifted laterally along an axis parallel to the axis of the spur gears, including gears 96a and 96b, to intermesh with a single gear at a time. The master gear 88 is rotatably mounted within a slot 98 in a yoke 100 which slides along a splined shaft 102. The yoke 100 is held away from rotatable engagement with splined shaft 102 by an interposed sleeve bushing 104. The yoke 100 includes a pair of upper and lower tooth troughs located on the upper and lower surfaces of the yoke 100. Only the upper tooth trough 106 appears in the drawing. As the yoke 100 and master gear 88 slide laterally along the splined shaft 102, the upper and lower laterally-extending tooth troughs entrap a tooth of each of the spur gears. The tooth troughs prevent rotational movement of any of the spur gears other than the spur gear meshed with the master gear 88.
The lateral position of yoke 100 is controlled by a stepping motor 84, the output shaft of which carries a splined gear 108. The splined gear 108 meshes with a rack 110 attached to yoke 100 at an L-shaped lower extension 112. The rotation of splined gear 108 upon energization of stepping motor 84 is translated into lateral movement of yoke 100 through the rack 110 and pinion or splined gear 108. The splined gear 108 also serves to prevent counter-clockwise rotation of yoke 100 about the axis of shaft 128 of stepping motor 82 during energization of that motor which might otherwise occur due to friction between rotating sleeve bushing 104 and the yoke 100. A roller 114 mounted beneath the L-shaped extension 112 prevents any clockwise movement of the yoke 100 about the axis of shaft 128.
When the print wheels within print drum 78 have been set to the correct postage value position, drum 78 is rotated by shaft 90 in a direction indicated by arrow 116 to imprint the postage. The drum 78 is then returned to a home or rest position sensed by a slotted disk 118 mounted on shaft 90. When a slot 120 in disk 118 is interposed between the arms of an optical detector 122, the shaft 90 is at its home position.
All optical detectors in the setting mechanism are basically U-shaped structures having a light emitting diode located in one arm and a phototransistor located in the other arm. Light emanating from the light emitting diode is transmitted to the phototransistor only when a slot in an interposed disc is aligned with the arms of the detector.
The home or "0" positions of nested shafts 86a and 86b are similarly sensed by slotted discs 124a and 124b, respectively, in combination with optical detectors 126a and 126b. The home or "0" positions of the lower pair of nested shafts are sensed by similar slotted discs and optical detectors, none of which are shown in the drawing.
The shafts and gears are returned to the home position upon startup of the meter. Subsequent setting is accomplished by stepping the motor 82 through a calculated number of steps using previously-established settings as a reference.
The angular movement of the stepping motor shaft 128 (and consequently splined shaft 102 and master gear 88), is monitored by means of an assembly of gears 130 and 132, slotted monitoring wheel 134 and optical detector 136. Gear 130 is rigidly mounted on and rotates with the stepping motor shaft 128. Gear 130 meshes with gear 132 which is attached to and rotates with the slotted monitoring wheel 134. Gears 130 and 132 are of the same diameter and cause slotted monitoring wheel to rotate through the same angles of rotation as stepping motor shaft 128. Each slot on slotted monitoring wheel 134 corresponds to a change of one unit of postage value. Every fifth slot 138 on monitoring wheel 134 is extra long to provide a check on the monitoring operation. Optical detector 136 has two photosensors. One of the photosensors is mounted deeply within the detector; that is, near the periphery of slotted monitoring wheel 134. The other sensor is located nearer the center of the slotted monitoring wheel 134. The latter photosensor receives light from an associated light source on the opposite side of the slotted monitoring wheel 134 only when the extra long slot 138 is aligned within the detector. Thus, this photosensor provides an output every fifth step of the monitoring wheel 134.
The output signals produced by the other photosensor are counted in the control system. If a count of five is not detected when the extra long slot 138 is aligned within detector 136, an error condition exists. Similarly, if the extra long slot 138 is not detected when a count of 5 has been accumulated, an error condition exists.
The lateral position of yoke 100 and master gear 88 is monitored by a position indicator including a pair of spaced plates 140 and 142 attached directly to yoke 100. The plates 140 and 142 include slot patterns which are a binary-encoded representations of different positions of the yoke relative to optical detectors (not shown) which would be attached to a bracket on stepping motor 84.
Preferably, plates 140 and 142 have five or more binary slot patterns identifying an equal number of lateral positions of the yoke 100. Each of the slot patterns consists of a unique triplet in which the presence of the slot in one of the plates 140, 142 is interpreted as a binary 1 while the absence of a slot in any position where a slot might appear is interpreted as a binary 0. The binary indicia for the two outside positions in each triplet are included in plate 140. The binary indicia for the center position in each triplet is included in plate 142.
The binary indicia are distributed between two vertically-aligned plates in one embodiment of the invention only because available optical detectors are too bulky to permit three detectors to be placed side-by-side on the single plate of reasonable size. From a logic standpoint, there would be no significance to the fact the indicia are distributed between two plates. The indicia would be read and interpreted as if they were contained on a single plate.
The binary signals produced by the optical detectors associated with plates 140 and 142 are internal inputs to the postal meter 10. These signals, along with other signals, are part of the meter setting detector array 30 shown in block diagram form in FIG. 3.
The electrical interconnections of the stepping motors 82 and 84 with the output ports 37 and 39 are described with reference to FIG. 5. The four parallel output leads from output/port 37 are connected to the coil select circuits 44 and 46 for the stepping motors 82 and 84, respectively. Each of the stepping motors is a conventional eight-phase stepping motor, which is rotated in predetermined angular increments by energizing different combinations of four coils contained within the motor.
The coils for stepping motor 82, included within a coil system 144, are identified as coils 144a, 144b, 144c and 144d. Similarly, the coil system 146 for motor 84 includes coils 146a, 146b, 146c, 146d. Each of the individual coils in each motor is connected in series with a Darlington amplifier. For example, coil 144a, is connected in series with Darlington amplifier 148a in which the base terminal of a first transistor 150 is connected to output port 37. A second transistor 158 has a grounded emitter, a base terminal connection to the emitter of transistor 150 and a collector connected to the collector of transistor 150. Darlington amplifier 148 is off or nonconducting when the associated output 162 from output port 37 is at a binary 0 or ground potential. In this state, the Darlington amplifier prevents current flow from an associated ground terminal 160 through the second transistor 158 and thus through coil 144a. When the output 161 drops to a more negative or binary 1 level, the Darlington amplifier 148a is switched to an on or conducting state.
Darlington amplifiers 148b, 148c, and 148d are identical to amplifier 148a except for the connections to different output leads and different motor coils.
The coils in coil system 146 are similarly connected in series with Darlington amplifiers 160a, 160b, 160c, 160d. Corresponding coils in each of the coil systems 144 and 146 are connected to the same output terminal of output port 37. For example, coils 144b and 146b are connected through respective Darlington amplifiers 148b and 160b to output 162. A binary 1 signal on output 162 switches both Darlington amplifiers 148 and 160b into their on or conducting state. However, coil current will be established in only the motor selected by operation of motor select circuit 48.
Motor select circuit 48 is connected to outputs from output port 39 and comprises switching circuits 164 and 166 connected in series with coil systems 144 and 146, respectively.
Switching circuit 164 includes an inverter amplifier 168 which provides an increased current at its collector terminal when the input to the amplifier 166 falls to the more-negative binary 1 level. The output of inverter amplifier 168 is applied to a Darlington amplifier 170 which, when conducting, provides a current path from a ground for each of the coils in coil system 144 to a -24 volt source 172.
The preferred embodiment of the improved input/output channel which links postal meter 10 and input/output unit 12 is described in detail with reference to FIG. 6. To simplify the drawing, postal meter 10 is shown as including only output port 39 and input buffer 76. Binary signals to be transmitted to the output section of output unit 12 from postal meter 10 are applied in serial fashion to an electrical-to-optical transducer 173. The signals are applied at the base terminal of a transistor 174 having a grounded emitter and a collector connected to the anode of a light-emitting diode 176. The cathode of diode 176 is connected to a -15 volt source 178 through a current-limiting resistor 180.
The light-emitting diode 176 is adjacent one end of a first light-transmitting fiber 182, the opposite end of which is adjacent a phototransistor 184 in a first optical-to-electrical transducer circuit 183.
The emitter of phototransistor 184 is connected to one input of a comparator amplifier 186, the second input to which is provided through a voltage divider 188 connecting a ground terminal to a -15 volt source 192. The input to the comparator amplifier 186 provided through the voltage divider 188 establishes a threshhold voltage which the output of phototransistor 184 must exceed before the transistor output will be read as a binary 1 signal. The threshold voltage reduces the chance that noise voltages generated within postal meter 10 or either of the transducers 173 or 183 will be interpreted as binary 1 signal voltages. Binary signals representing data or instructions to be input to the postal meter 10 from the input section of unit 12 are applied to a second electrical-to-optical transducer circuit 198. The signals are applied at the base terminal of a transistor 194 in circuit with a light-emitting diode 196 adjacent one end of a second light transmitting fiber 200. The opposite end of fiber 200 is adjacent a phototransistor 202 in a second optical-to-electrical transducer 204. Transducer 204, which is identical in construction to transducer 183, converts the optical signals to electrical signals which are applied to one input of buffer circuit 76 of postal meter 10.
Since the input/output information transmitted through the channel 14 is transmitted in the form of optical signals and since extraneous electric fields cannot induce noise voltages in such optical fibers, the channel 14 effectively resists induction of such noise voltages. Of course, light-transmitting fibers 182 and 200 must be coated or otherwise shielded from extraneous light.
Moreover, because the maximum output of the light emitting diodes is limited, the occurrence of a voltage surge or a static electrical discharge at the input/output unit cannot be transmitted at destructive levels to the postal meter 10. Even a direct short circuit across one of the electrical-to-optical transducers will not be destructive, since the output of the optical-to-electrical transducer is also inherently limited regardless of the intensity of the optical input.
FIG. 7 shows, in simplified form, one form of the preferred embodiment of the invention. In this arrangement, a secure housing 250 for a postal meter encloses a printing device 251, of conventional type, such as the modified model 5300 postage meter of Pitney Bowes, Inc., as disclosed in U.S. Pat. No. 4,050,374. In addition, the secure housing encloses an electronic accounting system 252 of the type above described, for example, with reference to FIGS. 2 and 3. The printing device discussed with reference to FIG. 4 is particularly adaptable in a postal meter of this type.
Such a postal meter is generally self-contained, in the sense that all of the critical functional elements of the accounting system are provided within the secure housing. The term "critical" is employed herein in the sense that such elements are necessary to maintain a complete and accurate record of any postage that has been printed, as well as a programmed system for ensuring the accurate printing of such postage in accordance with a determined program. It is therefore evident that these elements are provided within the secure housing 250, in order to insure that they are not tampered with, and that the registers provided therein thereby accurately and dependably record the printed postage and are substantially not subject to external influence.
On occasion, it is desirable to provide a postal meter of the above type as part of a larger system, such as, for example, an office system wherein a control panel and various displays may be positioned remotely of the postal meter itself. Such systems thereby require a communication path, such as the path 255, thereby enabling the communication between the postal meter and the input/output peripherals. The peripheral devices may of course constitute the only source of signals corresponding to the postage that is desired to be printed, i.e., the postal meter itself may not necessarily originate such signals since such information is not critical.
The communication path in accordance with the invention is preferably, although not necessarily, a fiber-optic cable, so that the signals may be carried in the form of pulses of light. These signals, in accordance with the invention, are directed, preferably serially, through a port 256 in the postal meter to interface with a transducer 257. While this system is essentially shown with respect to FIG. 3, and, in a proper system, photo transistors of the type illustrated in FIG. 6 may be employed, it is particularly to be noted that the transducers 257 are disposed at some distance within the secure housing. In the event that the communication path comprises a fiber-optic cable, the transducer may be in the form of photo-electric detection means, whereas if the communication path is in the form of an electric signal conveying cable, the transducer means 257 may be in the form of an optical-electric coupler. In other words, in accordance with the invention, it is apparent that the conversion of light signals to electric signals occurs within the secure housing, independently of the form of communication path employed. As a result, the application of high voltages by any means to the communication path will not result in the application of high voltage to the electronic system of the postal meter, unless, of course, such high voltages were applied in such a manner that damage due to their application is readily visible or detectable. Thereby, it is not possible to tamper with the postal meter of the invention by this technique, such that the tampering is undetectable or results in a wiping out of the memories of the electronic system.
In other words, in accordance with the invention, the transducer electrically isolates the electronic accounting system from receiving externally derived potentials that may erase the memories therein or otherwise damage the accounting system. Therefore, any such erasing of the memories or the like must be accompanied by physical evidence of the tampering. The positioning of the transducer is thus, broadly stated, not primarily to inhibit damage to the transducer, but to prevent defeat of the accounting system as a result of undetectable tampering. While it is preferred that opto-electronic coupling be employed for this purpose, it is, of course, apparent that other techniques may alternatively be employed. Thus, acoustic-electric, or saturable magnetic-electric coupling, may similarly be employed with the communication path being adapted thereto.
It is, of course, generally preferred that the communications path be removable from the postage meter, and for this purpose the entry of the communication path 255 to the port 256 may be by way of the releasable coupling or clamp 277. It will be noted in FIG. 7 that the communication path extends for some distance from the clamp into the interior of the housing 250, this path extending, for example, through a conduit 260 or the like in the postal meter. Thereby, upon removal of the communication path, the transducer means 257 may be exposed by way of the port. In accordance with the invention, however, the conduit 260 is sufficiently long and has a sufficiently small diameter that effective entry of a damaging probe into the secure housing is inhibited. In any case, only the transducer might be damaged by the probe. Such damages would be physical and thus detectable. Destruction of the transducer would destroy the communication path but not the internal electronics, thereby allowing a post office or factory inspection to become aware of the damage upon opening up the meter. Any efforts to defeat the system by the application of voltages within the port would therefore be readily detectable to the postal authorities.
It will, of course, be appreciated that the showing of FIG. 7 is schematic only, and the actual extension of the communication path into the secure housing 250 may be significantly greater.
In the alternative arrangement of FIG. 8, instead of providing a straight conduit 260, a convoluted conduit 260a is employed in order to inhibit external access to the transducer means 257. The conduit 260a may be curved so as to permit the bending therein of flexible communication path members, while inhibiting passage of any rigid elements that may be inserted into the port for the purpose of tampering.
It is again noted that the effect of tampering will be physically evident. Attempts to destroy the memory, as by high current or voltage sures will be ineffective as a result of the non-conductive path. In the case of an optical transducer, electrical surges will only overload the transducer element coupled to the electrical input portion. If the optical portion is accessed, and an optical overload introduced, only the receiving transducer will overload. In either event, no damage to the memory will occur.
In a still further embodiment of the invention, as illustrated in the enlarged cross section of FIG. 9, an insert such as a disc 265 may be provided permanently fixed in the wall 250 of the secure housing, the disc 265 having one or more small diameter holes 266 extending therethrough. The holes 266 are aligned with active areas of the transducer means 257 and the individual fine fibers 267 of the communication path 255 extend through separate holes 262 in the disc to engage the transducer means 257. A cable clamp 277 holds the fibers of the path 255 in their relative position. The transducer means 257 is preferably spaced from the disc 265, and the holes 266 have small diameters, such as, for example, 0.002", such that the application of damaging potentials to the transducer means 257 by way of these holes is practically impossible. While the communication path 255 is, in this case, preferably a fiber optic cable, it will be appreciated also that it may be comprised of one or more relatively fine conductors, as in the arrangement of FIG. 7.
In the arrangement of FIG. 9, the disc 265 is preferably of a material that is no less easy to penetrate than the wall of the housing 250, and the disc 265 may be held in position by any conventional means so as to not be removable exterially of the housing.
While there has been described what is considered to be a preferred embodiment of the invention, variations and modifications therein will occur to those skilled in the art once they become familiar with the basic concepts of the invention. Therefore, it is intended that the appended claims shall be construed to include all such variations and modifications as fall within the true spirit and scope of the invention.
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An improved input/output channel for linking a computer control unit for an electronic postal meter to input/output units. The invention includes a converter for converting unit-output electrical signals to non-conductive carrier signals and for converting the non-conductive carrier unit-input signals back to electrical signals. Non-conducting means are used to transmit the signals between the meter and the input/output units so that any attempts to interfere with meter operation will, of necessity, involve physical evidence of tampering, observable to an inspector.
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TECHNICAL FIELD
The present invention relates to a window screen. More particularly, the invention relates to a window screen having strong components that may be used as an impact protective system, particularly for window protection from impacts due to debris from wind storms, hurricanes, tornados and the like, as well as vandalism.
BACKGROUND OF THE INVENTION
Windows are typically provided in structures such as residential homes, schools, office buildings and other buildings designed primarily for human occupation. Oftentimes it is desirable to allow for the windows to be opened so that outside air may enter the building. Screens are typically provided on such window openings so that air may pass through the window opening, but undesirable objects such as insects are kept outside of the building. Most prior art screens are made of aluminum mesh and do not have adequate strength to protect against window breakage. Also, whether the window can open or not, prior art screens are known that can protect window glass from damage, if strong enough.
In areas that are subject to high winds, such as areas that may experience hurricanes or tornados, it is desirable to provide a screen that will protect window glass from flying debris. Additionally, buildings that are prone to be vandalized, such as schools and low income housing, use screens to protect against glass breakage. One prior art screen that provides protection against glass breakage comprises stainless steel mesh within an aluminum frame.
However, in the prior art, the mesh and the glass are proximate one another. As a result, deflections of the mesh from impacts to the mesh by objects could result in glass breakage.
SUMMARY OF THE INVENTION
The invention of the application is a high strength window screen frame adapted to fit within a window opening in an exterior wall of a building in front of a window pane. The window screen frame includes an extruded metal frame that defines an opening for receiving mesh. A fascia portion of the extruded metal frame is provided on the frame proximate the opening. A standoff leg portion of the extruded metal frame extends rearward from the fascia portion. The standoff leg portion is longer than the fascia portion to provide sufficient separation between the window pane and the mesh to prevent deflections in the mesh from making contact with the window pane. Heavy duty mesh screen is preferably used with the high strength window screen frame of the invention. The window screen frame is screwed by fasteners to an exterior wall surrounding a window opening of a structure.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a window screen frame of the invention.
FIG. 2 is a front view of the window screen frame of FIG. 1 .
FIG. 3 is a back view of a screen frame of FIG. 1 .
FIG. 4 is perspective cross sectional view of the window screen frame of the invention taken along line 4 — 4 of FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1, a high strength window screen frame 10 includes an extruded metal frame 12 . Preferably, the extruded metal frame is a hollow extruded aluminum frame. Variations may exist in the cross-sectional configuration, depending upon building materials and the type of window used in conjunction with the high strength window frame 10 . High strength window frame 10 is made up of window frame units 11 (FIGS. 1 - 3 ) mounted together to make up a single screen for a window. Window frame units 11 have a front 14 , a back 16 , and four frame members 17 that define an opening 18 . Extruded metal frame 12 is designed to be used in conjunction with a window opening in a wall 13 of a structure.
Frame 12 is L-shaped, having a fascia portion 20 (FIGS. 1, 2 , and 4 )of frame 12 that is provided on a forward end of extruded metal frame units 11 nearest openings 18 . Screen plate portion 20 has a front face 24 FIGS. 1, 2 , and 4 ), a rear face 26 (FIG. 3 )and an inside surface 28 . A standoff leg portion 30 (FIG. 4) of frame 12 extends rearwardly from fascia portion 20 . Standoff leg portion 30 is provided with longitudinal teeth or serrations 31 . Standoff leg portion 30 extends rearward from rear face 26 approximately 1.4 times the dimension of front face 24 from outer edge 35 b of frame 12 to inside surface 28 in the preferred embodiment. Preferably, front face 24 is approximately 1.4 inches from outer edge 35 b to inside surface 28 of frame 12 , inside surface 28 is approximately 0.5 inches from front face 24 to rear face 26 , and standoff leg portion 30 extends approximately 2.5 inches rearward from front face 24 to a rear face at groove 40 . The relatively longer length of the standoff leg portion 30 results in an extended standoff of mesh 32 relative to glass pane 34 (FIG. 4 ). The standoff is between approximately 2 to 5 inches in the preferred embodiment, which protects glass pane 34 from damage that might occur from any deflection of mesh 32 that might be caused by an impact of an object with the mesh. It should be noted that the dimensions recited herein are provided for the purpose of example only. Other suitable dimensions may be used within the scope of the invention.
Within a single window, depending on the length, there may be several frame units 11 . The upper edge 35 a (FIGS. 1, 2 , and 4 ) of the lowest frame unit 11 abuts the lower edge 35 b (FIGS. 1, 2 and 4 ) of the next upward frame unit 11 . The drawings show three frame units 11 . A cap 36 (FIGS. 3 and 4) is provided to fit over ends of standoff leg portion 30 to secure multiple window frame units 11 together. Cap 36 is a metal channel member with two side walls 37 a , 37 b and a base 38 (FIGS. 3, 4 ). A serrated portion 39 (FIG. 4) is on an inside surface 38 of each sidewall 37 a , 37 b for engaging longitudinal serrations 39 on standoff leg portion 30 . Standoff leg portions 30 are preferably provided with channels or grooves 40 that mate with a tongue 40 a on cap 36 . Additionally, end bracket supports 41 (FIG. 3) may be provided at ends of window frame units 11 that are not adjacent to other window frame units 11 . End bracket supports 41 provide additional strength to window frame units 11 .
Referring now to FIG. 4, a metal screen plate stiffener 52 is removably affixed to rear face 26 of fascia portion 20 with a plurality of self-tapping sheet metal screws 54 . Screen plate stiffener 52 is a channel strip, having a pair of outer rims 56 and a base 57 that define a longitudinal channel 58 . An inner slot 60 is formed on an inner surface of outer rims 56 . A slidable plastic cover 62 is received within interior slots 60 on the screen plate stiffener 52 . Screen plate stiffener 52 is secured to the rear face 26 for securing a heavy duty mesh screen 32 . Screws 64 (FIGS. 1-3) extend through front face 24 and the standoff portions 30 of frame 12 around the perimeter of frame 12 . Screws 64 engage structure within an opening in an exterior wall to secure frame 12 within the opening.
In use, the window screen frame 10 of the invention is positioned within an opening in wall 13 . Screws 64 (FIGS. 1, 2 and 3 ) secure extruded metal frame 12 to wall 13 . Screws 64 extend through frame 10 to secure window frame 12 within wall 13 . Window pane 34 is recessed from mesh screen 32 a considerable distance. The extended standoff leg portion 30 provides a standoff distance from mesh 32 to glass pane 34 that provides additional protection to glass pane 34 . Additionally, multiple window frame units 11 result in fascia portions 20 that extend horizontally across the face of the window frame 10 . The fascia portions 20 are integral parts of the individual window frame units 11 . The use of individual window frame units 11 provide strength to the window frame 10 and provide additional support to the mesh 32 . Standoff leg portion 30 of adjacent window frame units 11 , which contact one another, are secured together with cap 36 .
The invention has numerous advantages. The window frame of the invention has features to protect window glass and to provide extra strength to the window frame. The high strength construction of the frame, when used in conjunction with heavy steel mesh screen, provides an impact protective system that protects window glass from flying debris. The extended standoff leg portion of the window frame provides an extended standoff of the window pane from the mesh screen. Additionally, the multiple window frame units are combinable to form a strong window frame having connected adjoining cross-members. The window frame of the invention provides strength and protection to windows and is an attractive alternative to other devices, such as burglar bars or boarding up windows. An additional advantage is that the high strength window screen frame of the invention may be easily installed on existing structures.
While the invention has been shown in only one of its forms, it should be apparent to those skilled in the art that it is not so limited, but is susceptible to various changes without departing from the scope of the invention.
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A high strength window screen frame that includes an extruded metal frame that fits within a window opening in a building. The frame is made up of a plurality of window frame units, each defining an opening and covered with mesh. A standoff leg portion of the window frame units provides a standoff separation of the mesh from a glass pane so that when objects strike the mesh and deflect the mesh, the glass pane is not impacted.
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RELATED APPLICATIONS
This application is a divisional of U.S. application Ser. No. 12/614,231, filed Nov. 6, 2009.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OF DEVELOPMENT
This invention was made with Government support under Contract No.: HR0011-07-9-0002 awarded by (DARPA) Defense Advanced Research Projects Agency. The Government has certain rights in this invention.
CROSS REFERENCE TO RELATED APPLICATIONS
This application is related to the following commonly-owned, co-pending United States Patent Application filed on even date herewith, the entire contents and disclosure of which is expressly incorporated by reference herein in its entirety: U.S. Patent Application Serial No. (24258), for “AXIOCENTRIC SCRUBBING LAND GRID ARRAY CONTACTS AND METHODS FOR FABRICATION”.
BACKGROUND
The present invention relates generally to the electrical contact structures in the field of microelectronics, and more particularly, relates to electrical contact structures and a method for manufacturing the same for microelectronics and semiconductor manufacturing.
Typical Land Grid Array (LGA) interconnects are 2-dimensional arrays of compliant electrical contacts that are sandwiched between two electrical devices, and pressed together to establish electrical contact in an electrically connected package. The application of force using hardware which surrounds both electrical devices provides the pressing together of the electrical devices. Primarily, varieties of LGAs include: 1.the geometry and constituent materials of the individual contacts; 2.the method of fabrication. The method of fabrication typically includes: 2a.one-shot array formation, i.e., molded or sheet stamped; and 2b.sequential placement of individual contacts to form an array. Example of known LGA fabrication techniques are disclosed in U.S. Pat. Nos. 7,331,796. 7,137,827, and 7,452,212, all of which are commonly assigned with the instant application, and the subject matter of which are hereby incorporated by reference in their entirety.
However, decreasing the size of contact structures negatively affects mating of electrical contacts on each of the electrical devices being pressed together. For example, scaling LGA contact xy dimensions sacrifices z-dimension compliance or true positions (TP) when electrical contacts are pressed together to form an electrically connected package.
It would be desirable to provide an electrical contact structure and method for manufacturing the same which provides smaller scaling of the contact structure with increased contact between electrical contact structures. There is further a need for a method and structure which provides smaller contact size (xy dimension) for LGAs, without sacrificing contact mating (z direction) in an electrical package.
BRIEF SUMMARY
In an aspect of the present invention, a method for manufacturing a contact structure for microelectronics manufacturing, comprises: forming first and second metal sheets to form a plurality of outwardly extending bump each defining a cavity; symmetrically mating the first and second metal sheets in opposing relation to each other to form upper and lower bumps each defining an enclosure therebetween, the mated first and second sheets forming a contact structure; coating the contact structure with an insulating material; and fabricating helix shaped contacts from upper and lower bumps, the helix shaped contacts having first and second portions being in mirror image relationship to each other.
In a related aspect, the bump is frustoconical shaped. The method may further comprise: applying a plurality of conductive metal coatings to the bumps. The fabricating of the helix shaped contact may include using photolithography. The method may further comprise: positioning at least one contact point on each of the contacts between a pair of semiconductor substrates including electrically conductive members; and positioning the at least one contact point on each of the contacts to electrically communicate with respective electrically conductive members to form an electrically conductive package. Also, the method may further comprise: compressing the contacts between the semiconductor substrates such that the contacts twist on the electrically conductive members during the compression. Further, the method may further comprise: positioning a insulting carrier between the first and second metal sheets; and passing a conductive via through the insulating carrier between the upper and lower bumps. The method may further comprise: forming third and fourth metal sheets to form a plurality of outwardly extending bumps each defining a cavity, the third and fourth sheet bumps and corresponding cavities being larger than the bumps of the first and second metal sheets; positioning the third and fourth metal sheets over the first and second metal sheets in mating relation to form the contact structure.
In another aspect of the invention, a method for manufacturing a contact structure for microelectronics manufacturing, comprises: forming first and second metal sheets to form a plurality of outwardly extending bumps each defining a cavity; symmetrically mating the first and second metal sheets in opposing relation to each other to form upper and lower bumps each defining an enclosure therebetween, forming third and fourth metal sheets to form a plurality of outwardly extending bumps each defining a cavity, the third and fourth sheet bumps and corresponding cavities being larger than the bumps of the first and second metal sheets; positioning the third and fourth metal sheets over the first and second metal sheets in mating relation to form a contact structure; coating the contact structure with an insulating material; and fabricating contacts of a predetermined geometric shape from the upper and lower bumps and the third and fourth sheet bumps.
In a related aspect, the contacts are helix shaped contacts, the helix shaped contacts having first and second portions being in mirror image relationship to each other.
In another aspect of the invention, a contact structure for microelectronics, comprises: a contact structure including symmetrically mated first and second metal sheets in opposing relation to each other, the contact structure including third and fourth metal sheets being positioned over the first and second metal sheets in mating relation; upper and lower contact bumps of a predetermined geometric shape extending from the first, second, third and fourth metal sheet combination.
In a related aspect, the contact bumps are helix shaped contacts, and the helix shaped contacts having first and second portions being in minor image relationship to each other. The first and second portions may be right and left handed helixes, respectively. The upper and lower contact bumps may be symmetrical about a vertical axis bisecting the upper and lower contact bumps. The structure may further include: a pair of insulating substrates including electrically conductive members, and at least one contact point on each of the upper and lower contact bumps are attached and electrically communicating to respective electrically conductive members such that the upper and lower contact bumps between the pair of semiconductor substrates form an electrically conductive package; and the upper and lower contact bumps between the pair of semiconductor substrates being in a compressed state relative to an at rest state, the upper and lower contact bumps being helix shaped, and the helix shaped contact bumps having first and second portions being in mirror image relationship to each other; and a rotational displacement of the upper and lower contact bumps on the electrically conductive members between the compressed state and the at rest state. The method may further comprise: a pair of insulating substrates including electrically conductive members, and at least one contact point on each of the upper and lower contact bumps are attached and electrically communicating to respective electrically conductive members such that the upper and lower contact bumps between the pair of semiconductor substrates form an electrically conductive package; and the upper and lower contact bumps between the pair of semiconductor substrates being in a compressed state relative to an at rest state, and the first, second, third and fourth metal sheets move independently when the electrically conductive package moves from the at rest state to the compressed state. In a related aspect, the first, second, third and fourth metal sheets move radially outward with respect to a vertical axis passing through the upper and lower contact bumps when the electrically conductive package moves from the at rest state to the compressed state.
In another aspect of the invention, a process for manufacturing a contact structure for microelectronics manufacturing, comprises: providing at least one metal sheet; forming the metal sheet to form a plurality of outwardly extending bumps each defining a cavity; coating the molded element with a layer of photoresist; and fabricating contacts of a predetermined geometric shape from the bumps using photolithography and etching. In a related aspect the predetermined geometric shape is a helix shaped contact.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
These and other objects, features and advantages of the present invention will become apparent from the following detailed description of illustrative embodiments thereof, which is to be read in connection with the accompanying drawings. The various features of the drawings are not to scale as the illustrations are for clarity in facilitating one skilled in the art in understanding the invention in conjunction with the detailed description. In the drawings:
FIG. 1 is flow chart of a method of the invention according to one embodiment of the invention;
FIGS. 2A-2F are diagrammatic views of process steps depicting the process for manufacturing a hollow LGA array according to an embodiment of the invention;
FIG. 2G is a cross sectional isometric view of the structure shown in FIG. 2C having an array of frustoconical protuberances;
FIG. 3 is an isometric view of an illustrative metal and photo resist coated drawn metal bump with hollow interior sitting within a form fitting cavity of an upper portion of a mask;
FIG. 4A is an isometric view of an insulating carrier with vias according to another embodiment of the invention;
FIG. 4B is a side elevational view of a drawn metal sheet having frustoconical bumps;
FIG. 4C is an isometric view of the carrier and vias of FIG. 4A mated with the frustoconical bumps of FIG. 4B ;
FIG. 5A-5D are diagrammatic views of process steps depicting the process for manufacturing a hollow LGA array according to another embodiment of the invention.
FIG. 6 is a plan view of a mask pattern shaped as a four leg helix;
FIG. 7 is an isometric view of a helix spring contact;
FIGS. 8A-8B are isometric views of helical contacts in reverse directions;
FIG. 8C is a side elevational view of a contact assembly having helical contact in mirror image relation separated by a carrier element;
FIG. 8D is an isometric view of the contact assembly in FIG. 8C ; and
FIG. 9 is an isometric view of a plurality of helical contacts used in high frequency electrical simulation.
DETAILED DESCRIPTION
Referring to FIG. 1 , a method 10 according to one embodiment of the present invention includes the general steps below including step 14 for beginning the formation process of a 2D array of land grid array (LGA) contacts. In step 20 , protrusions are made from spring metal by deep drawing sheet metal into arrays of pockets. A thin second metal coating, for example, gold for joining purposes or Be for alloying, may be formed over the array of pockets in metallization step 24 .
The next step 30 includes joining two metal sheets each having a mating array pattern of pockets. The sheets are joined back to back as shown in FIG. 2C using metallurgical bonding techniques, for example, gold-gold joining, soldering, electron beam welding, copper to copper thermobonding, etc. The joined sheets form a contact structure having metal protrusions opposite one another.
Step 40 includes injection molding a plastic carrier plane onto one side of the joined metal sheets, or alternatively, inserting contacts into a perforated plane and gluing in place.
The contact structure is coated with additional metal layers in some embodiments and photo resist in step 48 . In one embodiment of the invention, a conformally coating resist such as electrophoretically deposited resist is used to coat the metal protrusions.
A metal mask (shown in FIG. 3 ) on both sides of the LGA protrusions includes cavities 212 of complementary shape to the protrusions and is placed over an array of protrusions in steps 52 and 56 . The cavities are of similar shape to a desired contacts, but slightly larger to account for the photo resist thickness and any tolerance. The masks have patterns in the top formed as slots by wire electric discharge machining (EDM), laser, and chemical etching or other techniques. The patterns transmit light into a pattern onto the photo resist covered contacts or LGA protrusions, without allowing for significant reflections from one contact to another because they are nestled into individual cavities. Referring to FIG. 3 , a top portion of the mask is shown, a bottom portion (not shown) is clamped together with the top portion of the metal mask to encase the protrusions.
An ultraviolet light (of specified wavelengths) is shined onto the photo resist in step 60 . The photoresist on the contact structure sandwiched between the top and bottom metal masks is sensitive to the light. The clamped together metal masks are rotated and tilted during illumination to optimize uniformity of exposure on every surface of the photo resist covered contact structure.
The masks are removed and the resists are developed in step 64 . For example, development of the resists is by etching away unwanted metal to reveal a desired pattern of contacts and to separate contacts from one another.
Referring to FIG. 2A , a process 100 for manufacturing hollow LGA array using a mold includes a flat sheet metal 104 . The flat sheet metal 104 is subjected to deep drawing to provide deep wells 112 resulting in bumps or protuberances 114 on the opposite side of the flat sheet metal 104 as shown in FIG. 2B to provide a single contact array structure 110 . Two single contact array structures 110 are joined metallurgically back to back as shown in FIG. 2C , with the wells 112 and protuberances 114 opposite one another to form combined contact array structure 120 .
A thin layer of insulator 126 is coated on one side of the contact array structure 120 to hold together the two structures 110 as shown in FIG. 2D and to maintain the array positioning after etching to singulate the bumps 140 as illustrated in FIG. 2F . The protuberances 114 are coated with photoresist 130 as shown in FIG. 2E , and developed to expose metal in a desired pattern, for example a helix, and to singulate the contacts from one another. The exposed metal is then etched away to form a pattern, for example, a helix, forming a helix spring contact 140 , as shown in FIG. 2F . Referring to FIG. 2G , an array of joined structures 120 is shown in isometric view and cross section.
Referring to FIG. 3 , an illustrative mask and hollow bump combination 200 includes a metal and photo resist coated hollow bump having a top portion 204 and a bottom portion 206 the thin insulator on one side is shown in FIG. 3 reference numeral 208 . The bump sits within a form fitting cavity 212 of a top portion of a mask solid 210 . The mask solid 210 includes a pattern 216 open to the outside. This example shows a slot pattern 216 , however, other patterns including multileg helix patterns can be used. A bottom portion of the mask (not shown) typically is clamped together with the top portion 210 . The closed mask solid is rotated and illuminated to provide light access through the slot pattern 216 , producing the desired image on the bump 204 , 206 .
Referring to FIG. 4A , another embodiment of the invention includes a insulating substrate or carrier, for example, a printed circuit board (PCB) 300 , between two drawn metal sheets 350 , shown in FIG. 4B , having frustoconical bumps 354 in geometric relation similarly to the structure 120 shown in FIG. 2C . The PCB 300 includes conducting vias 304 therethrough. After lithography, the contacts 360 shown in FIG. 4C are electrically communicating using the conducting vias 304 , and the metal portion 358 between the frustoconical bumps 354 has been etched away.
Referring to FIGS. 5A-5D , another embodiment according to the invention includes two metal sheets 400 as shown in FIG. 5A . The metal sheet 400 are drawn and patterned similarly to form a first patterned sheet 404 having bumps 408 , and a second patterned sheet 410 having bumps 414 . A cavity 406 formed by the bump 408 is larger than a cavity 412 formed by bump 414 . The bumps and cavities are positioned to mate when the first sheet 404 is positioned over the second sheet 410 , as shown in FIG. 5C . The first and second sheets 404 , 410 , respectively, are metallurgically joined on the flat surfaces and adjacent in the overlapping bump areas to form nested structure 411 . A second combination of first and second sheets 404 , 410 is mated with the first combination shown in FIG. 5C to form the combined structure 450 shown in FIG. 5D to form an array of hollow bumps. A pre-coat 454 (e.g., of Au) (not shown) may be formed over the nested structure 411 for joining the two sides back to back as shown in FIG. 5D reference numeral 450 . The resulting structure has a thin insulating layer molded to one side for mechanical structure. Etching is performed to impart a pattern and to singulate the bumps from one another. The resulting contact structure 450 after etching a pattern into the bumps, provides a leaf spring action with independent moving layers 404 , 410 , respectively, as shown in FIG. 5D .
Referring to FIG. 6 , a mask 500 , is cut out of metal, and the pattern is cut out from the mask 500 as a four legged 504 helix pattern 502 . The helix pattern 502 allows light to pass through the cut away portions 510 . The helix pattern 502 includes the four legs 502 having circular pads 508 .
Referring to FIG. 7 , a helical spring contact 610 is shown after fabrication steps wherein the helically shaped contact has been formed. Also shown is a conducting metal baseplate 620 which may be used in some instances to form mechanical anchoring of the helix legs and to electrically connect top and bottom sides of the contact 610 . The baseplate 620 may be used as a conductive element connecting the contact through a via.
Referring to FIGS. 8A and 8B , two LGA helical spring contacts are shown. A right handed helical contact 704 extending in the clockwise direction. A left handed helical contact 708 extending in the counter clockwise direction is shown in FIG. 8B . Referring to FIGS. 8C and 8D , a contact assembly 712 includes a right handed helical contact 704 in minor image relation with a left handed helical contact 708 having a carrier element 716 therebetween. The minor image relation of the right handed and left handed helical contacts 704 , 708 , respectively, or helix reversal, imparts a signal performance enhancement of the contacts at high frequencies.
Referring to FIG. 9 , a plurality of helical contact assemblies 712 (as shown in FIG. 8 ) including right hand and left hand winding directions as described regarding FIG. 8 , are used in a package 800 . The package 800 includes the contact assemblies 812 between upper and lower substrates 804 , 808 , respectively. The package 800 provides helical contact assemblies 812 for high frequency electrical applications.
The present invention achieves a rotational or twisting effect of the helical contacts. This rotation upon compression is desirable to achieve scrubbing through oxide and other thin contaminant layers normally present on electronic contacts. A feature of these helical electrical contact structures is that the direction of helicity reverses as it passes through the central carrier plane, i.e. that the top and bottom helix structures are mirror images with respect to the carrier plane. This preserves the signal integrity of a computer signal at high frequencies by causing significant cancellation of electromagnetic induction.
The advantage of having a rotational scrubbing over typical lateral scrubbing is that as xy dimensions of LGA arrays are decreased, traditional lateral scrubbing increases the chance of the contact moving off the mating contact pad and resulting in an open circuit. Rotational scrubbing of an axiosymmetric contact does not move the contact relative to the position of the mating surface pad, and thus reduces the chances of a contact moving off a mating contact pad.
Additionally, metalization over the initially drawn metal, may include the methods for metalizing including electroplating, electro less plating, physical vapor deposition such as meal evaporation or sputtering, chemical vapor deposition, plasma spray, powder coating, etc. The metalizing could be a single layer or multiple layers of different metals.
In addition, coating with a photo resist, may include electrophoretic or other type of conformal coating method. The extreme z-dimension of LGA contacts complicates photolithography processes in several ways. In order to apply photoresist uniformly, one alternative is to use electrophoretic type photo resists. Electrophoretic resist may be used to provide uniform coverage of photo resist. Other methods of photo resist coating include spraying, spinning and liquid dipping.
3D Masks are used to expose all coated surface with a uniform dose of light using the photo resist coated LGA pre-contacts inserted into form fitting cavities on the underside of a mask. The desired contact pattern is then cut into the top of the mask using a very fine resolution machining technique called wire EDM (electro discharge machining). The LGA precontact protrusions on both sides of a carrier plane are accordingly inserted into masks in a sandwich form. Thus, the part can be illuminated and photo lithographically defined from both sides. 3D masks include a plate of metal where the bottom has machined cavities that are form fitting to the metalized and photo resist coated LGA contact arrays. In practical application the cavities need to be a little bigger in dimension than the coated LGA contacts to account for any fabrication tolerances etc.
The final desired contact pattern is imparted to the mask by cutting or etching light pathways, or slots by wire EDM (wire electrodeposition machining) using very fine cutting wires. Alternatively, slots can be made by laser cutting, chemical etching, plasma etching etc. This slotting is expected to be most practically exercised cutting at right angle to the plane of the mask, i.e., through the z-direction of the mask metal. However, it can be advantageous to cut in a direction at right angles (normal) to the surface of the contact at any given location along the contact. Such normal-to-surface (NTS) slotting allow superior lithographic resolution and superior illumination uniformity.
During photoexposure the entire part and mask sandwich assembly is tilted and rotated to affect as uniform a photoexposure as possible. This is most easily accomplished by moving the assembly with rotation and tilt stages programmed to move through a path optimal for a given contact pattern. Alternatively, the light source can be made to move around the part. Alternatively, the light source can be shaped by holographic and other types of lenses to provide a uniform distribution of light from many directions at once. Once the lithography is completed, the LGA can be removed from the mask sandwich, and lithography steps of developing resist and etching metal into desired pattern are completed.
In an alternative embodiment of the invention, the deep drawing may be initially done with a soft metal like pure copper, and then a second metal such as beryllium is applied to the surfaces of that metal. This multilayer could be heat treated at high temperatures to diffuse one metal into another to form an alloy and quenched or cooled to produce an alloy with the desired microstructure. This sheet, thus formed, would then be used in the process described above regarding FIG. 2A-2F to be joined and lithographically defined into an LGA.
In another embodiment a secondary set of bumps are sacrificial to aid in the alignment before joining two sheets. For the top sheet the secondary bumps may be in the same direction as the main bumps. For the bottom sheet, the secondary bumps may be in the opposite direction as the main bumps. Thus allowing the nesting of secondary bumps of a top sheet into a bottom sheet. These secondary bumps would be placed in areas that would be etched away later in the lithography step.
The present invention thereby, describes deep drawing of high spring constant sheet metals to form array of contours. The metallurgical joining of two structures in a back to back relation with precise alignment. Metalize further with a joining layer if necessary, such as a thin layer of gold. Coating with photo resist, preferably electrophoretic or other type of conformal coating method. Injection mold carrier polymer layer on just one side in between contours. Sandwiching between top and bottom 3D masks of the back to back structures. Photoexposing, and removing LGA from mask to complete lithography.
There are many variations for joining of two metal sheets, bottom to bottom without the intermediate substrate with vias. Such a part could be stabilized by injection molding a plastic sheet on one side only, followed by similar process steps previously described. Any metal to metal bonding technique could be used including electron beam welding, Gold to Gold joining, ultrasonic joining, high pressure joining, laser weld joining, etc. Additionally, there are other ways to form the contoured sheets besides deep drawing. For instance, various constituent pure metals required for an alloy could be deposited in layers upon a sacrificial template that was molded into the exact shape desired in a prior step. The sacrificial template could consist of molded plastic that would burn away cleanly upon heating the entire assembly to high enough temperatures that the metal layers diffuse into one another to form the alloy of interest. An example would be to form a plastic template with an array of bumps of a desired shape, and then to coat copper by electroplating and then beryllium by PVD sputtering. This is heated to 800 deg. C for one or two hours and then cooled at a rate to optimize the formation of desired grain structure to form CuBe spring metal. Once this contoured sheet is thus formed then it can be metallurgically joined as described earlier. As part of that joining operation other metals or materials may be needed to assist, for instance a thin layer of plated or sputtered gold may be necessary.
The present invention describes how sheet metals can be formed by deep drawing using various standard sheet metal forming techniques (for example, with piston driven tool and die at high temperature) to form a uniform array of bumps. The metal is either a hard spring like metal alloy to begin with or is treated in different ways to result in a hard spring
The present invention achieves a rotational or twisting effect of the helical contacts. This rotation upon compression is desirable to achieve scrubbing through oxide and other thin contaminant layers normally present on electronic contacts. A feature of these helical electrical contact structures is that the direction of helicity reverses as it passes through the central carrier plane, i.e. that the top and bottom helix structures are mirror images with respect to the carrier plane. This preserves the signal integrity of a computer signal at high frequencies by causing significant cancellation of electromagnetic induction.
The advantage of having a rotational scrubbing over typical lateral scrubbing is that as xy dimensions of LGA arrays are decreased, traditional lateral scrubbing increases the chance of the contact moving off the mating contact pad and resulting in an open circuit. Rotational scrubbing of an axiosymmetric contact does not move the contact relative to the position of the mating surface pad, and thus reduces the chances of a contact moving off a mating contact pad.
Additionally, metalization over a polymer, may include the methods for metalizing including electroplating, electro less plating, physical vapor deposition such as meal evaporation or sputtering, chemical vapor deposition, plasma spray, powder coating, etc. The metalizing could be a single layer or multiple layers of different metals.
In addition, coating with a photo resist, may include electrophoretic or other type of conformal coating method. The extreme z-dimension of LGA contacts complicates photolithography processes in several ways. In order to photo resist uniformly, one alternative is to use electrophoretic type photo resists. Electrophoretic resist may be used to provide uniform coverage of photo resist. Other methods of photo resist coating include spraying, spinning and liquid dipping.
3D Masks are used to expose all coated surface with a uniform dose of light using the photo resist coated LGA pre-contacts inserted into form fitting cavities on the underside of a mask. The desired contact pattern is then cut into the top of the mask using a very fine resolution machining technique called wire EDM (electro discharge machining). The LGA precontact protrusions on both sides of a carrier plane are accordingly inserted into masks in a sandwich form. Thus, the part can be illuminated and photo lithographically defined from both sides. 3D masks include a plate of metal where the bottom has machined cavities that are form fitting to the metalized and photo resist coated LGA contact arrays. In practical application the cavities need to be a little bigger in dimension than the coated LGA contacts to account for any fabrication tolerances etc.
The final desired contact pattern is imparted to the mask by cutting or etching light pathways, or slots by wire EDM (wire electrodeposition machining) using very fine cutting wires. Alternatively, slots can be made by laser cutting, chemical etching, plasma etching etc. This slotting is expected to be most practically exercised cutting at right angle to the plane of the mask, i.e., through the z-direction of the mask metal. However, it can be advantageous to cut in a direction at right angles (normal) to the surface of the contact at any given location along the contact. Such normal-to-surface (NTS) slotting allow superior lithographic resolution and superior illumination uniformity.
During photoexposure the entire part and mask sandwich assembly is tilted and rotated to affect as uniform a photoexposure as possible. This is most easily accomplished by moving the assembly with rotation and tilt stages programmed to move through a path optimal for a given contact pattern. Alternatively, the light source can be made to move around the part. Alternatively, the light source can be shaped by holographic and other types of lenses to provide a uniform distribution of light from many directions at once. Once the lithography is completed, the LGA can be removed from the mask sandwich, and lithography steps of developing resist and etching metal into desired pattern are completed.
In an alternative embodiment, a process includes depositing constituent metal layers over the sacrificial polymer protrusions. For instance, to make a thin film copper beryllium contact, first electroplating 12.50 μm copper, then sputter (or by alternative methods) deposit 2.5 μm of Beryllium, followed by deposition of a second layer of 12.5 μm copper. This metal deposition would be followed by coating with photo resist (e.g., electrophoretic photo resist) and would be sandwiched into 3D egg carton like mask and exposed to light (e.g., Ultraviolet). The part would then be removed from the mask, the photo resist developed to remove protection from any metal desired to be removed. The unprotected areas of the metal would then be etched away. The part is then heated in an oven at sufficiently high temperatures and long enough period of time for the metals to diffuse together to form the alloy of interest after cooling at appropriate rates to obtain the temper of interest by controlled quenching. In this example, Cu and Be would need temperatures of 850 degrees C. for about an hour to diffuse (see Table 1 below). In the heating process the sacrificial polymer protrusions would have burned away and the remaining photo resist will have burned away (or could be removed chemically after the etching).
While the present invention has been particularly shown and described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that changes in forms and details may be made without departing from the spirit and scope of the present application. It is therefore intended that the present invention not be limited to the exact forms and details described and illustrated herein, but falls within the scope of the appended claims.
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A structure and method for manufacturing the same for manufacturing a contact structure for microelectronics manufacturing including the steps of forming first and second metal sheets to form a plurality of outwardly extending bump each defining a cavity. Symmetrically mating the first and second metal sheets in opposing relation to each other to form upper and lower bumps each defining an enclosure therebetween wherein the mated first and second sheets form a contact structure. Coating the contact structure with an insulating material, and fabricating helix shaped contacts from upper and lower bumps. The helix shaped contacts having first and second portions being in minor image relationship to each other.
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RELATED APPLICATION
This application claims the benefit of and priority to U.S. Provisional Application Ser. No. 61/384,810, filed Sep. 21, 2010, the content of which is incorporated by reference herein in its entirety.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not Applicable.
THE NAMES OF THE PARTIES TO A JOINT RESEARCH AGREEMENT
Not applicable
BACKGROUND OF THE INVENTION
1. Field
The invention relates to sports training devices; and, more particularly, to a device for improving the swing of a player of a particular sport, such as golf.
2. Description of Related Art Including Information Disclosed Under 37 C.F.R. 1.97 and 1.98
Various sports such as golf, tennis, baseball, etc. rely on the swing of the participant for effectiveness in attaining excellence in such sport. This is particularly true for golf and many devices have been suggested over the years for improving one's golf swing. The rigid shaft of a golf club makes it very hard for anyone to learn to swing a golf club as it should be swung. In order to reach maximum club speed, a golfer must apply torque from initiation to impact and keep his hands in a pendulum path.
BRIEF SUMMARY OF THE INVENTION
It is an object of this invention to teach a player, such as a golfer, how to execute a real golf swing.
It is a further object of this invention to carrying out the foregoing object by teaching the player to apply a pulling force (tension) at the grip end of a club or the like to cause a pendulum effect without the use of any other type of force.
These and other objects are preferably carried out by providing a shaft or handle tethered to a weighted member by a flexible cord or the like.
A target is provided having a cushioning member engaged by the weighted member when the latter is swung against and into contact with the target.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
The above-mentioned features and objects of the present disclosure will become more apparent with reference to the following description taken in conjunction with the accompanying drawings wherein like reference numerals denote like elements and in which:
FIG. 1A is an elevational view of a sports training device in accordance with the teachings of the invention;
FIG. 1B is a view similar to FIG. 1A showing the interior of the weighted member in FIG. 1A ;
FIG. 2 is a perspective view of a target used with the device of the invention shown in FIGS. 1A and 1B ;
FIGS. 3 to 5 illustrate the device of the invention used to practice a golf swing using the target of FIG. 2 ;
FIGS. 6 and 7 illustrate the device of the invention used to practice a batting swing;
FIGS. 8 and 9 illustrate the device of the invention used to practice a tennis swing;
FIG. 10 is an elevational view, partly in section, showing another embodiment of the device of FIGS. 1A and 1B ;
FIG. 11 is an elevational view, partly in section, showing a modification of a target in accordance with the teachings of the invention;
FIG. 12 is another modification, partly in section, of a target in accordance with the teachings of the invention;
FIG. 13 is a view of the target of FIG. 12 taken along lines 13 - 13 thereof; and
FIG. 14 is an elevational view of a modification of the weighted member of the embodiment of FIG. 10 .
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIGS. 1A and 1B of the drawing, a sport training device 10 is shown having a handle 11 attached to a weighted member 12 by a tether 13 . Weighted member 13 is filled internally with a cushioning material, such as cotton batting 13 . Tether 13 is attached to a ring 14 integral with weighted member 12 at the top thereof. Tether 13 is a string or cord such as a nylon cord, that is comprised of a plurality of strands of threads braided, twisted or woven together.
As seen in FIG. 2 , and as will be discussed further, a target 15 adapted to be used with device 10 of FIGS. 1A and 1B is shown. Target 15 is comprised of a flat base support plate 16 , of metal or the like, adapted to be placed on a supporting surface. A plurality of holes 17 are provided for securing plate 16 to the supporting surface. However, in some sports, such as golf, a driving mat (not shown) may be provided having a hole therein for receiving pole 18 .
Plate 16 may be disposed under such a mat with pole 18 extending upwardly therefrom. Pole 18 may be comprised of telescoping sections having a release pin 19 disposed in aligned holes in such sections for adjusting the overall height of pole 18 . A strike plate 20 is swingably mounted on pole 18 by a pivot member 21 attached to plate 20 mounted on pole 18 for rotation thereof.
In operation, as seen in FIGS. 3 to 5 , player 22 grasps handle 11 with weighted member 12 adjacent his shoulder ( FIG. 3 ). Player 22 swings device 10 ( FIG. 4 ) with weighted member 12 moving away from the player's shoulder. As seen in FIG. 5 , he swings the weighted member 12 against the face of strike plate 20 . The technique illustrated in FIGS. 3 to 5 will improve one's golf swing.
FIGS. 6 and 7 are similar, but show how device 10 can be used to swing the weighted member 12 against strike plate 20 ( FIG. 7 ) to improve one's batting swing.
FIGS. 8 and 9 illustrate how device 10 can be used to improve one's tennis swing by swinging weighted member 12 about tether 13 from the FIG. 8 to the FIG. 9 position.
FIG. 10 is another embodiment of the invention showing a device 23 having a weighted member 24 attached in any suitable manner by a tether 25 , such as a nylon cord, to a solid ball 26 , such as a golf ball. Note that tether 25 passes through a portion 27 of golf shaft having a golf shaft grip 28 on the outside thereof. Tether 25 is preferable a flexible string or cord made up of plurality of fibers passing through a hole 29 in ball 26 and tied or otherwise secured thereto. Weighted member 24 is also filled with suitable material, such as cotton batting. Ball 26 controls the overall length tether 25 .
Although a strike plate 20 is shown in FIG. 2 , a modification thereof is shown in FIGS. 11 to 13 . Here, plate 16 , similar to plate 16 in FIG. 2 , has a pole 18 , which may also be telescopingly adjustable as in FIG. 2 , but, instead of a rigid metal plate, has a cushioning member 30 which may be filled with a suitable cushioning material such as cotton batting 32 ( FIG. 12 ) mounted on pole 18 . This may be accomplished by providing a hole 31 through member 30 at one end thereof (see FIG. 13 ), pole 18 extending therethrough (also seen in FIG. 14 ).
In the embodiment of FIG. 14 , the cylindrical member 33 demonstrates the true mechanics of tension when it is swung against a target as in FIGS. 3 to 5 . Using the grip or handle 28 of FIG. 10 , one quickly notices how one's nervous system tries to apply leverage. The ball 26 acts as a slip-type retainer or buckle and also displays the feel for the transfer of momentum.
In operation, instead of swinging weighted members 12 , 24 or 33 , against plate 20 , the weighted members 12 , 24 and 33 are swung against cushioning member 30 .
It can be seen that there is apparatus for reactive movements with the application of a pendulum and the relating second pendulum, like walking, throwing, striking, as in most natural movements of human body.
The object of the invention is to provide a group of apparatus for the purpose of identifying the different phases of movements which make up the actions of the different sequences very clear and understood by the nervous system.
Thus, my invention teaches someone how to execute a real golf swing by applying a pulling force (tension) at the grip end to cause a “pendulum effect” without the use of any other type of force. This is accomplished by a golfer or the like applying forces to push his club head in the direction of the target (e.g, a golf ball). A more accurate and powerful impact of the club head with the ball will be accomplished when the golfer allows the club head to free-wheel through the ball.
The foregoing is accomplished by use of a mass attached to a grip by a yielding link, such as a rope. The reality of a swinging pendulum is approached as closely as possible. By becoming more proficient with the yielding link of the invention, one's swing becomes smoother both backward and forward by establishing one's body's fixed axes, swinging one's lead arm in the same way using tension to the fixed axes to power the swing instead of pushing the following arm to the target. The swinger's following bent elbow is close to the swinger's side allowing the swinger's body to supply torque.
The overall length of the device is approximately the length of a mini iron golf club. The user swings the device by gripping handle 11 and swings the weighted member 12 . The swinger's hand also not control the swing; the swinging hands create tension to pull the swinging device 10 through an arc to control one's swing.
As one swings device 10 , the mass or weighted member 12 , 24 or 33 falls against one's back at the swing begins to pull the “yielding link (string or rope 13 ) taut by settling one's lead hip to clear the path. This also makes for the extended stretch of the body just before turning into impact. One's lower body and upper torso turn in unison with the greater moment of inertia of the swinger's extended passive arm and golf club, the lower body will lead the upper body.
It can be seen that angular momentum will cause the passive hands to be pulled in front of one's body, leading the orbiting mass. It is easier to continue a motion than to start one.
Without this move, a wide sweeping ARC will occur at the top of the down swing and the club will release immediately and the large moment of inertia will slow the swing.
The hands are passively being pulled along at the same speed of the rotating upper torso. With one's hands holding on to the handle of the golf club, the club head stays in the orbit. The grip end of the club moves as fast as one's hand; due to inertia, the club head will maintain a 90° angle between the club shaft and the lead arm.
The point that one's hand approaches his following knee, the “pivot” is turned into a “power pivot,” with the muscular action of the mid-upper torso. One's following hand begins to assist the catapulting lead hand to automatically increase the speed of the angular momentum of the club head.
This speed is delivered in the form of a circular path of the catapulting extended arm and not the forces from individual parts of the arm.
Once one's arms and club head are on an in-line orbit to the golf ball, moving like a gyroscope, it will act like a self regulating mechanism.
Any attempt to force the hands forward ahead of orbit impedes the natural are and timing of club head acceleration.
The device herein includes an ‘impact reminder.’ It can be used in one's yard or at the driving range. It can be used to find and feel one's “acceleration zone” and one's “free-wheeling zone.”
Striking of the “impact reminder” is a very important part of one's learning experience.
You can't move properly, perceive properly or predict properly if you can't determine how long events last.
Precision, clarity, and power of what you perceive to represent the exact timing and incredibly controlled sequencing of movement determines one's ability to perform.
Once one's “point of impact”’ is located, you will be able to organize your swing.
Most players feel this cuts their swing in half and they have also heard that they should not hit at the ball.
After a few swings the light goes on and they begin to feel that the golf swing is simpler than ever. Body turn becomes clear and deliberate. A passive arm begins to work.
All of one's efforts to accelerate the club head happens in the ‘acceleration zone.’ It ends before impact.
In order to strike the ball in a downward direction one's hands must be ahead of the club head at impact.
The purpose of a golf swing is to strike the ball and not to make a follow through.
The ‘free-wheeling zone’ starts where the ‘acceleration zone’ ends. Striking the ‘impact reminder’ will automatically stop all of the follow-through.
Any effort to try to accelerate the club head in the ‘free-wheeling zone’ is a waste of effort.
The ‘impact reminder’ will teach someone in a very natural way to release his wrist properly to allow for ‘conservation of angular momentum’ to happen, instead of pushing through that zone.
The acceleration of the upper pendulum will be easier and quicker when you maintains the 90° angle between the lead arm and the golf club due to a smaller moment of inertia.
the faster one swings the more angular velocity obtained for the same torque. The earlier in the down swing the release occurs, an equivalent increase in the braking torque on the arm takes place.
The ‘impact reminder’ will teach one in a very natural way, to deliberately accelerate the club head where it counts.
A golf club is designed to have the club head lead the shaft into impact. You do not push though the ball at impact. Pushing through at impact rearranges the conserved angular momentum that has been created.
As one continues to use the ‘impact reminder,’ you will begin to feel the releasing of momentum through impact as one's hands slow automatically like a self regulating mechanism.
During the down swing momentum is continuously being generated. In a swing ‘free-wheeling’ through impact there is a second half of the down swing, the redistribution of angular momentum towards the club head.
Angular momentum requires a pulling force to keep the momentum on a circular path. The angle at the wrist will automatically straighten at the same rate as the equivalent braking torque on the arm.
Simply catapult one's lead arm against one's upper pectoral muscles, weight posting on the left leg, head and upper body back, following shoulder coming down and through, lead arm fully extended and ‘free-wheel’ through the ball.
Loosening of one's lead hands weakens the forearm and elbow at impact. Steering the club head through impact with the hands going down the target line is a linear deceleration of the club head.
The device disclosed herein may be attached to a ‘golf grip’ which is like the one on one's golf club. Because the grip is attached to a golf club, one uses the grip to control the ‘rigid shaft.’ The ‘mass’ and the ‘yielding link’ will train one to use the grip correctly. All one needs to do is to keep it ‘pointed at the mass,’ throughout the swing.
The force applied to the handle of the golf club propagates down the length of the shaft. The handle moves first and then the part of the club closest to the handle and then a part just a bit further away until the club head moves as well. It is like a wave propagating in a string until the handle stops its forward motion.
In a simple pendulum, maximum speed would be when the shaft is in a straight line. Golf clubs are manufactured to reached maximum speed when the club head is forward of a straight line.
There are many influences on how angular momentum is generated and distributed during the golf swing.
In a swing where one strives to maintain significant acceleration/torque during impact, there will be less redistribution. Only by letting the wave propagating from the handle will redistribution take place.
Only by letting the handle and then the next closest part slow, will the redistribution of angular momentum speed up the furthest point which is the club head.
the golfer using the device herein will eliminate unnecessary moves and allow the alignment of the club head path and direction to become the greater part of the golf-swing.
The target is not an impact bag but rather a “Swing-Through Reminder’ that allows one to feel the ‘free-wheeling’ follow-through of one's golf swing. The user will begin to learn what really happens after striking the ball, the follow through of one's body, arms and club head.
One begins to feel the generation of speed and the precise timing of the whipping through impact, that is released earlier and not at impact.
The whole swing sequence is a continuous motion. The whole swing sequence is a deliberate and well throughout motion.
After impact with the ‘Swing-Through Reminder,’ the strike plate will return to its original position. This will allow one to maintain most of one's structure, since you don't have to bend to replace it. This gives one the opportunity to really use it as a learning tool. Use each swing's feedback as a feed-forward to perfect one's ability to make deliberate movements, until you are able to make every motion deliberately and not a chaotic whim.
Balanced throughout the entire swing allows deliberately delivers speed and accuracy.
Like a professional baseball player who just hit a home run, one can see how balanced he is as the follow through of his swing seem to flow along with his turning body. Sometimes one releases their following hand and allow the lead arm to ‘free-wheel.’
There is no fast abrupt finish, but rather, one where the arms are orbiting at the same speed as the body until the bat's momentum carries the bat beyond the hands.
The device herein is pulled ‘taut’, ‘free-wheeling’ through impact while maintaining this in line set up through follow-through like the home run hitter is at the conclusion of the ‘perfect path of an orbiting mass on a yielding link.’
With one's knees bent and body tilted forward, one makes a back swing using a whole body turn where one's hips are at least 45° and one's shoulder turned 90°.
As device 10 is about to wrap around one's back, you down-swing with your feet, legs and hips, which will begin your shoulder turning and the passive arm will drag the device into orbit.
It is easier to continue a motion than to start one.
One's axis becomes fixed as gravity and one's body orbits one's hand and one's hand pulls the device 10 until one's hand reaches the following leg.
Here you will catapult and speed the swing; i.e., more angular velocity for the same torque and the release occurs with an equivalent increase in the braking torque on the arm.
One's lead arm against your upper pectoral muscle maintains one's structure. One's lead hand will pass the golf ball and the lead shoulder will pull your lead arm away from the ball as your following arm is pulled by your lead hand into the ball.
With your upper body back and posting on your lead leg, you ‘free wheel’ through the golf ball.
All of the work is done in the ‘acceleration zone.’ From there on the ‘momentum of the club’ will be the ‘driving force,’ ‘free-wheeling’ and the ball all the way to a ‘compliant’ finish of the ‘swing.’
While the apparatus and method have been described in terms of what are presently considered to be the most practical and preferred embodiments, it is to be understood that the disclosure need not be limited to the disclosed embodiments. It is intended to cover various modifications and similar arrangements included within the spirit and scope of the claims, the scope of which should be accorded the broadest interpretation so as to encompass all such modifications and similar structures. The present disclosure includes any and all embodiments of the following claims.
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A training device for improving one's swing in a particular sport having a weighted member flexibly tethered to a handle. The handle is gripped swinging the weighted member against a target.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to materials for the manufacture of nonwoven wipers particularly suited for industrial uses. Industrial wipers are currently either reusable cloth, in the form of manufactured wipers or rags, or nonwoven fabric material intended for disposable or limited use applications. The nonwoven material segment of this market has grown due to the economy of such products as well as the ability to tailor the wipers for specific applications. For example, nonwoven wipers are available having absorbency properties particularly suited for oil wiping, for food services wiping, and for wiping of high technology electronic parts. Such nonwoven wiper materials may be manufactured by a number of known processes including wet forming, air forming, and extrusion of thermoplastic fibers. The present invention is related to improvements in nonwoven wipers formed using a meltblowing process to produce microfibers and resulting wipers having utility and diverse applications, particularly where clean wiping properties are essential.
2. Description of the Prior Art
Meltblown nonwoven microfiber wiper materials are known and have been described in a number of U.S. Patents, including 4,328,279 to Meitner and Englebert dated May 4, 1982, U.S. Pat. Nos. 4,298,649 to Meitner dated Nov. 3, 1981, and 4,307,143 to Meitner dated Dec. 22, 1981. The preparation of thermoplastic microfiber webs is also known and described, for example, in Went, Industrial and Engineering Chemistry, Vol. 48, No. 8 (1956) pages 1342 through 1346, as well as in U.S. Pat. Nos. 3,978,185 to Buntin, et al. dated Aug. 31, 1976, 3,795,571 to Prentice dated Mar. 5, 1975, and 3,811,957 to Buntin dated May 21, 1974, for example. These processes generally involve forming a low viscosity thermoplastic polymer melt and extruding filaments into converging air streams which draw the filaments to fine diameters on the average of up to about 10 microns which are collected to form a nonwoven web. The addition of pulp to the air stream to incorporate pulp fibers into the meltblown fiber web is also known and described, for example, in U.S. Pat. No. 4,100,324 to Anderson, Sokolowski, and Ostermeier dated July 11, 1978. The incorporation of staple thermoplastic fibers into meltblown webs is further known and described, for example, in British Published Patent application No. 2,031,039A to Jacques dated Apr. 16, 1980, as well as earlier U.S. Pat. Nos. such as 2,988,469 to Watson dated Jun. 13, 1961 and 3,016,599 to Perry dated Jan. 16, 1962.
While wipers produced in accordance with the disclosures of these patents have, in some cases, achieved good acceptance for a number of wiping applications, it remains desired to produce a nonwoven wiper having extremely good clean wiping properties, i.e., the ability to wipe quickly leaving little or no streaks or residue. In addition, the pulp additive materials tend to be weak and linty and, therefore, unsuitable for many wiping applications. Further, it is desired to produce such a wiper at a cost consistent with disposability and having strength properties for rigorous wiping applications. The wipers of the present invention attain to a high degree these desired attributes and yet further improve the economies of the manufacture of nonwoven disposable wipers.
SUMMARY
The present invention relates to improved nonwoven wipers including thermoplastic microfibers having an average diameter in the range of up to about 10 microns. Further, the invention relates to such improved wipers having not only excellent clean wiping properties for aqueous liquids as well as low and high viscosity oils but also good tactile and physical properties such as strength, all achieved at further economies in the manufacture of such wipers. The wipers of the invention comprise a matrix of microfibers, preferably meltblown thermoplastic fibers having distributed throughout a staple fiber mixture of synthetic fibers and cotton fibers. The mixture or blend is present in an amount of up to about 90% by weight based on the total matrix weight, and the mixture contains up to 90% synthetic fibers based on the total weight of the mixture. Preferred embodiments include microfibers formed from polypropylene and a mixture of fibers including cotton and polyester staple. In a further preferred embodiment, the staple fibers have a denier in the range of up to about 6. Wipers of the invention are demonstrated to possess excellent clean wiping properties as determined by a wiping residual test as well as excellent absorbency for both oil and water as demonstrated by capillary suction tests and oil absorbency rate tests with both low and high viscosity oils. When compared with conventional wipers, wipers of the invention exhibit a unique combination of performance, physical properties, and economy of manufacture.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic view of a process useful to prepare the webs of the present invention;
FIG. 2 is an enlarged view in partial cross section of an unbonded wiper web produced in accordance with the invention;
FIG. 3 is a graph comparing capillary suction results obtained on wipers incorporating a range of stable fiber compositions; and
FIG. 4 is a graph of oil absorbency capacity for different viscosity oils comparing blends of staple fibers of varying proportions.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
While the invention will be described in connection with preferred embodiments, it will be understood that it is not intended to limit the invention to those embodiments. On the contrary, it is intended to cover all alternatives, modifications, and equivalents as may be included within the spirit and scope of the invention as defined by the appended claims.
The invention will be described in reference to certain tests carried out on the material of the invention as well as conventional wipers. These tests were performed as follows:
Tensile results were obtained essentially in accordance with ASTMD-1117-74 . Samples 4" by 6" were prepared with five each having its length in the "machine" and "cross" directions. An Instron machine was used having one jaw face 1" square and the other 1" by 2" or larger with a longer dimension perpendicular to the direction of load. At a crosshead speed of 12" per minute, the full scale load was recorded and multiplied by a factor as follows: readings (pounds): 2, 5, 10, 20, 50; factors (respectively): 0.0048, 0.012, 0.024, 0.048, 0.120. The results were reported in energy (inches/pounds).
Capillary sorption pressure results were obtained essentially as described in Burgeni and Kapur "Capillary Sorbtion Equilibria in Fiber Masses", Textile Research Journal, May 1967, pages 356 through 366. A filter funnel was movably attached to a calibrated vertical post. The funnel was movable and connected to about 8 inches of capillary glass tubing held in a vertical position. A flat, ground 150 milliliter Buchner form fitted glass medium pyrex filter disc having a maximum pore diameter in the range of 10 to 15 microns supported the weighed sample within the funnel. The funnel was filled with Blandol white mineral oil having a specific gravity in the range of 0.845 to 0.860 and 60° F. from Whitco Chemical, Sonneborn Division, and the sample was weighed and placed under 0.5 psi pressure on the filter. After one hour during which the miniscus was maintained constant at a given height, starting at 35 to 45 centimeters, the sample was removed, weighed, and the grams per gram absorbed calculated. The height was adjusted and the process repeated with a new sample until a height of one centimeter was reached. Results were plotted in FIG. 3. In general, the results obtained below 20 centimeters oil indicate oil contained within web voids, and results obtained above 20 centimeters oil are significant as representing oil absorbed within the fibers, themselves, which is a factor in wiper retention.
Bulk was determined using an Ames bulk tester Model 3223 equipped with a long range indicator having 0-100 units with 0.001 inch graduation over a full span of 3 inches. A J50B (Wisconsin Bearing Company) universal joint was attached to the bottom of the vertical weight attachment rod and to the top of a 5 inches by 5 inches platen with total weight of 0.4 lb. ±0.01 lb. Ten 4 inches by 4 inches samples without folds or creases were stacked with the machine direction oriented in the same direction. The platen was centered over the stack and released gently. After 15 to 20 seconds, bulk was read to 0.001 inch, and the average of 5 tests reported.
Water absorption capacity was determined in accordance with Federal Specification UU-T-00595 (GSA-FSS) sections 4.4.4 and 4.4.5 using samples 4 inches by 4 inches.
Water or oil absorption rate was determined as follows: A sample 4 inches by 4 inches was held close to the surface of a distilled water or oil bath at least 4 inches deep maintained at 30° C. ±1° C.; the sample was dropped flat onto the water surface and the time (to the nearest 0.1 sec) measured until the sample was completely wetted. The test was repeated five times and the results averaged.
Water residue was determined as follows: 2 ml. water was placed on the surface to be tested, either stainless steel or nonwettable Formica resting on a top loaded balance and having a surface area 4 in. by 6 in.; a sample 4 in. by 6 in. was attached to a nonabsorbent flat surface above the surface to be tested, and the test surface raised to contact the sample at a pressure of 3 g/cm 2 for 5 seconds. The residue was recorded as the milligrams of water remaining on the test surface as an average of eight tests.
Detergent solution residue was determined in the same manner using a solution of water and 1% by weight Ivory nonionic liquid dishwashing detergent.
Oil residue was determined in the same manner using Blandol oil.
The meltblown fiber component of the matrix of the present invention may be formed from any thermoplastic composition capable of extrusion into microfibers. Examples include polyolefins such as polypropylene and polyethylene, polyesters such as polyethylene terephthalate, polyamides such as nylon, as well as copolymers and blends of these and other thermoplastic polymers. Preferred among these for economy as well as improved wiping properties is polypropylene. The synthetic staple fiber component may also be selected from these thermoplastic materials with polyester being preferred. The cotton component includes staple length cotton fibers. As used herein, "staple length" means fiber average length of 3/8 inch generally in the range of from about 1/4 in. to 3/4 in. and denier from about 1 to 11/2. For economy, the staple fiber mixture of synthetic and cotton fibers is preferably obtained as bulk waste fiber which is available containing generally about 10% to 90% cotton fibers and 90% to 10% polyester fibers. These compositions, it will be recognized, may also contain minor amounts of other fibers and additives which will not adversely affect properties of the resulting wipers.
A process for making the wiper material of the present invention may employ apparatus as generally described in U.S. Pat. No. 4,100,324 to Anderson, Sokolowski and Ostermeier dated July 11, 1978 and, particularly, with respect to FIG. 1 thereof, which is incorporated herein by reference. In particular reference to FIG. 1 hereof, in general, a supply 10 of polymer is fed from an extruder (not shown) to die 16. Air supply means 12 and 14 communicate by channels 18 and 20 to die tip 22 through which is extruded polymer forming fibers 24. Picker 26 receives bulk waste fibers 28 and separates them into individual fibers 30 fed to channel 32 which communicates with air channel 34 and to the die tip 22. These fibers are mixed with meltblown fibers 24 and incorporated into matrix 35 which is compacted on forming drum 36 and directed over feed roll 38 for bonding between patterned roll 40 and anvil roll 42 after which the material may be cut into individual wipers or rolled and stored for later conversion. It will be recognized that, instead of feeding the polyester and cotton fibers as a mixture, the fibers may be fed individually to mix with meltblown fibers 24 at the exit of die tip 22.
The particular bond pattern is preferably selected to impart favorable textile-like tactile properties while providing strength and durability for the intended use. In general, embossing will take place at a pressure in the range of from about 130 pli to about 500 pli, preferably at least 150 pli for 14% bond area. For a different bond area, the preferred pressure may be obtained by multiplying by the ratio of % areas to maintain constant p.s.i. on an individual bond point. The temperature will generally be in the range of from about 180° F. to 325° F. and preferably about 260° F. where the meltblown fibers are polypropylene and the synthetic fibers are polyester, for example. The bond pattern will preferably result in individual embossments over 5% to 30% of the material surface with individual bonds in the range of from about 20 to 200 bonds/in 2 .
When rapid fiber quenching is desired, the filaments 24 may be treated by spray nozzle 44, for example, during manufacture. The material may be treated for water wettability with a surfactant as desired. Numerous useful surfactants are known and include, for example, anionic and ionic compositions described in U.S. Pat. No. 4,307,143 to Meitner issued Dec. 22, 1981. For most applications requiring water wettability, the surfactant will be added at a rate of about 0.15% to 1.0% by weight on the wiper after drying.
Turning to the schematic illustration in FIG. 2, an embodiment of the wiper material of the present invention will be described. As shown prior to embossing for purposes of clarity, wiper 46 is formed from a generally uniform mixture of microfibers 48 with staple cotton fibers 50 and staple polyester fibers 52. While it is not desired to limit the invention to any specific theory, it is believed that the improved performance is obtained by the staple polyester and staple cotton fibers separating the fine microfibers and producing voids for absorption of liquids. Furthermore, the nature of the cotton fibers is believed to contribute to improved texture, wettability and clean wiping properties. Depending upon the particular properties desired for the wiper, the percentage of staple cotton fibers in the mixture with polyester staple may vary in the range of up to about 90% by weight with the range of from about 30% to 70% by weight preferred. This mixture may be added to the microfibers in an amount within the range of up to about 90% mixture by weight with the range of from about 40% to 80% preferred. In general, the greater the amount of the staple synthetic and staple cotton fiber mixture added, the more improved will be the clean wiping capacity properties.
The total basis weight will also vary depending upon the desired wiper application but will normally be in the range of from about 25 to 300 grams per square meter and, preferably, in the range of from about 65 to 150 grams per square meter.
EXAMPLES
The invention will now be described with reference to specific examples.
EXAMPLE 1
Using apparatus assembled generally as described in FIG. 1 having a picker setting of feed roll to nose bar clearance of 0.003 in., nosebar to picker distance of 0.008 in. and picker speed of 320 RPM, polypropylene was extruded at barrel pressure of 200-350 PSIG at a temperature of about 640° F. to 760° F. to form microfibers with primary air at about 630° F. to 715° F. at a fiber production rate of 1.2 to 2.3 PIH. To these microfibers in the attenuating air stream was added about 50% by weight of a mixture of staple polyester fibers and cotton fibers (Product No. A1122 Leigh Textiles, nominally a 50/50 weight % mixture) at a rate of 1.2 to 2.3 PIH. The resulting matrix was bonded by heat and pressure conditions of 260° F. and 20 psi in a pattern covering about 14% of the surface area with about 140 bonds per square inch. The material had a basis weight of 95.95 grams per square yard and a bulk of 0.054 inch. It was soft and conformable and had excellent tactile properties.
EXAMPLE 2
Example 1 was repeated except that yellow pigment (Ampaset 43351) was added at about 0.7% by weight. The resulting material had a basis weight of 102.33 grams per square yard and a bulk of 0.045 inch.
EXAMPLE 3
For comparison, Example 1 was repeated except that the mixture of cotton and staple fibers was replaced with a supply of pulp fibers. The resulting material had a basis weight of 81.98 grams per square yard and a bulk of 0.056 inch. Example 3A is a similar sample of two layers of about 1.5 oz/yd 2 of a mixture of pulp and meltblown polypropylene fibers, one layer on each side of an about 0.4 oz./yd 2 reinforcing spunbonded polypropylene layer.
EXAMPLE 4
Also for comparison, Example 1 was repeated without the addition of fibers to produce a pure meltblown polypropylene web. This material had a basis weight of 89.41 grams per square yard and a bulk of 0.032 inch.
EXAMPLES 5 THROUGH 8
Example 1 was repeated except that a fiber blend (nominally 50/50 weight %) designated A141M was used and the ratio of staple mixture to meltblown microfibers was varied as follows: 30/70, 40/60, 50/50, and 60/40.
EXAMPLES 9 THROUGH 11
Example 1 was repeated except that the denier of the polyester in the staple cotton fiber mixture was varied from 15, to 6, to 3 denier.
The materials of Examples 1 through 11 were tested for wiping and certain physical properties and are reported in the Table I which follows. For comparison tests were also made of a wiper containing staple fibers only added to meltblown. microfibers (Example 12), standard shop towels (Example 13), terrycloth bar towels (Example 14), paper wipers (Example 15), spunbonded material alone (Example 16), heavier basis weight meltblown material alone (Example 17), spunbonded/meltblown/spunbonded laminate wiper material (Example 18), a laminate of Example 3 material between two spunbonded layers (Example 19), polyester wiper material (Example 20) and carded web wipers (Example 21).
FIG. 3 demonstrates by capillary suction curves that the wiper materials of the present invention exhibit properties unexpected considering the curves for the individual components separately tested. Thus, the oil absorbed is much higher for the materials of the present invention except at the lowest oil pressures.
Turning to FIG. 4, it can be seen that oil capacity increases with increasing amounts of staple fiber and values of at least about 500% are readily obtained. The materials tested contained 60%, 50% and 40% staple mixture by weight based on the combined weight and basis weights of 108.69, 116.44 and 89.71 g/m 2 , respectively. They were tested with 10, 30 and 80 W motor oil.
TABLE I__________________________________________________________________________ EXAMPLE 1 2 3 3A 4 5 6 7 8 9 10 11__________________________________________________________________________TESTWater AbsorbtionCapacity (%) 793 560 972 751 435 534 520 591 648 631 638 675Rate (Seconds) 1.99 1.07 1.10 1.16 3.40Oil AbsorbtionCapacity (%) 677 506 810 618 414 405 500 530 565 596 527 547Rate (Seconds) 3.99 7.37 2.73 3.19 18.87Dry Water Residue: (mg)1 Layer - Formica 65 9 75 33 1131 Layer - St. Steel 45 14 69 25 774 Layer - Formica 22 4 16 12 14 Layer - St. Steel 3 1 24 8 2Wet Sample WaterResidue: (mg)1 Layer - Formica 12 69 21 14 5831 Layer - St. Steel 12 97 3 27 4934 Layer - Formica 4 0 12 0 254 Layer - St. Steel 3 1 3 0 131% Ivory SolutionResidue: (mg)1 Layer 62 261 471 345 251 316 470 251 1784 LayerOil Residue: (mg)1 Layer 55 48 1304 Layer 33 45Basis Wt. (g/m.sup.2) 96.0 122.4 98.3 124.2 106.9 106.9 114.8 112.8 100.2 115.5 105.3 99.2Tensile Strength (g) 1022 4490 3538 3265 2950Thickness (cm) 0.137 0.114 0.142 0.081 0.005 0.005 0.005Bulk Density g/cm.sup.3 7.004 10.736 6.905 13.0__________________________________________________________________________ EXAMPLE 12 13 14 15 16 17 18 19 20 21__________________________________________________________________________TESTWater AbsorbtionCapacity (%) 243 272 412 782 396 422 642 593Rate (Seconds) 00 0.64 0.80 25.10 1.41 49.52Oil AbsorbtionCapacity (%) 1571 289 300 563 357 362 512 342Rate (Seconds) 3.10 11.53 1.05 4.19 17.30 22.15 4.21 44.30Dry Water Residue: (mg)1 Layer - Formica 1895 1643 0 6 1750 429 36 1153 2091 Layer - St. Steel 1852 1579 0 1 510 69 692 1534 Layer - Formica 1895 1643 0 1 1750 380 12 691 174 Layer - St. Steel 1852 1579 0 0 16 25 515 62Wet Sample WaterResidue: (mg)1 Layer - Formica 1216 733 2 149 651 50 335 471 Layer - St. Steel 774 1020 64 167 1111 803 42 210 214 Layer - Formica 1235 44 0 4 128 0 4 54 Layer - St. Steel 708 30 0 3 734 265 0 1 01% Ivory SolutionResidue: (mg)1 Layer 207 13 949 269 548 564 Layer 25 202 7 39 9Oil Residue: (mg)1 Layer 80 250 534 Layer 61 41Basis Wt. (g/m.sup.2) 69.5 180.5 378.9 87.7 62.2 120.0 89.2 126.3 44.1__________________________________________________________________________
To demonstrate improved oil absorbtion rates obtainable in accordance with the present invention, tests were performed on materials having varying proportions of blend and microfiber components and using various weight or viscosity oils. The results are shown in the following Table II and illustrate that in all but one case the rate improved with increasing blend addition and the improvement was even more significant with the higher weight oils.
TABLE II______________________________________Oil Absorption Rate (Sec.) Motor Oil Grade (SAE)Blend/Meltblown 10 20 50 85______________________________________40/60 3.55 3.59 11.86 28.3350/50 2.61 3.18 8.17 20.7460/40 2.67 2.32 8.07 16.21______________________________________
As is demonstrated by the above examples, the wiper material of the present invention provides a unique combination of excellent wiping properties for different liquids including oils of various viscosities with strength and appearance contributing to an improved wiper at substantial economies resulting from the ability to incorporate reprocessed fibers containing cotton and polyester. It is thus apparent that there has been provided, in accordance with the invention, a wipe material that fully satisfies the objects, aims and advantages set forth above. While the invention has been described in conjunction with the specific embodiments thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, it is intended to embrace all such alternatives, modifications and variations as fall within the spirit and broad scope of the appended claims.
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Wiper comprising a matrix of nonwoven fibers having a basis weight generally in the range of from about 25 to 300 gsm and including a meltblown web having incorporated therein a staple fiber mixture including synthetic and cotton fibers. The combination provides highly improved wiping properties as well as strength and absorbency for many industrial applications requiring wiping of oily and/or aqueous materials. The wipers may be formed by a conventional meltblowing process involving extrusion of a thermoplastic polymer as filaments into airstreams which draw and attenuate the filaments into fine fibers having an average diameter of up to about 10 microns. The staple fiber mixture of synthetic and cotton fibers may be added to the airstream, and the turbulence produced where the airstreams meet results in uniform integration of the staple fiber mixture into the meltblown web. The matrix may contain up to 90% by weight of the synthetic and cotton fiber blend, which, itself, may contain up to about 90% by weight of the synthetic fibers.
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[0001] The present application claims the benefit of the priority filing date of provisional patent application No. 60/200,015, filed Apr. 27, 2000.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] This invention relates to a method and devices using the method for measuring incident gamma-ray energy and direction. More particularly, the invention relates to measuring energy losses and positions of two Compton scatter interactions followed by a measurement of the position of a third Compton scatter or photoelectric interaction to determine the incident gamma-ray energy and direction cone without the necessity for absorbing the full energy of the incident gamma ray.
[0004] 2. Description of the Related Art
[0005] Gamma ray imaging and detection is used in many scientific and commercial applications, including medical imaging, nuclear spectroscopy, and gamma ray astronomy.
[0006] One application that makes use of gamma ray imaging is gamma ray astronomy. In the conventional approach two position-sensitive detector arrays are used. The first array uses low-Z scintillation detectors and the second array, separated some distance from the first, uses high-Z scintillation detectors. Gamma rays incident on the first detector array undergo Compton scattering, and the Compton scattered gamma rays must be fully absorbed in the second detector array in order to estimate the energy and direction of the initial gamma ray. This approach has several limitations, including low efficiency, poor energy resolution and poor angular (imaging) resolution.
[0007] Alternative concepts to improve on these limitations have been proposed or undertaken that use detectors with improved position and/or energy resolution. However, in all of these approaches the fill energy of the initial gamma ray must be absorbed in order to determine the energy and direction of the incident gamma ray.
[0008] Another application is medical imaging using positron emission tomography (PET). In PET, a radio-pharmaceutical positron emitter is administered to a patient. In some PET applications, the radio-pharmaceutical is selected for its ability to preferentially concentrate in a desired tissue, e.g. a tumor. In other applications, the biological uptake or distribution of the radio-pharmaceutical is used to study organ function (e.g. brain or heart). In these applications, PET applies the mechanism whereby the positrons from the radio-pharmaceutical annihilate with electrons to create two annihilation gamma rays, each having an energy of 511 keV, that are emitted in opposite directions at an angle of almost exactly 180 degrees. The gamma rays are detected with position-sensitive detectors and the location of the detections determines a line on which the radioactive decay is located. Multiple events allow a more precise, 3-dimensional determination of the location of the concentration of radio-pharmaceutical and thus the location/morphology of the tumor or the function of the organ of interest. Typically, two identical detectors, each a combination of scintillators and photomultiplier tubes, are required for PET. This instrumentation, however, provides only moderate energy resolution and position resolution capabilities.
[0009] Another application is single photon emission computed tomography (SPECT). In SPECT, an injected radio-pharmaceutical emits a single gamma ray per radioactive decay. The direction of the emitted gamma ray is determined by using a collimator in conjunction with a position-sensitive scintillator-photomultiplier detector. The collimator only allows gamma rays from a single direction to reach the detector. This provides a two-dimensional view of the radioactivity. By moving the detector/collimator assembly to view the region-of-interest from many directions, or using multiple collimators and/or detectors, a three dimensional image can be reconstructed. The disadvantage of this technique is that the sharpest images are generated by collimators with narrow apertures. This is very inefficient and hence requires large doses or long collection times.
[0010] An application similar to SPECT is planar imaging, which is the traditional form of medical gamma ray imaging, in which a patient is injected with a radio-pharmaceutical as in SPECT but in which the collimator and detector are planar and are not rotated around the patient. The disadvantage is that the image generated is then a 2-dimensional projection rather than a 3-dimensional image of the radiation distribution.
[0011] In order to address the disadvantages of the current imaging systems, several concepts have been implemented or proposed that use the Compton scattering process. In Compton scattering, an initial gamma ray scatters off an electron in a position-sensitive detector and the Compton scattered gamma ray, reduced in energy, is detected by a second position-sensitive detector. The angle of scatter is determined from knowledge of the energy loss at the first and second detectors, where it is required that the full energy of the Compton scattered gamma ray is deposited in the second detector. With this information, the direction of the initial gamma ray is restricted to a cone whose axis is the line joining the two interaction sites and whose opening angle is twice the Compton scatter angle. This technique, for example, was the basis for a scintillation-detector imaging gamma ray instrument that was flown on a NASA mission to image the gamma ray sky. That instrument used low-Z and high-Z detectors for the first Compton scatter detector and the second full absorption detector, respectively. Significant disadvantages of this approach are poor detection efficiency and poor imaging resolution, the latter due to the poor energy resolution of the scintillation detectors.
[0012] Another proposed concept for an improved Compton imaging detector employs multiple Compton scattering in arrays of position-sensitive silicon detectors. In this approach, the initial gamma ray undergoes several Compton scatters in the silicon detector array, with the initial gamma ray energy either fully absorbed in the silicon array, or the gamma ray escaping the silicon array being absorbed in a scintillation detector surrounding the silicon array. Knowledge of the full energy loss is used, along with the energy losses and positions of the first two interactions to determine the Compton scatter angle at the first interaction site. The most probable interaction sequence for the Compton scatter events is determined from the consistency of the energy losses and scattering angles with the known physics of the Compton scattering process. An alternative to this technique recognizes that the full energy of the incident gamma ray need not be fully absorbed, and proposes that if the interaction order for four Compton scatters and the initial gamma-ray energy are unknown, the initial gamma ray energy and direction can still be deduced.
[0013] Another Compton imaging approach employs the use of position-sensitive gas or liquid detectors. A low-Z material (e.g. argon) is used for the Compton scatter detector while a high-Z material (e.g. xenon) is used to absorb the Compton scattered gamma ray. Disadvantages of this concept are the poor energy resolution of gas and liquid detectors relative to solid-state detectors, the low interaction efficiency in gas detectors compared to solid-state detectors, and the associated limitation to low-energy gamma-rays.
[0014] There is, therefore, a need for a gamma ray imaging device having improved imaging, improved detection efficiencies, better energy resolution, and capable of extending gamma-ray imaging capabilities to higher gamma-ray energies.
SUMMARY OF THE INVENTION
[0015] According to the invention, a device for determining the photon energy E 1 and direction cone angle of incident gamma ray with two Compton scattering interactions and one subsequent interaction includes a first radiation detector for receiving an incident gamma ray having an unknown photon energy E 1 and an unknown direction cone angle, for scattering a photon energy E 2 in a first Compton scattering interaction at a first scatter angle θ 1 , and for providing a first output corresponding to the first Compton scattering interaction; a second radiation detector for receiving photon energy E 2 and scattering some photon energy E 3 in a second Compton scattering interaction at a second scatter angle θ 2 , and for providing a second output corresponding to the second Compton scattering interaction; a third radiation detector for receiving photon energy E 3 , and interacting with photon energy E 3 in a third interaction, and for providing a third output corresponding to the third interaction; and a processor for receiving and processing the first, second, and third outputs and for calculating the photon energy E 1 and direction cone angle of the incident gamma ray based on the outputs. The first, second, and third radiation detectors are sensitive to the position and energy of incident gamma ray, e.g. by virtue of being in a three-dimensional array providing a very accurate determination of the position of a scattering or other event. The device and processor include the capability to calculate the photon energy E 1 and direction cone angle of the incident gamma ray without the necessity for the absorption and measurement of the entire or substantially all of the energy E 1 in the detector. The detector also preferably includes the processor being programmed to reject a selected detection event, e.g. in an algorithm that also calculates the respective energy losses L 1 , L 2 , and L 3 in the first, second, and third radiation detectors.
[0016] The invention also includes a method for determining the photon energy E 1 and direction cone angle of incident gamma ray with two Compton scattering interactions and one subsequent interaction, comprising the steps of receiving an incident gamma ray having an unknown photon energy E 1 and an unknown direction cone angle, for scattering a photon energy E 2 in a first Compton scattering interaction at a first scatter angle θ 1 , and providing a first output corresponding to the first Compton scattering interaction; receiving photon energy E 2 and scattering some photon energy E 3 in a second Compton scattering interaction at a second scatter angle θ 2 , and providing a second output corresponding to the second Compton scattering interaction; receiving photon energy E 3 , and interacting with photon energy E 3 in a third interaction, and providing a third output corresponding to the third interaction; and processing the first, second, and third outputs and calculating the photon energy E 1 and direction cone angle of the incident gamma ray based on the outputs, without necessarily absorbing and measuring the entire or substantially all of the energy E 1 .
[0017] The invention provides substantially improved efficiency and imaging resolution compared to current systems.
[0018] The invention further provides a system that produces gamma-ray images having improved spectral resolution.
[0019] The invention is useful in military applications, for example for the location of fissile materials or for the location and identification of radioactive waste materials. The system and method also has non-military applications, for example in nuclear medical imaging and non-destructive testing, to name but a few.
[0020] The invention may have specific application in certain nuclear medical imaging applications, such as that described in pending U.S. patent application No. ______ filed on ______ , entitled “Coincident Multiple Compton Scatter Nuclear Medical Imager”.
[0021] Additional features and advantages of the present invention will be set forth in, or be apparent from, the detailed description of preferred embodiments which follows.
BRIEF DESCRIPTION OF THE DRAWINGS
[0022] [0022]FIG. 1 is a diagram illustration of the Compton scatter process.
[0023] [0023]FIG. 2 is a diagram of an embodiment illustrating the use of a monolithic position-sensitive detector system according to the invention.
[0024] [0024]FIG. 3 is a cross sectional view of a Compton imaging instrument illustrating the use of arrays of position-sensitive solid-state detectors according to the invention.
[0025] [0025]FIG. 4 illustrates the multiple Compton scattering process and detection scheme according to the invention.
[0026] [0026]FIG. 5 shows an array of three position-sensitive solid-state strip detectors (germanium) applicable to the invention.
[0027] [0027]FIG. 6 is an illustration of using relative timing of anode and cathode signals in a germanium strip detector to achieve 3-dimensional positioning. The x-y position is derived from the orthogonal strips that receive the signals, and can determine positions to the strip pitch that may be less than 1 mm. The z-dimension is derived from the signal arrival times and can be determined to less that 0.5 mm.
[0028] [0028]FIG. 7 illustrates the several components of the uncertainty in the Compton scatter angle including those due to energy resolution, position resolution, and Doppler broadening.
[0029] [0029]FIG. 8 shows a depiction of the direction cone illustrating factors leading to its calculation and determination, including the uncertainty in the Compton scatter angle.
DETAILED DESCRIPTION
[0030] The invention makes use of the Compton scattering of gamma rays. Referring to FIG. 1, a gamma ray 52 is incident on a detector 50 in which the gamma ray undergoes a Compton scatter interaction at location 53 . The detector 50 is such that both the location 53 and the energy loss to a Compton scattered electron can be precisely determined. The Compton scattered gamma ray 62 undergoes a photoelectric (full-energy) interaction at location 63 in a second detector 60 such that the location 63 and the energy loss at location 63 can be precisely determined. It is well known to those skilled in the art that the scatter angle θ 1 is uniquely determined by the energy losses at locations 53 and 63 under the assumption that the initial momentum of the Compton scattered electron is zero. The angle of scattering is given by:
cos ϑ 1 = 1 - m c 2 ( 1 E 2 - 1 E 1 ) ( 1 )
[0031] where E 2 is the energy of the scattered gamma ray (and the energy deposited at location 63 ) and E 1 is the energy of the incident gamma ray (and also the sum of the energy losses at locations 53 and 63 ).
[0032] Referring now to FIG. 2, a gamma ray detection system 10 includes detector 12 , which comprises a device capable of interacting with and scattering an incident gamma ray 14 while providing an output 16 to processor 15 from each scattering event as will be further explained below. Detector 12 may comprise a position-sensitive solid-state detector or a position-sensitive gaseous detector or a position-sensitive liquid-filled detector. The solid-state detector could be one of a number of solid state detector materials as are described further below.
[0033] Gamma ray 14 is scattered in detector 12 in a first Compton-scattering interaction at a first location 18 . First Compton-scattered gamma ray 24 interacts in a second Compton-scattering event at a second location 28 to produce a second Compton-scattered gamma ray 34 . Gamma ray 34 may interact in a third Compton-scattering event or may undergo a photoelectric interaction at a third location 38 . In the event that gamma ray 34 interacts through a third scattering event at location 38 , a third Compton-scattered gamma ray is produced which can exit the detector 12 . The output data 16 , i.e. the location and energy deposited from each scattering event in detector 12 , is input to a processor 15 . Processor 15 includes a program for calculating, based on the energy losses at locations 18 and 28 and the angle of scattering at location 28 determined from the locations 18 , 28 , and 38 , the direction cone and energy of the incident gamma ray 14 as is described below. The processor outputs this data to display unit 25 which can display, among other information, the incident direction cone of each gamma ray, a two-dimensional map representing the gamma ray sources in the field, and the energy spectra of sources in selected regions in the map.
[0034] Referring now to FIG. 3, in another embodiment of the invention, a gamma ray detection system 200 includes a detector array 210 that comprises a plurality of individual detector layers 212 each of which serves as a position-sensitive solid-state detector. Each layer 212 of array 210 comprises a material able to interact with an incoming gamma ray 232 by Compton scattering and by additional interaction mechanisms as are well known in the art. Useful materials for layers of 210 that exhibit good spectral resolution include germanium, silicon, CZT, CdTe, and GaAs, although other semi-conductor detectors known to provide acceptable spectral resolution are also within the scope of the invention. Silicon is a preferred material, as it combines highest relative probability of Compton scattering over a broad range of energies and can be used at near-room temperatures, unlike germanium-based prior art Compton detectors that are cryogenically cooled for acceptable performance.
[0035] Gamma ray 232 is Compton-scattered in a first interaction layer 230 at location 238 . First Compton-scattered gamma ray 242 is then Compton-scattered in a second layer 240 at location 248 . Second Compton-scattered gamma ray 252 is then Compton-scattered in a third layer 250 at location 258 or may be absorbed by a photoelectric interaction at location 258 . If second Compton-scattered gamma ray 252 is Compton-scattered at location 258 , then a third Compton scattered gamma ray 262 is produced that may exit the detector array 210 . Since the detectors in each layer are position-sensitive, it is understood by those skilled in the art that two interactions may occur in the same layer. The output data 216 (the location and energy deposited from each interaction event) of detector array 210 is input to a processor 215 . Processor 215 as in the case of processor 15 includes the program for calculating the direction cone and energy of the incident gamma ray 232 (described below). The processor outputs this data to display unit 225 which as before can display the incident direction cone of each gamma ray, a two-dimensional map, and the energy spectra of sources in selected regions in the map. For each interaction, the processor processes the electronic signals from the detector to determine the energy deposited at each interaction site and the x, y, and z coordinates for each energy loss.
[0036] We now show that the energy and direction angle of a gamma ray can be determined from only the partial energy loss at the first three interaction sites if the first two interactions are Compton scatters. Referring to FIG. 4, consider the two successive Compton scatter interactions followed by a third interaction. An initial gamma ray 132 with energy E 1 , is incident on a detector array 100 which has good position resolution and good energy resolution. Gamma ray 132 interacts by a Compton scatter interaction in position-sensitive detector 110 at position 133 . First Compton scattered gamma ray 142 leaves position 133 at an angle θ 1 relative to the direction of the initial gamma ray 132 , and interacts in position-sensitive detector 120 at position 143 . Second Compton scattered gamma ray 152 leaves position 143 at an angle θ 2 relative to the direction of the first Compton scattered gamma ray 142 and interacts in position-sensitive detector 130 at position 153 . The interaction at position 153 can be a Compton scatter interaction producing third Compton scattered gamma ray 162 or a photoelectric interaction. Only the position in detector 130 is required. The energy losses (to the scattered electrons) at positions 133 and 143 are L 1 , and L 2 , respectively.
[0037] The Compton scattering formulae for the two interactions at positions 133 and 143 are:
cos ϑ 1 = 1 - m c 2 ( 1 E 2 - 1 E 1 ) ( 2 ) cos ϑ 2 = 1 - m c 2 ( 1 E 3 - 1 E 2 ) ( 3 )
[0038] where mc 2 is the rest mass of the electron, and the energies of the scattered electrons are:
(4) L 1 =E 1 −E 2
(5) L 2 =E 2 −E 3
[0039] Solving eq. (5) for E 3 and substituting into (3) yields an equation with E 2 as the only unknown, since θ 2 is determined from the locations of the three interactions sites 133 , 143 and 153 . This quadratic equation can be solved for the energy E 2 , and is given by:
E 2 = L 2 2 + 1 2 [ L 2 2 + 4 m c 2 L 2 1 - cos ϑ 2 ] 1 2 ( 6 )
[0040] Therefore the incident gamma ray energy, E 1 is also determined from (4), and is:
E 1 = E 2 + L 1 = L 1 + L 2 2 + 1 2 [ L 2 2 + 4 m c 2 L 2 1 - cos ϑ 2 ] 1 2 ( 7 )
[0041] Now having E 1 and E 2 , the scatter angle at the first interaction site and hence the direction cone for the initial gamma ray can be determined from equation (2). It is clear that determination of the correct energy and direction cone of the incident gamma ray requires that the correct sequence of interactions is known. This is accomplished through a procedure of testing the several possible interaction sequences and testing whether the Compton scatter interactions for each sequence is consistent with the kinematic relations for Compton scattering at each interaction site. In undertaking these tests, the probabilities for gamma rays of the inferred energies for each test sequence to travel from the nth interaction site to the (n+1)st interaction site through the required material can also be used to optimize the probability for obtaining the correct interaction sequence. This procedure is known to those skilled in the art and, for example, is described in U.S. Pat. No. 4,857,737, which is herein incorporated by reference.
[0042] The uncertainties in E 1 and θ 1 can also be determined. The uncertainty in E 1 , dE 1 , is given by:
dE 1 = [ ( ∂ E 1 ∂ L 1 d L 1 ) 2 + ( ∂ E ∂ L 2 d L 2 ) 2 + ( ∂ E 1 ∂ ϑ 2 d ϑ 2 ) 2 ] 1 2 ( 8 )
[0043] where dL 1 and dL 2 are the uncertainties in the energy depositions at interaction sites 133 and 143 , and dθ 2 is the uncertainty in the scattering angle at site 153 determined from the typical positional errors in the detector.
[0044] The position-sensitive device 200 illustrated in FIG. 3 indicates one possible implementation of a gamma ray detection system 210 that provides both excellent spectral resolution and excellent spatial resolution. Each of the several layers of the detector, exemplified by layers 230 , 240 and 250 could consist of arrays of position-sensitive solid-state detectors. Referring to FIG. 5, an array 500 of three germanium strip detectors, 510 , 520 and 530 is shown which are examples of the type of detectors that can be used to populate a detector device. Each of the strip detectors has an active area of 50 mm×50 mm and is 10 mm thick. The detectors have 25 orthogonal electrical contact strips on opposite sides of the planar faces as indicated by the strip 525 . The pitch of the strips is 2 mm. One skilled in the art will know that when a gamma ray interacts by Compton scattering or photoelectric interaction in the active detector volume, electron-hole pairs are created. Under an applied electric field, the electrons drift toward one planar face and the holes drift toward the opposite face. The collection of the holes and electrons produce signals on a strip on each side of the detector. The location of the interaction in the planar dimension is determined by the intersection of the two strips that record the signals. For the devices shown, this location is determined to 2 mm accuracy in the x and y directions. Those skilled in the art will know that use of finer strip pitch enables position information in the x and y directions to be less than 1 mm.
[0045] Excellent position resolution can also be achieved in the direction perpendicular to the x-y planar surfaces. This is achieved by measuring the relative arrival times of the electron and hole signals at the two strip surfaces. Referring to FIG. 6 a, the orthogonal strips are shown schematically on opposite surfaces of a germanium strip detector. FIG. 6 b shows the electron signal 615 acquired on strip 610 on the front face and the hole signal 625 acquired by the strip 620 on the back face of the detector for an interaction that occurs very near the front surface. It is understood by those skilled in the art that the rise time of the signal 615 precedes the rise of the signal 625 by about 100 nanoseconds. FIG. 6 c shows the comparable signals 616 and 626 for an interaction that occurs near the back face of the detector. In this case the hole signal 626 arriving at strip 620 precedes the electron signal 616 arriving at strip 610 by about 100 nanoseconds. The total difference in the relative arrival times is about 200 nanoseconds. With an intrinsic resolving time of 10-20 nanoseconds, it is clear that the location of the interaction can be determined to less than 1 mm in the direction perpendicular to the strip faces of the detector. Combined with the x-y positions measured with the strip signals, the location of the interaction is measured to 1 mm or better in 3 dimensions. The uncertainty dθ 2 is derived from the location uncertainties at the first three interaction sites.
[0046] Next, proceeding with equation (8) and evaluating the partial differential terms using equation (7), we obtain:
dE 1 = [ d L 1 2 + ( 1 2 + 1 4 [ L 2 2 + 4 m c 2 L 2 ( 1 - cos ϑ 2 ) ] - 1 2 [ 2 L 2 + 4 m c 2 ( 1 - cos ϑ 2 ) ] ) 2 d L 2 2 + ( sin ϑ 2 4 [ L 2 2 + 4 m c 2 L 2 ( 1 - cos ϑ 2 ) ] - 1 2 [ 4 m c 2 L 2 ( 1 - cos ϑ 2 ) 2 ] ) 2 d ϑ 2 2 ] 1 2 ( 9 )
[0047] The error in θ 1 can also be determined. From (2) we have:
cos ϑ 1 = 1 - m c 2 E 2 + m c 2 E 1 = 1 - m c 2 E 1 - L 1 + m c 2 E 1 ( 10 ) d cos ϑ 1 = [ ( ∂ cos ϑ 1 ∂ E 1 dE 1 ) 2 + ( ∂ cos ϑ 1 ∂ L 1 d L 1 ) 2 ] 1 2 then: ( 11 ) d ϑ 1 = m c 2 sin ϑ 1 [ ( 1 ( E 1 - L 1 ) 2 - 1 E 1 2 ) 2 dE 1 2 + d L 1 2 ( E 1 - L 1 ) 4 ] 1 2 ( 12 )
[0048] This uncertainty in the scattering angle at the first interaction site is due only to the uncertainty in the incident energy and the uncertainty in the energy loss in detector 110 . In addition, there is an error associated with the uncertainties in the locations of the interactions at the three interaction sites. There is also an error associated with the initial momentum of the electron at position 133 . This is assumed to be zero in the standard Compton formula derivation. Including the motion of the electron adds another uncertainty, commonly referred to as a Doppler broadening uncertainty and familiar to those skilled in the art. FIG. 7 shows the several components of the angular uncertainty as a function of Compton scatter angle for a 1 MeV incident gamma ray. These components include uncertainties due to the detector energy resolution 710 , the detector position resolution 720 and the Doppler broadening 730 .
[0049] The overall uncertainty in the direction of the incident gamma ray is given by the root-mean-square (RMS) sum of the three components 710 , 720 and 730 due to the finite energy resolution of the detectors, the finite position resolution of the detectors and the Doppler broadening, respectively. This is given by:
(13) dθ 1 2 ( total )= dθ 1 2 ( energy )+ dθ 1 2 ( geometric )+ dθ 1 2 ( Doppler )
[0050] [0050]FIG. 7 shows these uncertainties for the energy resolution 710 , the geometric resolution 720 and the Doppler uncertainty 730 as a function of the Compton scattering angle for a 1 MeV incident gamma ray. In this case we have assumed a 2 keV FWHM energy resolution for the strip detectors, a 1 mm position resolution in three dimensions at each of the first three interaction sites, and a 15-cm mean-free-path between interactions (including the gaps between the layers of detectors). It is seen that for a broad range of scatter angles from about 20 degrees to 120 degrees, over which scatter angles the Compton cross section has a broad maximum, the total angular uncertainty is about 1 degree or less.
[0051] The angular uncertainty in the direction of the incident gamma ray is indicated in FIG. 8. Incident gamma ray 800 Compton scatters at location 815 and Compton scattered gamma ray 810 leaves at an angle θ 1 relative to the direction of incident gamma ray 800 . The direction cone of the incident gamma rays is shown as 825 , where the possible directions of the incident gamma ray is confined to an annular conical volume with a half opening angle of θ 1 and an angular width of 2 times dθ 1 (total).
[0052] The excellent energy and spatial resolution of the detector enables the analysis of the several energy losses associated with an incident gamma ray (nearly coincident in time) to determine the sequence of interactions that are consistent with the energy and momentum Compton scattering laws at the first two interaction sites. This provides a unique determination of the direction cone and energy of the incident gamma ray, without necessitating the full absorption-based measurement and calculation from the incident gamma ray; however, it should also be understood that such a full absorption event is also accurately recorded, i.e. the incident gamma ray direction cone and energy accurately determined according to the technique elaborated on above, by the device and method of the invention.
[0053] Furthermore, background events, which are internal to the instrument or come from directions other than the field-of-view, are rejected with high efficiency. This is particularly important for gamma ray devices that operate in a high radiation environment such as those used in space. Take as an example a silicon detector array operating in space. A significant limitation on sensitivity and capability is imposed by the radiation produced by the interaction of cosmic ray and trapped particles in the Earth's high-energy radiation belts with the materials in the detector system and structure. Among the radioactive nuclei produced in abundance are for example, 22 Na and 24 Na which decay with the emission of gamma rays with characteristic energies (511 keV and 1275 keV for 22 Na and 1369 keV and 2754 keV for 24 Na). The techniques of this subject patent will prove useful to eliminate much of this background as follows. When a radioactive nuclide is produce and subsequently decays, the gamma ray will typically interact in the detector through several Compton interactions with escape of a Compton scattered gamma ray possible or likely. For those events that interact at least three times the several possible interaction sequences can be investigated to determine the likely energy and direction cone of the initial gamma ray. If this is consistent with the known gamma ray emission line energies of abundant spallation products and/or consistent with the direction of a coincident particle emitted during the decay, this event can be rejected by including the programming or algorithm run on processor 16 or 216 to discriminate out the selected detection event based on the positon and energy calculation matching or closely matching one or more of the predetermined values or parameters. It is evident that the ability to achieve this internal background rejection is greatly enhanced with detectors that provide both excellent energy and position resolution.
[0054] Obviously many modifications and variations of the present invention are possible in the light of the above teachings. It is therefore to be understood that the scope of the invention should be determined by referring to the following appended claims.
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A device for determining the photon energy E 1 and direction cone angle of incident gamma ray includes a radiation detector for receiving an incident gamma ray having an unknown photon energy E 1 and an unknown direction and for scattering the gamma ray with two Compton scattering interactions and a subsequent scattering or absorption interaction. The detector provides three outputs, each output corresponding to one of the Compton scattering and the subsequent scattering or absorption interactions, to a processor, which is programmed to calculate the photon energy E 1 and direction cone angle of the incident gamma ray based on these outputs. The detector configuration, for example one that includes multiple detector layers, provides an accurate determination of both the position and energy of the incident gamma ray, while the calculation of the photon energy E 1 and direction cone angle of the incident gamma ray does not require absorption and measurement of the entire or substantially all the energy E 1 in the detector.
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FIELD OF THE INVENTION
This invention relates generally to methods and apparatus for efficiently heating biological tissues with high intensity ultrasound for therapeutic purposes, and in particular, to endoscopic devices for applying ultrasound energy to uterine fibroids and other pathologic tissues that are inside body or organ cavities, to destroy the tumor or the diseased tissue.
BACKGROUND OF THE INVENTION
Fibroids are benign tumors in women's uteri. There are different types of fibroids, including submucosal, which are inside the uterine cavity; intramural, which are in the uterine wall; and subserosal, which are outside the uterus. Fibroids may cause excessive bleeding and pain. For symptomatic fibroids, surgery is the predominate treatment. Every year in the U.S., there are more than 200,000 cases of fibroid-caused hysterectomies. To preserve the uterus, the patient may choose myomectomy, which removes the fibroids only. There are more than 80,000 abdominal myomectomies each year in the U.S. These surgical procedures cause significant trauma to the patients and result in significant costs. Consequently, patients need several days of hospital stay and suffer from the prolonged recovery.
Minimally invasive surgical (MIS) procedures have been explored to treat uterine fibroid trans-abdominally or trans-cervically under laparoscopic or hysteroscopic guidance. Many MIS apparatus have been developed to make the procedure less difficult. Several prior art devices are described in U.S. Pat. No. 5,304,124; U.S. Pat. No. 5,662,680; and U.S. Pat. No. 5,709,679. Besides surgically resecting and removing the tumor tissue, alternative treatments include using different energy forms, such as laser, radio frequency (RF), and cryo-therapy, to thermally ablate or necrose the fibroid tissue. Most of these techniques require the insertion of needles or other types of devices into the body of the fibroid. The mechanical damage to the fibroid and the uterus can cause bleeding during the treatment and adhesions after the treatment. Suturing the damage in the uterus is very difficult in the laparoscopic MIS procedure. Also, most of these alternative treatments are time consuming and technically challenging.
Uterine arterial embolization (UAE) has been investigated as an alternative treatment for uterine fibroids. In UAE, a catheter is inserted into the patient's femoral artery. The catheter is then advanced until its tip reaches the uterine artery. Many small particles are then injected into the uterine artery to block the blood flow. Both left and right uterine arteries are treated. Blood vessels supplying uterine fibroids are typically larger than the vessels in the normal uterine tissue. With properly sized particles, the blood vessels feeding the uterine fibroids are embolized, but not those in the normal uterine tissue. The fibroids then starve and die due to lack of a blood supply. The uterus survives, however, on the blood supplied from the ovarian artery and other collateral circulation. The embolization procedure may cause severe pain in the first few days after the treatment. Other disadvantages of UAE may include long X-ray radiation exposure during the procedure and other long-term potential adverse effects. The procedure is not recommended if the patient seeks a future pregnancy.
Ultrasound is a term that refers to acoustic waves having a frequency above the high limit of the human audible range (i.e., above 20 KHz). Ultrasound waves have the capability of penetrating into the human body. Based on this property, ultrasound in the frequency range of 2-20 MHz has been widely used to image internal human organs for diagnostic purposes. Ultrasound imaging has also been suggested as a tool for guidance during a resectoscopic surgery (U.S. Pat. No. 5,957,849).
When ultrasound energy is absorbed by tissue, it becomes thermal energy, raising the temperature of the tissue. To avoid thermal damage to tissue, the power level in diagnostic ultrasound imaging is kept very low. The typical ultrasound intensity (power per unit area) used in imaging is less than 0.1 watt per square centimeter. High intensity focused ultrasound, which can have an intensity above 1000 watts per square centimeter, can raise the tissue temperature at the region of the spatial focus to above 60-80 degrees Celsius in a few seconds and can cause tissue necrosis almost instantaneously.
High intensity ultrasound has been proposed to treat and destroy tissues in the liver (G. ter Haar, “Ultrasound Focal Beam Surgery,” Ultrasound in Medicine and Biology, Vol. 21, No. 9, pp.1089-1100, 1995); in the prostate (N. T. Sanghvi and R. H. Hawes, “High-intensity Focused Ultrasound,” Experimental and Investigational Endoscopy, Vol. 4, No. 2, pp.383-395, 1994); and in other organs. In U.S. Pat. Nos. 5,080,101, 5,080,102, 5,735,796, 5,769,790, and 5,788,636, for example, ultrasound imaging is combined with a high intensity ultrasound treatment to target the treatment region and to monitor the treatment process. In U.S. Pat. Nos. 5,471,988, 5,492,126, 5,666,954, 5,697,897, and 5,873,828, endoscopic ultrasound devices with both imaging and therapeutic capabilities are disclosed. These devices all have an elongated tube or shaft, so that they can be inserted in organ cavities (e.g., into the rectum) or into the abdominal cavity through a puncture hole in the abdominal wall to bring the ultrasound imaging and treatment sources closer to the disease sites. Some of them have flexible ends, which can be bent to fit the anatomy of a specific patient.
The therapeutic ultrasound beam is focused inside tissue to a small spot of a few millimeters in size. At the focus, tissue temperature rapidly exceeds a level sufficient to cause tissue necrosis, thus achieving the desired therapeutic effect. Outside of the focus, ultrasound energy is less concentrated, tissue temperature rise remains below the necrosis level during the typically short exposure times employed. To treat a tissue volume larger than the focal spot, in the prior art, the ultrasound focus is deflected mechanically or electronically to scan, or incrementally expose, the target tissue volume. One disadvantage of the current high intensity ultrasound therapy is its inefficiency when treating large tumors or heating a large volume of tissue. Even though a three-second ultrasound pulse can increase the temperature of tissue at its focus dramatically, the ultrasound treatment must typically pause 40-60 seconds between two subsequent pulses to allow the intermediate tissue between the focus and the ultrasound transducer to cool sufficiently to avoid thermally damaging the tissue. The volume of tissue necrosis for each treatment pulse is very small (˜0.05 cm 3 ). For example, to treat a volume of tissue within a 3 cm diameter sphere, it will take more than 4 hours, too long to be practical in most clinical situations. Many symptomatic uterine fibroids are larger than 2-3 cm in diameter, and multiple fibroids are also common. To be acceptable for clinicians and patients, the ultrasound treatment time must be significantly reduced.
Large device size is the second disadvantage of the therapeutic ultrasound apparatus in much of the prior art. Most of these devices have two separated ultrasound transducers, including one for imaging and the other for therapy. For effective treatment, the diameter of the treatment transducer is approximately equal to the maximum depth, where the f-number (transducer diameter divided by its focal length) of the transducer is about one (f/1). The transducer surface area must also be sufficiently large to generate high ultrasound power. In some prior art endoscopic devices (for example, in U.S. Pat. Nos. 5,471,988 and 5,873,828), there is a large orifice in the center of the therapy transducer for positioning an imaging transducer. This orifice reduces the area of the treatment transducer and increases its effective f-number. In this case, the size of the treatment transducer must be increased to maintain its effectiveness, so that the overall dimensions of the device are increased. For endoscopic (trans-cervical or trans-abdominal) uterine fibroid treatments, the maximum acceptable diameter of an ultrasound device is about 10 mm. It is seen that it is very difficult to meet this requirement with the large two-transducer configuration.
There is another disadvantage of the two-transducer configuration in which there is an orifice in the center of the treatment transducer. In endoscopic uterine fibroid treatment, the ultrasound device is directly brought against the surface of the fibroid tumor. The tumor surface near the orifice of the transducer will not be treated unless the transducer is moved away or aside from its initial position. Oftentimes, the space is very limited, especially inside the uterus. There may not be sufficient space to permit the device to move, a limitation that results in incomplete treatment of the tumor.
What is needed is a minimally invasive or noninvasive device for treating uterine fibroids. The device should preferably cause minimal or no trauma to the patient body so that the patient requires minimum or no recovery time; it should be easy to use; and, the treatment should be quickly administered. The device should preferably not cause blood loss during the treatment procedure; it should not mechanically damage the treated organ (e.g. uterus) to avoid the need for complicated organ repair (such as suturing or extensive cauterization); and, it should not increase the risk of post-operative adhesions and other complications. In addition, the device should be capable of carrying out the following functions:
(1) Ultrasonically increase the tissue temperature in the uterine fibroid to cause tumor necrosis. Shrinkage of the necrosed tissue will reduce the blood supply to the tumor. This occlusion effect will further reduce the chance of survival for the tumor. (2) Significantly reduce the ultrasound treatment time and thereby improve physician and patient acceptance. A positive feedback heating process can be provided to efficiently and rapidly raise the temperature in a large volume of tissue. (3) Combine the ultrasound imaging and therapy transducer in one to enable the dimensions of the apparatus to be more compact so that the device can be inserted into patient's uterine cavity or permit practical laparoscopic use (e.g., be inserted trans-abdominally). (4) Include a treatment transducer that does not have an orifice in its center, so that the tumor tissue can be treated thoroughly. (5) Provide ultrasound imaging capability for treatment guidance. The imaging capability should provide real-time assessment of the anatomy before, during, and after the treatment. Doppler imaging can be advantageously employed to aid targeting and the assessment of treatment. (6) Use ultrasound to detect and differentiate the tissue property changes before and after the treatment to make an assessment of the treatment result possible. (7) Create an acoustic absorption barrier inside the treated tissue to prevent the tissue beyond the desired treatment zone from being thermally damaged. (8) Provide a feedback control mechanism to turn the treatment transducer element off when the transducer is not properly coupled to the tissue to prevent the device from being damaged by reflected ultrasound power. (9) Provide an effective cooling mechanism to prevent the device from being thermally damaged. (10) Use an ultrasound contrast agent (micro-bubbles) to enhance the treatment effect. (11) Provide effective means to acoustically couple an ultrasound source to targeted tissue structures. (12) Use elasticity imaging to assess the state of tissues prior, during, and after ultrasonic treatment. (13) Employ cavitation as a therapeutic means to necrose selected tissues.
Currently, an endoscopic ultrasound probe is not available that can provide the above-noted functions. Accordingly, it will be apparent that both such a device and an effective and efficient method for treating uterine fibroid tumors and other internal tissues and diseased tissue masses is needed that overcomes the problems with prior art apparatus and methods.
SUMMARY OF THE INVENTION
The present invention is directed to a method and apparatus for efficiently treating uterine fibroids and other diseases with high intensity ultrasound, where the apparatus is small enough to fit in the limited space in a patient organ cavity or a limited puncture size on an abdominal wall.
Specifically, an ultrasonic system for destroying undesired tissue at an internal site within a body of a patient includes a probe that is sized to be inserted within a body of a patient. An ultrasonic transducer is mounted proximate a distal end of the probe and is adapted to couple to a power supply used to selectively energize the ultrasonic transducer so that it produces a focused beam of high intensity ultrasonic energy. An ultrasound transmissive interface is coupled to the distal end of the probe and is disposed and adapted to conform to a surface of the undesired tissue. The interface provides a liquid layer that more efficiently transmits the high intensity ultrasonic energy produced by the ultrasonic transducer into the undesired tissue. The high intensity ultrasonic energy increases a temperature of the undesired tissue sufficiently to cause the tissue to necrose.
In one form of the invention, the ultrasound transmissive interface comprises an elastomeric cavity that is adapted to contain a liquid. The elastomeric cavity is disposed between the ultrasonic transducer and the surface of the undesired tissue so that the high intensity ultrasonic energy passes through the liquid within the elastomeric cavity and into the undesired tissue. The elastomeric cavity is formed at least in part from a semi-permeable membrane, so that the liquid from within the elastomeric cavity weeps onto a surface of undesired tissue to increase the efficiency with which the high intensity ultrasonic energy is coupled into the undesired tissue.
In another form of the present invention, the ultrasound transmissive interface comprises a cap made of an elastomeric material, which is disposed to surround the ultrasonic transducer. The cap is adapted to seal against the undesired tissue and to contain a liquid that increases an efficiency with which the high intensity ultrasonic energy is coupled into the undesired tissue. In addition, the cap preferably includes a rim having a double lip seal formed around a perimeter. A passage in the cap is adapted to couple the double lip seal to a vacuum line so that the rim of the cap is held against a surface of the undesirable tissue, sealing the liquid inside of the cap.
Another aspect of the present invention is directed to a method for administering an ultrasonic therapy to destroy at least a portion of an undesired tissue mass. The method includes the steps of providing an ultrasonic transducer that emits a focused high energy ultrasonic energy when energized, and positioning the ultrasonic transducer proximate the undesired tissue mass. The ultrasonic transducer is directed toward a desired focal point within the undesired tissue mass. Then, the ultrasonic transducer is energized so that it emits the focused high energy ultrasonic energy at the desired focal point, causing necrosis of a portion of the undesired tissue mass disposed at the desired focal point. At least one of an f-number, an intensity, a time, and a direction of the high intensity ultrasonic energy emitted into the undesired tissue mass is controlled to achieve a desired shape and size of a necrotic zone of undesired tissue, destroyed as a result of being heated by the high intensity ultrasonic energy. The necrotic zone substantially blocks the high intensity ultrasonic energy from penetrating beyond the necrotic zone. The desired shape and size of the necrotic zone are preferably selected and formed so as to cause substantially of the undesired tissue mass to ultimately be destroyed.
The step of controlling preferably includes the step of repositioning the ultrasonic transducer to direct the high intensity ultrasonic energy at a different portion of the undesired tissue mass, to achieve the desired shape and size of the necrotic zone. In one application of the method, the desired shape and size of the necrotic zone are selected so that formation of the necrotic zone substantially deprives the undesired tissue mass of a blood supply, causing the ultimate destruction of the undesired tissue mass. In another application of the method, the desired shape and size of the necrotic zone are selected to control bleeding at a treatment site.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
The foregoing aspects and many of the attendant advantages of this invention will become more readily appreciated as the same becomes better understood by reference to the following detailed description, when taken in conjunction with the accompanying drawings, wherein:
FIG. 1 is a block diagram of the positive feedback mechanism of the improved tissue heating process;
FIG. 2A-2D illustrate different thermal lesion shapes;
FIG. 3A is a cross-sectional view of a portion of a patient's body, illustrating application of an endoscopic device in accord with the present invention, which can both acquire ultrasound images and generate high intensity therapeutic ultrasound at its distal end;
FIGS. 3B and 3C are side elevational views of a portion of the device shown in FIG. 3A , illustrating an imaging field and a treatment field of the device;
FIGS. 4A and 4B are schematic diagrams of different treatment beam forming techniques used to control the lesion geometry and illustrating spatial lesion formation;
FIGS. 5A and 5B are schematic diagrams of different treatment beam forming techniques used to control the lesion geometry and illustrating spatial-temporal lesion formation;
FIG. 6 is a schematic diagram of the trans-cervical ultrasound device with an articulated end;
FIGS. 7A and 7B are schematic diagrams showing transcervical hemostasis treatment performed in combination with resectoscopic removal of submucosal fibroids;
FIGS. 8A and 8B are schematic diagrams respectively showing the trans-cervical and the trans-abdominal ultrasound device treating intramural fibroids from inside and from outside of the uterus;
FIGS. 9A and 9B are schematic diagrams respectively showing laparoscopic occlusion treatment of subserosal fibroids, and a wedge of necrosed tissue produced thereby;
FIG. 10 is a block diagram of the trans-cervical ultrasound device connected with its control unit, display, and fluid management unit;
FIG. 11 is a side elevational view of the ultrasound device and a cross-sectional view of a liquid-filled vacuum cap that provides coupling between the fibroid tumor and the ultrasound transducer;
FIG. 12 is a system block diagram of the control electronics in the control unit; and
FIG. 13 is an isometric view of a portion of an ultrasound device that includes a structure to maintain a gap between the tissue being treated and an ultrasound transducer array, to convey a coolant liquid.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In the following description of the present invention, its application in treating uterine fibroid tumors is discuss in some detail. However, it should be emphasized that the device and methods described herein may also be used to apply ultrasound therapy treatment to other organ systems, lesions, and disease states. The therapy delivered may be thermal ablation, where a temperature rise is established to a level at which tissues are no longer viable; mechanical ablation, where cavitation is employed as the primary ablative means; or may achieve hemostasis wherein bleeding or blood flow in intact organs is arrested. Such applications of the present invention may be accomplished in open, invasive surgery, by way of established minimally invasive techniques (for example, by way of body entry through one or more small incisions or punctures), or in some cases, noninvasively, through the skin surface or through the linings of body cavities such as the rectum, vagina, or esophagus. Ablative treatment with the present invention may be applied to a wide range of benign or cancerous lesions of the liver, kidney, pancreas, spleen, prostate, breast, bowel, rectum or similar organ systems, wherein the device described herein may be placed in close proximity to the disease location. Also, acoustic hemostasis treatment may be employed to deprive a disease lesion of its blood supply or used to facilitate surgical procedures by arresting bleeding or blood flow.
Many tumors, such as uterine fibroids, locate superficially inside or outside the organ. During hysteroscopic or laparoscopic surgeries, surgeons can easily reach the surfaces of those tumors with an intra-cervical or intra-abdominal instrument. For an ultrasound transducer at the tip of the intra-cavity instrument touching the tumor directly, there will be little or no intermediate tissue that needs to be spared and cooled, so that pauses in the treatment for this purpose may become unnecessary.
According to conventional wisdom, the pre-focal heating is considered to be a negative effect and needs to be minimized. In the case of intra-cavity treatment of uterine fibroids, however, this pre-focal heating can provide significant enhancement to the efficiency of tissue heating when the ultrasound transducer can be disposed in close contact with the tumor surface. A positive feedback mechanism of tissue heating (illustrated in FIG. 1 ) is preferably used to improve the efficiency of the treatment provided by the present invention. The positive feedback indicated by a block 2 of FIG. 1 enhances acoustic absorption. The acoustic energy is converted to heat, as noted in a block 4 , resulting in a greater temperature rise in the tissue, as indicated in a block 6 . Tissue acoustic absorption increases significantly when its temperature rises above 50° C. Referencing FIG. 2A , a small f-number, high intensity ultrasound transducer 10 , running in continuous-wave (CW) mode, raises the temperature in tissue 12 at its focus to 70-90° C. in less than two seconds and forms a small lesion 14 . This isolated thermal lesion serves two purposes. First, it is the initial seed to start the positive feedback heating process; and, secondly, its high acoustic absorption blocks ultrasound energy from penetrating beyond the focal depth to cause undesirable damage to normal tissue. In an experimental study, it was observed that after the lesion started at the focus, it first grew along the central axis of the transducer and towards the transducer to form an elongate lesion. Then, the end of the elongate lesion closer to transducer began growing laterally wider. Eventually, the lesion became a wedge shape 16 ( FIG. 2B ). The tissue layer near the surface, adjacent to transducer 10 , was the last portion to necrose.
In an experimental study, a wedge-shaped lesion of tissue necrosis was generated with this mechanism by running the ultrasound power continuously, while keeping the transducer position fixed. The volume of the thermal lesion was about 4.5 cm 3 , and the treatment time was approximately two minutes. The average treatment rate was about 2.25 cm 3 /min, which was 45 times faster than provided by a conventional pulse-pause treatment strategy.
Using the present invention, the size and the shape of the large thermal lesion can be readily controlled. To form a thin elongate lesion column 20 in the tissue ( FIG. 2C ), a circular transducer 18 with a relatively large f-number (˜2) is used to treat the tissue over a relatively short time. To create a conical shaped lesion, a circular transducer with a small f-number (˜1) is used to treat the tissue for a relatively long time. To form a thin, wedge-shaped lesion, i.e., shaped like a slice of pie ( FIG. 2B ), a cylindrical or truncated circular transducer is used to treat the tissue over a relatively long time. A generally rectangular lesion plane 21 ( FIG. 2D ) can be generated by forming a row of tightly spaced lesion columns 22 , 24 , and 26 . Each column is formed from a fixed transducer position in a short time. The transducer may then be quickly shifted laterally to generate the next adjacent column, moving from position “A” to “B” to “C” as shown in FIG. 2D . Thermal diffusion in the tissue fuses the columns together to form rectangular lesion plane 21 . It is also possible to create a large lesion in the tissue without damaging the organ surface. One approach is to cool the tissue surface with circulating water or saline. The other approach is to use an attenuation measurement technique described below, to monitor lesion progress (growth) and control power, accordingly.
The basic concept and configuration of a high intensity ultrasound device 29 in accord with the present invention are shown in FIGS. 3A and 3 B. The device has a thin, elongate shaft 28 that can be inserted through the cervix into the uterine cavity, or, as shown in FIG. 3A , through a laparoscopic opening 34 in the abdominal wall and into the abdominal cavity. A distal end 30 of the shaft contains a concave-shaped ultrasound transducer array 36 ( FIG. 3B ) and may be formed into different curves to fit different anatomies of individual patients. The distal end that is thus formed can be permanently fixed or articulated by turning a control knob 32 on a handle 33 of the device. Transducer array 36 in FIG. 3B is operable for both ultrasound imaging and treatment. To form an ultrasound image, the transducer array generates ultrasound pulses and receives echoes from the imaged anatomy in a cross-sectional area 40 . The two-dimensional (2D) ultrasound image displays the cross-sectional view of the anatomy. The image can be updated rapidly in real-time with a frame rate of, for example, 10-30 frames per second. Physicians can then view this real-time image to locate the tumor or other tissue that needs to be treated or spared from treatment. When the treatment area is identified in the image, the transducer array is employed to generate high intensity ultrasound focused in a treatment area 38 . After the tissue in the treatment area has been necrosed, the distal end of the ultrasound device is moved to a new location to sequentially treat another part of the tumor tissue. The imaging and the treatment are interleaved in time so that the treatment process and the progress of the treatment may be monitored.
Doppler flow imaging (spectral Doppler or power mode Doppler) may be utilized to assist targeting and to monitor treatment effects and to determine the endpoint of the therapy. Imaging blood flow is particularly useful when a blood flow occlusion strategy is being utilized, since the cessation of blood flow can be directly monitored. Doppler imaging facilitates localization of the vascularity typically surrounding uterine fibroid tumors or other tumor masses.
There are many possible combinations of the imaging and treatment capabilities. Imaging and therapy may be one-, two-, or three-dimensional in various combinations; scan geometries may be fixed or selectable; and imaging and therapy may proceed either simultaneously or sequentially in time. A preferred embodiment of the ultrasound intra-cavity device discussed herein has the capability to carryout 2D real-time imaging and the capability to produce tissue necrosis in a substantially 2D slice (thickness of this slice is nominally less than one centimeter). Including the lesion-control techniques discussed above, there are many ways to control treatment geometry with this device. Different spatial beam patterns can be generated from by the ultrasound transducer array included on the device to form a specific lesion shape, or potentially, to reduce treatment time. Multiple sequential exposures of different spatial beam patterns can also be used to control the treatment dosage at different locations to form lesion shapes that cannot be generated by fixed beam patterns.
As shown in FIG. 6 , a trans-cervical ultrasound device 68 is adapted to treat submucosal fibroids. The device is inserted into a patient's uterine cavity through the vagina and the cervical canal. The uterine cavity is distended with sterile water or saline under 50-80 mm Hg pressure delivered through internal channels inside a shaft 70 of the device and connected to couplings 78 and 76 . The water provides working space for manipulation of the device, and the water thus infused also serves as a transducer coupling and cooling medium.
The fibroid is visualized by ultrasound imaging using trans-cervical ultrasound device 68 . As a function of the tumor size and shape, the physician selects the appropriate treatment geometry and turns the therapeutic ultrasound power on to necrose a slice volume of the tumor tissue in front of the transducer. The entire tumor is then treated typically piece by piece. During the treatment, the transducer (not separately shown) at a distal end 72 of the device does not have to directly contact the tumor surface—the water in the uterus is a good acoustic coupling and transmission medium. After the tumor is completely treated, the physician removes the device and drains the water from the patient's uterus. The procedure is finished without any surgical invasion to the tissue.
There are two possible approaches for providing treatment of a submucosal fibroid tumor 94 with trans-cervical ultrasound device 68 . The physician can treat the whole tumor directly with the ultrasound device, as shown in FIG. 7A , or treat only a remaining tumor base 96 , as shown in FIG. 7B , after a portion of the tumor is removed by using a resectoscope. In FIG. 7A the transducer in distal end 72 is placed adjacent to tumor 94 inside a water-filled uterine cavity 90 . For the latter approach, the ultrasound device works not only as an ablation tool, but also as a hemostasis tool to seal off the open, bleeding vessels around and inside the exposed tumor base.
A similar technique may be used to treat intramural fibroids as illustrated in FIGS. 8A and 8B . If a tumor 93 is closer to the inside of the uterus ( FIG. 8A ), a trans-cervical ultrasound device is the choice for the treatment. Otherwise, a trans-abdominal device may be used ( FIG. 8B ). Some intramural fibroids 96 are imbedded inside normal uterine tissue, e.g., in a uterine wall 92 . The physician may want only to necrose the tumor but not the uterine wall that covers the tumor. In this case, the physician can use the lesion geometry control techniques described above to heat only the tumor inside the uterine wall without thermally damaging the surrounding tissue.
Subserosal fibroids are disposed substantially outside of the uterus. When these are symptomatic, they may be larger than submucosal and intramural fibroids. However, the trans-abdominal ultrasound device according to the present invention can also be used to treat them. If the physician uses the same treatment technique as described above to thermally necrose the entire tumor, it will take longer time, because they are relatively large. An alternative approach is shown in FIGS. 9A and 9B , where only the tumor base is treated by a series of sectors, or pie-shaped applications 100 , 102 ( FIG. 9B ) that are circumferentially disposed around the base of a tumor 98 . After the entire tumor base is heated sector by sector, the tumor tissue in the base shrinks. The tissue shrinkage occludes blood vessels in the base and achieves effective tumor starvation as oxygen and nutrient supplies are interrupted. Without a blood supply, the tumor will die. The necrosed tumor will then shrink in volume, so that the pressure symptoms experienced by the patient due to the growth of the tumor will be relieved.
A system 104 that supports operation of trans-cervical ultrasound device 68 is shown in FIG. 10 . The system consists includes one or more ultrasound applicators 126 , an optional optical hysteroscope (not separately shown), which is inside the applicator, and its associated camera 112 , a treatment control unit 110 , a TV monitor 122 , and a fluid management system that includes a fluid management system pump 120 , tubing 116 , and a waste collection container 114 . The hysteroscope, camera, monitor, and fluid management system are typically available in a well-equipped gynecology operating room. The optional hysteroscope may be useful for visually locating the tumor. Control unit 110 provides electronic signals and power to the ultrasound transducer for both imaging and therapy. The ultrasonic image and the optical image from the camera attached to the hysteroscope are combined in the control unit and are preferably displayed on the monitor in a “picture-in-a-picture” format 124 . Alternatively, either one of the images may be displayed alone. Fluid management system pump 120 controls the saline or water pressure and the flow rate into the uterus.
Different configurations of the trans-cervical ultrasound device shown in FIG. 6 have specific advantages. They all have two irrigation channels for fluid in and out, one electrical cable to connect to the control unit, and one utility channel for the hysteroscope. The difference is in their tip configuration. In FIG. 6 , the distal end of the applicator can bend to different angles 80 about a pivot 74 , to accommodate different approaches to the treatment zone. A knob 77 at the device handle controls the tip articulation, providing an adjustable head angle over a range of up to 90 degrees. Alternatively, the distal end of the device may be fixed, and several applicators of different fixed tip angles can be provided for different treatments.
The ultrasound transducer in the end of the trans-cervical applicator may have a limited usable lifetime. The tip of the device may be a reposable (disposable, with a limited number of times of reuse). A used tip can thus be removed, and a new tip attached. The reposable portion may include shaft 70 , so that the connection port will be in the handle, which stays outside the patient and is not immersed in fluid.
Trans-abdominal ultrasound device 29 shown in FIGS. 3A and 3B has a long shaft 28 that can be inserted into the patient's abdominal cavity through laparoscopic surgery cannula 34 , which is disposed in a puncture hole on the abdominal wall. Under visual guidance of a laparoscope, distal end 30 of the device is brought in close contact with the uterine fibroid. As in the trans-cervical device, ultrasound array transducer 36 is preferably mounted at distal end 30 of the device for imaging and therapy. Guided by the ultrasound image, the physician uses the device to necrose the fibroid tissue. The distal end of the device is preferably articulated at a flexible shaft segment 31 , as shown in FIG. 3C , with one or two knobs 32 (depending upon whether one or two axes of articulation are provided) that are disposed on handle 33 of the device. This flexible shaft segment permits treatment zone 38 to point in different directions to accommodate different tumor positions. The ultrasound transducer may be disposed in a cover case balloon 41 or other cover at the tip of the device ( FIG. 3C ).
Cover case balloon 41 is elastomeric and conforms to an outer surface of a tumor, providing more efficient acoustical coupling between the transducer and the treatment area; the curvature of the tumor contour will, in general, be different from the curvature of the ultrasound transducer. Moreover, during a conventional laparoscopic procedure, the patient's abdomen is inflated with CO 2 gas to create a large working space. A gas gap between the transducer and the tumor, however, would block the ultrasound transmission. Instead of penetrating into the tumor, the ultrasound beam would be reflected back to the transducer. The therapeutic effect would thus be diminished and the transducer might be damaged by the reflected ultrasound energy.
It thus is important to maintain good acoustic coupling between the treatment tissue and the ultrasound transducer while provide the ultrasound therapy. Water, saline, and most water-based solutions and gels are excellent coupling media. In diagnostic ultrasound imaging, water-based coupling gel is widely used. However, gel may have limitations in trans-abdominal ultrasound therapy for treating uterine fibroids. Unlike skin, the fibroid is much less compressible. It is also more difficult to apply manual pressure during a laparoscopic procedure to conform the fibroid to the surface contour of the transducer. Gel may be used to fill the remaining gaps, but gas bubbles trapped in the gel are difficult to squeeze out.
In this preferred embodiment of the present invention, water-filled cover case balloon 41 ( FIG. 3C ) is fabricated of thin elastic material and is placed between the transducer and the fibroid to ensure effective coupling of the ultrasonic energy into the tumor mass. Under a small manual pressure, the balloon is conformed to both the transducer surface and the fibroid surface. If the transducer is inside the balloon, only the fibroid surface needs to be wetted with sterile saline to keep a good coupling to the balloon surface. Alternatively, cover case balloon 41 may be fabricated of a semi-permeable membrane material that enables liquid to weep from inside the balloon. The “weeping” of the fluid from the balloon thus can keep the fibroid surface wet during the treatment. When the internal pressure is higher than the pressure in the abdominal cavity, the sterile saline or water inside the semi-permeable balloon readily weeps through the semi-permeable membrane to create a fluid interface-layer that maintains continuous effective coupling.
Alternatively, as shown in FIG. 11 , a vacuum cap 138 made of soft rubber, plastic, or other elastomeric material, may also be applied at the distal end of the device to provide the acoustic coupling as shown in cross section at FIG. 11 . The cap surrounds ultrasound transducer array 36 and is open at its front, opposite the array. The front opening of the cap is large enough to permit the ultrasound beam to pass without obstruction. Around the open end of the cap, a rim 131 has a double lip 130 . The double lip is soft and elastomeric and can conform to the shape of a tumor surface 136 . A vacuum port 134 is provided in fluid communication with the double lip, and a vacuum source coupled to this port provides a negative pressure within the double lip that holds the cap tightly on the tumor. Sterile water is then provided through a port 132 that communicates with an interior of the cap to provide the acoustic coupling between the transducer and the tumor. The cap works as a wall to block gas from getting into the cap. In case there are any minor leaks, the leaking gas and water are removed immediately at the double lip.
To protect the ultrasound transducer against accidental damage caused by the reflected ultrasound power when there are large gas bubbles or gaps between the transducer and the tumor, or when the device is lifted from the tumor while the high intensity ultrasound output is still on, the present invention preferably uses the ultrasound imaging capability to detect the existence of gas. When a gas gap exists, it causes a strong reflection detected when ultrasound imaging. The reflection may also bounce back and forth between the transducer and the gas gap, resulting in a reverberation (multiple reflections). The strong reflection or reverberation appear(s) as very bright echoes in a large portion of the image. When observing this unique echo image, the medical practitioner may adjust the position or the coupling of the ultrasound device to eliminate the trapped gas. As an alternative, an automatic gas detection technique may be used to avoid the reflection damage. By using the unique characteristics of the gas in the reflected echo signal, the system may detect its existence during the imaging process. When the strong echo is detected, the system may automatically turn off the high intensity ultrasound output to the area where there are gas gaps. This automatic power shut down process is accomplished almost instantaneously, so that thermal damage to the transducer array is avoided.
During therapy application, the ultrasound transducer generate heat internally. This heat can possibly cause damage or reduce the service life of the transducer array. Moreover, if the transducer array touches the tumor tissue directly, the high temperature of the transducer array can prematurely, or inadvertently, necrose the tissue surface. The high acoustic absorption of the necrosed tissue at the surface would also prevent the ultrasound beam from penetrating deep into the tumor, so that the deep tumor tissue might not be properly treated. It is therefore very important to keep the temperature of the transducer array and at the tissue interface relatively low during the treatment.
A plurality of techniques can be employed to cool the transducer array. The simplest approach is to immerse the transducer in water, maintain a gap between the transducer surface and the tumor, and then ensure that the water flows through the gap during the treatment. Two water channels preferably disposed inside the device casing to circulate the cooling fluid may optionally be used for this purpose. The ultrasound transducer array is disposed in one of the channels. Alternatively, both the transducer and the tumor may be immersed in water. In the trans-cervical approach, the uterine cavity is conveniently filled with water. In certain trans-abdominal situations, it may be possible to fill a portion of the abdominal cavity with water. And, in some non-invasive situations it is possible to construct a water dam, sealed at its periphery to the organ surface, creating a water pool in which the applicator may be positioned. As shown in FIG. 13 , a thin-wire fence 162 or frame attached to distal end 72 maintains a gap between transducer array 36 and the first interface of patient tissue (e.g., the tumor's outside surface). A variety of such useful standoff structures may be employed, as best suited for the geometric requirements of the application and specific applicator designs. During treatment, a water jet from a port 160 introduces water, or saline, into the gap. Circulation of conditioned water through one or more such ports may be used to control water temperature, pressure, chemical composition, gas content, or volume. Alternatively, the transducer array may be cooled by using a thermal-conductive, acoustic-matching layer (e.g., aluminum) bonded to the piezoelectric ceramic of the ultrasound transducer array. This thermal-conductive layer removes the heat from the transducer ceramic. The heat is removed by water flowing in attached lines or by heat sinks that are connected to the thermal-conductive layer.
To simplify the device design and to reduce the size of the endoscopic instrument, one ultrasound transducer array is used for both imaging and therapy. A concave transducer array provides a good compromise to simplify the design for both functions. Natural focusing of the concave geometry simplifies the ultrasound beam forming, where there is no (or less) phase delay needed, and cross-talk among array elements is less of a problem. Because of the minimum phase delay required, larger element pitch size can be used. Large pitch size reduces the number of elements in the array and the number of electronic signal channels required. It also helps to reduce the cost of the transducer and the cost of the control unit. Treatment area 38 is geometrically inside imaging area 40 of the array (see FIG. 3B ). The entire treatment area is under the ultrasound imaging monitoring—there is no blind spot in the treatment area.
FIG. 12 is a simplified block diagram of the electronic control system according to the invention. The specific applicator device connected to the control system is recognized electronically by a system controller 206 , which reads applicator data from a memory device, an ID tag 172 . Such data include specific functional and calibration information. A switch matrix 176 connects a concave transducer array 170 to the therapeutic circuitry or to the imaging circuitry. During imaging, an imaging transmitter 186 generates pulse sequences to drive the ultrasound transducer array through a transmit-receive switching matrix 190 . The imaging receiver amplifies and processes the echo signals captured by the transducer array. During the therapy phase, switch matrix 176 connects the transducer array to the therapeutic transmitter chain to form and steer a high intensity ultrasound beam within the tissue being treated. To monitor the treatment process, the transducer array may be periodically switch back to the imaging circuitry to form frames of ultrasound images during the treatment.
System controller 206 provides overall control and synchronization of the multiplicity of functions executed by the system including an operator interface control panel 208 , a foot switch 200 that is used for initiating and arresting therapy, and a timing logic 194 , employed for establishing appropriate phasing of the therapeutic phased array transmit chain. This chain comprises a primary oscillator 182 , a phase locked loop 184 , a multi-channel power amplifier 180 and matching networks 178 . Additionally, timing logic 194 provides data to the imaging chain that includes the receive amplifiers and time-gain compensation circuits 188 , a quadrature detection circuit 196 , an analog-to-digital conversion circuit 192 , an Intensity (B) mode processing circuit 198 , an attenuation processing circuit 204 , a Doppler flow processing circuit 212 , and a scan conversion circuit 202 . Images of the target tissue are converted to a format compatible with standardized operating room video display in image merging circuits 210 and mixed with other video sources (e.g., hysteroscopic optical imaging), and user interface graphics, and processed in graphic overlay 216 , which is included in a video processor module 214 , for display.
Thermally necrosed tissue has a much higher acoustic attenuation (>1.0 dB/cm/MHz) than the untreated tissue (0.4-0.7 dB/cm/MHz). This property may be used to monitor or visualize the treatment area. One technique to measure the tissue attenuation change is to measure the frequency spectral change in the echo signal. High frequency components in the frequency band are attenuated more than the low frequency components. By subtracting the spectrum before the treatment from the spectrum after the treatment, the attenuation change can be measured. If the subtracted spectrum is near zero, it indicates that the tissue where the echo is acquired has not been treated. If the result of spectrum subtraction has a significant slope, it means the tissue attenuation has changed, indicating that this area has been necrosed.
Alternatively, or in combination with this attenuation imaging, elasticity imaging may be employed to assess tissue state before, during, or after ultrasonic treatment. Elasticity imaging, the principles of which are well known in the art, provides a visualization of physical and mechanical tissue properties. Necrosed tissues are stiffer and demonstrate elasticity changes. Treatment endpoints may be manually or automatically controlled (under operator control) by use of elasticity imaging parameters.
As an alternative method of therapy that may reduce the treatment time even further, the patient may be given an injection of ultrasound contrast agent, which is a solution of encapsulated air-containing micro-bubbles that are sufficiently small to circulate safely in the blood and blood vessels. When the bubbles are flowing through the fibroid, they will be hit by the high intensity therapeutic ultrasound. The bubbles enhance the ultrasound heating process at the treatment area and make the treatment more efficient.
As a further alternative method of therapy, cavitation may be utilized as a mechanism for speeding effective treatment. Ultrasound with high acoustic pressure and lower frequency increases the likelihood of stimulating the onset of cavitation. The presence of contrast media or bubbles also encourages cavitation. Cavitation can aggressively disrupt tissue and increase energy transfer for an enhanced heating effect.
Although the present invention has been described in connection with the preferred form of practicing it, those of ordinary skill in the art will understand that many modifications can be made thereto within the scope of the claims that follow. Accordingly, it is not intended that the scope of the invention in any way be limited by the above description, but instead be determined entirely by reference to the claims that follow.
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An ultrasound system used for both imaging and delivery high intensity ultrasound energy therapy to treatment sites and a method for treating tumors and other undesired tissue within a patient's body with an ultrasound device. The ultrasound device has an ultrasound transducer array disposed on a distal end of an elongate, relatively thin shaft. In one form of the invention, the transducer array is disposed within a liquid-filled elastomeric material that more effectively couples ultrasound energy into the tumor, that is directly contacted with the device. Using the device in a continuous wave mode, a necrotic zone of tissue having a desired size and shape (e.g., a necrotic volume selected to interrupt a blood supply to a tumor) can be created by controlling at least one of the f-number, duration, intensity, and direction of the ultrasound energy administered. This method speeds the therapy and avoids continuously pausing to enable intervening normal tissue to cool.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to the decoding of digital video images.
2. Art Background
Video images in digital format, referred to frequently as digital video (DV) is achieving greater usage as the use of computers for developing video images increases. The digital video data is stored or transmitted in a compressed encoded format, often referred to as "DV" format. The encoding process typically includes a discrete cosine transform (DCT) to translate the pixel data into DCT coefficients and a weighting function to weight the values (See e.g., "Specifications of Consumer-Used Digital VCRs Using 6.3 mm Magnetic Tape", HD Digital VCR Conference, (December 1994)). After the data is decoded, the image is sized for the viewing window, for example, by using a pixel decimation process wherein specified spatially spaced pixels are removed to reduce the number of pixels representative of the image. Thus, a number of pixels decoded are not subsequently displayed.
The decoding process is time consuming due to the number of operations required to decode the data. Thus it is desirable to minimize the time required to perform the decoding process while maintaining a high quality image.
SUMMARY OF THE INVENTION
The system and method of the present invention decodes encoded video images in such a manner as to maintain high quality images while reducing the computation time needed to decode the images. The system takes into account that the resultant display generated may only have a fraction of the resolution of the original image. Thus, optimizations are realized by modifying and combining the inverse discrete cosine transform (IDCT) and inverse weighting (IW) processes to process only the portion of the image to be displayed.
In one embodiment of a decoding of a 1/4 size image, a horizontal 4-point IW/IDCT process is applied to the lower four coefficients in each of the first four rows in an 8×8 matrix of transformed coefficients, referred to herein as a block, which is part of a frame of video. A vertical 8-point IW/IDCT process is applied to all eight coefficients in each of the first four columns with the higher four coefficients in each column set to a value of zero.
In an alternate embodiment, when the input block consists of two 4×8 matrices of sum and difference coefficients, a horizontal 4-point IW/IDCT is applied to the coefficients. A vertical 4-point IW/IDCT is applied to the sums of corresponding sum and difference coefficients.
BRIEF DESCRIPTION OF THE DRAWINGS
The objects, features and advantages of the present invention will be apparent to one skilled in the art from the following detailed description in which:
FIG. 1a is a simplified block diagram of one embodiment of a decoder which operates in accordance with the teachings of the present invention, and FIG. 1b is a simplified block diagram of a general purpose computer that operates in accordance with the teachings of the present invention.
FIG. 2 is a flow diagram illustrating one embodiment of the method of the present invention to perform a combined inverse cosine transform and inverse weighting function on an 8×8 block of coefficients.
FIG. 3 is a diagram illustrating the coefficients processed in accordance with the flow diagram of FIG. 2.
FIG. 4a and FIG. 4b are a butterfly diagrams illustrating one embodiment of the combined one-dimensional 4-point inverse cosine transform and inverse weighting function utilized in accordance with the flow diagram of FIG. 2.
FIG. 5 is a flow diagram illustrating an alternate embodiment of the method the present invention that performs a combined inverse cosine transform and inverse weighting function on two 4×8 matrices of sum and difference coefficients.
FIG. 6 is a diagram illustrating the coefficients processed in accordance with the flow diagram of FIG. 5.
FIG. 7 is a butterfly diagram illustrating one embodiment of a vertical inverse discrete cosine transform and inverse weighting function utilized in accordance with the flow diagram of FIG. 5.
FIG. 8 illustrate alternate representations of butterfly diagrams.
FIG. 9a and FIG. 9b illustrate mathematical implementations of the flow diagram of FIG. 2 and FIG. 5, respectively.
DETAILED DESCRIPTION
In the following description, for purposes of explanation, numerous details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one skilled in the art that these specific details are not required in order to practice the present invention. In other instances, well-known electrical structures and circuits are shown in block diagram form in order not to obscure the present invention unnecessarily.
FIG. 1a illustrates, in simplified block diagram form, one implementation of the decoding circuitry of the present invention. It is readily apparent that the present invention can be implemented in a dedicated microcontroller circuit in logic circuitry or software operable on a general purpose computer. The applications of such decoders are varied. For example, the decoder may be implemented in a computer system that receives digital video signals from an external source such as satellite, broadcasts or digital video players. Alternately, the decoder circuitry may be embodied in digital video player recorders, cameras or other digital video equipment.
Referring to FIG. 1a, the compressed image is input to a deframing subcircuit 110, which unpacks every five fixed-length synchronization blocks into thirty blocks of variable-length coded quantized coefficients. A block is a portion of a frame of video image. In the present embodiment, each encoded block is a matrix of 8×8 discrete cosine transform (DCT) coefficients. In an alternate embodiment, each block consists of two matrices of 4×8 DCT coefficients, one matrix containing sum coefficients and one matrix containing difference coefficients. VL decoder 115 performs a variable length decoding process in accordance with teachings known in the art to generate run-level pairs of DCT coefficients. The flatten run-level circuit 120 expands the run-level pairs into individual DCT coefficients. For example, if a run-level pair sequence consists of (2,2), (4,1), the flattened representation consists of (0,0,2), (0,0,0,0,1). The unzig-zag subcircuit 125 receives the one-dimensional representation of the quantized coefficients and turns it into a two-dimensional representation. The I/Q subcircuit performs an inverse quantization process on the DCT coefficients. The inverse weighting (IW) function 135 inversely weights the coefficients that originally were weighted during the encoding process. One example of the weighting performed is described in "Specifications of Consumer-Used Digital VCRs Using 6.3 mm Magnetic Tape", HD Digital VCR Conference, (December 1994), page 28.
An inverse discrete cosine transform (IDCT) 140 is then applied to transform the DCT coefficients into pixel values. Once the pixel values are generated, a deshuffling process 145 is applied to generate the completed image. The subcircuits 110, 115, 120, 125, 130 and 145 may be embodied a variety of ways known to one skilled in the art and will not be discussed further herein. For further information see, for example, "Specifications of Consumer-Used Digital VCRs Using 6.3 mm Magnetic Tape", HD Digital VCR Conference, (December 1994).
As will be explained below, an innovative combination of inverse weighting (IW) and inverse discrete cosine transform implementation has been developed to provide high quality reduced-sized images with minimal processing overhead. As noted earlier, the present invention also may be implemented on a general purpose computer as illustrated in FIG. 1b.
In this embodiment, the compressed image is received through input port circuitry 150 which forwards the data to the processor 155 which executes instructions from memory 160 to perform the steps described, and in some embodiments, display the decoded image on display 165.
FIG. 2 is a simplified flow diagram of one embodiment of the innovative process for decoding a 1/4 size image in accordance with the teachings of the present invention. The embodiments described herein combine the application of the inverse weighting (IW) and inverse discrete cosine transforms (IDCT) into one function. The advantage to this is that the number of multiplications or computations required is reduced. However, it should be realized that the IW and IDCT of the processes described herein can be applied in a serial manner.
Referring to FIG. 2, at step 205, a one-dimensional (1D) horizontal 4-point IW/IDCT function is applied four times to the lower half, in this embodiment, four, coefficients in the matrix. This is graphically illustrated with respect to FIG. 3.
Matrix 300 is representative of an 8×8 block of DCT coefficients representative of a portion of an image where x represents an encoded coefficient. The index of the matrix 300 increases from left to right and from top to bottom. The coefficients with smaller indices are referred as lower coefficients. The coefficients with larger indices are referred as higher coefficients. Block 305 is representative of the block after application of the 4-point IW/IDCT as set forth at step 205. Referring to block 305, the "A" coefficient is representative of the DCT coefficients after application of the 4-point 1D horizontal IW/IDCT. It should be noted that the present embodiment describes the process with respect to an 8×8 block; however it is contemplated that the process may be applied to n×m blocks, where n is greater than or equal to 4 and m is greater than or equal to 4.
FIG. 4a is representative of one example of a 4-point IW/IDCT applied at step 205 of FIG. 2. IN0, IN1, IN2 and IN3 correspond to locations 301, 302, 303, 304 in each row 306, 307, 308, 309. This particular embodiment of the 4-point IW/IDCT is specified to decode a digital video image encoded in accordance with the specification set forth in "Specifications of Consumer-Used Digital VCRs Using 6.3 mm Magnetic Tape", HD Digital VCR Conference, (December 1994). It should be readily apparent that the 4-point IW/IDCT applied may vary according to the particular encoding process utilized.
The IW/IDCT depicted in FIG. 4a is represented in a form known as a butterfly where, ##EQU1## a diagonal line is representative of an addition operation, an arrow is representative of a multiplication operation by a -1, and values along the line represent a multiplication operation by the noted values. For example, with respect to FIG. 4a, at stage 410, the modifications performed on the input IN0 correspond to IN0+4CS6CS4*IN2 where 4CS6CS4 is equal to 4*CS6*CS4. At a corresponding point stage 411, the modifications performed on IN2 equals IN0-IN2*4CS6CS4. Following through with respect to output 0 (OUT0), output 0 equals IN0+IN2*4CS6CS4+IN1*4CS7+IN3*4CS5CS2+CS4*(IN1*4CS7-IN3*4CS5CS2); where 4CS5CS2=4*CS5*CS2.
Referring back to FIG. 2, at step 210, the higher half, e.g., 4, coefficients in the vertical direction are set to zero. This is graphically represented by block 310 of FIG. 3. It should be noted that it is preferred that the remaining unprocessed coefficients are essentially ignored (as shown by omission in blocks 305, 310, 315) to save additional processing time as the coefficients are not used. At Step 215, an 8-point IW/IDCT is applied vertically. This is illustrated at block 315, which shows that the coefficients represented by the variable B result in pixel data at even coordinates after the 8-point IW/IDCT. The 8-point IW/IDCT implemented in the present embodiment is represented by the butterfly diagram of FIG. 4b. It should be noted that the sequence of operations is interchangeable; thus the horizontal IW/IDCT applied can be applied after application of the vertical 8-point IW/IDCT.
Referring back to FIG. 3, after application of the vertical 8-point IW/IDCT, the 4×4 image generated, represented by block 320, contains a high quality portion of the image. This quality image was generated with minimum processing overhead. Thus substantial time savings is realized.
An alternate embodiment is shown with respect to FIG. 5. FIG. 5 processes a representation of an image which is formed by two 4×8 blocks. One 4×8 block consists of sum DCT coefficients and one 4×8 block consists of difference DCT coefficients. The use of 4×8 blocks is defined in "Specifications of Consumer-Used Digital VCRs Using 6.3 mm Magnetic Tape", HD Digital VCR Conference, (December 1994), pages 27 and 84. It is contemplated that blocks of m×n dimensions may be used, where m is greater than or equal to 4 and n is greater than or equal to 4.
At step 505, a sum of each sum and corresponding difference coefficients are generated to get the coefficients of the even field. Referring to FIG. 6, blocks 600 and 602 are the original sum and difference coefficients, respectively. Block 605 shows the sum of the sum and corresponding difference coefficients e.g., X0+X4 of each column, where 0 represents row 0 and 4 represents row 4. It is preferred, in order to realize further time savings as 4-point IW/IDCTs are subsequently applied, that horizontally only the lower half of the sum and difference coefficients are summed.
At step 510 a one-dimensional horizontal 4-point IW/IDCT is applied to the lower half, in the present embodiment, four, coefficients. Block 610 contains the summed coefficients (identified by "A" variable) modified after application of the one-dimensional horizontal 4-point IW/IDCT. Preferably, the 4-point IW/IDCT used is the same as that utilized in the prior process and is represented by the butterfly diagram of FIG. 4a.
At step 515, a 4-point IW/IDCT is vertically applied four times to the lower half of the coefficients represented in block 610 to generate the pixel data ("B") shown in block 615. One example of a 4-point IW/IDCT vertically applied is represented in FIG. 7. The IW/IDCT applied differs from that earlier described as the weighting function specified for encoding and therefore the decoding process is slightly different for the two 4×8 block representations.
Block 620 represents the portion displayed 4×4 image portion generated. It should be noted that steps 505, 510 and 515 are not sequentially dependent; thus, for example, step 510 can be performed before step 505 and 515. Likewise, step 515 can be performed before steps 505 and 510. Step 515 can also be performed before 510 and after 505. Thus, the sequencing is interchangeable. Although the sequence can be changed, the sequence of operations affects the total number of computations required. For example, if step 510 is performed before step 505, the horizontal IW/IDCT is applied to the sum and difference coefficients (e.g., 8 rows of data) effectively doubling the number of computations.
It should be noted that the butterfly diagrams shown in FIGS. 4a, 4b and 7 can be represented a variety of ways. Examples are shown in FIG. 8. Furthermore, it is contemplated that the calculations performed in accordance with the butterfly functions shown can be scaled. The scale can be applied at any stage of the computations so long as the scaling is consistently applied to maintain the relationships among the outputs. For example, a scale factor can be applied at each input immediately prior to each output or at some common stage in between the inputs and outputs.
The IW/IDCT processes described in FIG. 2 through FIG. 8 can be represented by mathematical formulae shown in FIGS. 9a and 9b. For example, the equation 905 illustrates the computation for each block location (x,y) where P(x,y) is the pixel at that location and Q(h,v) is the weighted DCT coefficient at each location (h,v). Equation 905 corresponds to the IW/IDCT process applied to an 8×8 block, as described in FIG. 2, in which the ordering is the horizontal operation 906 (corresponding to e.g., step 205, FIG. 2) followed by the vertical operation 907 (corresponding to e.g., steps 210, 215, FIG. 2). Equation 910 represents another embodiment of a two dimensional implementation to generate a 1/4 image in which the vertical operation 911 is performed before the horizontal operation 912. Block 915 defines the parameters used to describe the equations 905, 910.
Similarly, FIG. 9b, specifically equations 920 and 925 represent embodiments of two-dimensional IW/IDCTs performed during the process described by FIG. 5. In equation 920, the vertical operation 921 (corresponding to e.g., steps 505, 515, FIG. 5) is initiated prior to the horizontal operation 922 (corresponding to e.g., step 510, FIG. 5) and in equation 925 the horizontal operation 926 (corresponding to, e.g., steps 505, 510) is initiated before the vertical operation 927 (corresponding to, e.g., step 515). The embodiments described implement one-dimensional IW/IDCTs (i.e., a horizontal IW/IDCT and a vertical IW/IDCT). However, as is illustrated above in FIGS. 9a and 9b, it is contemplated that the IW/IDCTs can be applied two-dimensionally.
The invention has been described in conjunction with the preferred embodiment. It is apparent that numerous alternatives, modifications, variations and uses will be apparent to those skilled in the art, in light of the foregoing description.
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A system and method to decode encoded video images in such a manner as to maintain high quality images while reducing the computation time needed to decode the images. The system takes into account that the resultant display generated may only have a fraction (1/4) of the resolution of the original image. Thus, optimizations are realized by modifying and combining the inverse discrete cosine transform (IDCT) and inverse weighting (IW) processes to process only the portion of the image to be displayed.
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FIELD OF THE INVENTION
The present invention relates to devices and methods for compensating for ground voltage elevations within an integrated circuit.
BACKGROUND OF THE INVENTION
Modern integrated circuits are required to operate at very high frequencies while consuming a relatively low supply voltage which has dramatically decreased during the last decade.
This supply voltage reduction has some drawbacks such as an increased sensitivity to ground voltage elevations that are proportional to a current (I) consumed by components of the integrated circuit and to the resistance (R) of grounding elements through which the current flows.
A ground voltage elevation can reduce the voltage that is provided to internal components of the integrated circuit, increase the noise level within the integrated circuit and thus can temporarily prevent the integrated circuit from operating in a proper manner.
There is a need to provide a device and method for efficiently compensating for ground voltage elevations.
SUMMARY OF THE PRESENT INVENTION
A device and a method for compensating for ground voltage elevations, as described in the accompanying claims.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be understood and appreciated more fully from the following detailed description taken in conjunction with the drawings in which:
FIG. 1 illustrates a device and voltage supply units according to an embodiment of the invention;
FIG. 2 illustrates various portions of an integrated circuit, according to an embodiment of the invention;
FIG. 3 is a schematic electric diagram of a compensation circuit as well as various equivalent components according to an embodiment of the invention; and
FIG. 4 is a flow chart of a method for compensating for a ground voltage elevation according to an embodiment of the invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The following figures illustrate exemplary embodiments of the invention. They are not intended to limit the scope of the invention but rather assist in understanding some of the embodiments of the invention. It is further noted that all the figures are out of scale.
According to various embodiments of the invention a method and device for compensating for ground voltage elevations are provided. The compensation can involve comparing the voltage at a sensing point to a voltage at a reference point and providing a source path to a negative voltage supply unit when a ground voltage elevation (especially of above a certain value) is detected. Conveniently, the compensation process is relatively fast, in comparison to the development of the ground voltage elevation.
FIG. 1 illustrates device 10 , and voltage supply units 44 and 48 according to an embodiment of the invention.
Device 10 can include one or more integrated circuits, can be connected to multiple voltage supply units, and can be a mobile device such as but not limited to a cellular phone, a laptop computer, a personal data accessory and the like.
For convenience of explanation only FIG. 1 illustrates device 10 as including integrated circuit 20 that is connected to positive voltage supply unit 44 and negative voltage supply unit 48 . It is noted that device 10 can include one or more of these voltage supply units, but this is not necessarily so.
According to an embodiment of the invention negative voltage supplied by negative voltage supply unit 48 is used by integrated circuit 20 only for ground voltage elevation compensation purposes, but this is not necessarily so. For example, the negative voltage can be used for additional purposes.
Positive voltage supply unit 44 provides a positive supply voltage Vcc 45 while the negative voltage supply unit 48 provides a negative supply voltage Vc 49 . Conveniently Vc 49 is supplied to one or more negative voltage supply inputs of integrated circuit 20 and Vcc 45 is supplied to one or more positive voltage supply inputs of integrated circuit 20 .
The value of Vcc 45 can substantially equal the absolute value of Vc 49 , but this is not necessarily so. For example, Vc 49 can be substantially lower than Vcc 45 .
Integrated circuit 20 includes multiple current consuming components (such as cores, cache memory units, DMA controllers) that can rapidly increase their current consumption thus causing ground voltage elevations.
Conveniently, multiple compensation circuits are located near current consuming elements that are connected to the ground grid through grounding elements which are expected to experience ground voltage elevations, and provide local compensation for local ground voltage elevations. The grounding elements can form one or more ground grids, as illustrated in FIG. 2 .
The provision of local compensation circuits that are relatively small and can be connected to one or more negative voltage supply inputs via relatively narrow (and hence relatively highly resistive) conductors reduces a die area penalty associated with the ground voltage elevation compensation scheme.
FIG. 2 illustrates various portions of an integrated circuit 20 , according to an embodiment of the invention.
Integrated circuit 20 includes multiple grounding elements that can form one or more ground grids. FIG. 2 illustrates a single ground grid 22 that includes multiple grounding elements that are represented by portions of the vertical and horizontal lines that represent a single ground grid. An ellipse surrounds grounding element 29 that connects reference point 33 ′ and sensing point 32 ′. It is noted that reference point 33 ′ is not necessarily connected to ground through pin 61 . Integrated circuit 20 also includes one or more power supply grids that are not shown for convenience of explanation. Ideally, the voltage level across the whole power grid is the same but in reality, due to the resistance of grounding elements that form ground grid 22 , the voltage level can differ from one grounding element to another, and thus local compensation circuits can be very effective.
Integrated circuit 20 also includes current consuming components such as cores 24 and 24 ′, peripherals (I/O pads etc.) 26 and memory units 28 and 28 ′.
Ground grid 22 is connected to one or more pins 61 that also can serve as a ground voltage reference point 33 .
Ground grid 22 is connected to core 24 , core 24 ′, memory unit 28 , memory unit 28 ′, and to peripherals 26 .
Two exemplary, non-limiting and out of scale sensing points 32 and 32 ′ are also illustrated. Sensing point 32 is positioned within the area of core 24 while sensing point 32 ′ is located within core 24 ′. It is noted that much more than a pair of sensing points can be defined within integrated circuit 20 . It is further noted that sensing points can be located within other components of the integrated circuit 20 as well as between components of the integrated circuit 20 . Each compensation circuit can detect the voltage potential between such a sensing point and a reference point that is expected to be less affected or not affected at all by the ground voltage elevation. The reference points can be located near pins 61 , especially between pins 61 and a decoupling capacitor (not shown).
Ground voltage elevations are formed when the current consumption of one or more of these components increases, and especially when the consumed currents are relatively high. Such an increase in current consumption is usually associated with complex computational tasks, memory transfer bursts and the like.
The multiple sensing points are selected such as to detect these ground voltage elevations. The selection is usually based upon a simulation of the integrated circuit. Designers are usually well aware of the possible current consuming components. Typically, more than one local compensation circuit is positioned such as to take care of a single core. In addition, the local compensation circuits can be placed at any distance from pins 61 .
FIG. 3 is a schematic electric diagram of a compensation circuit 90 as well as various grid components 71 , 72 , 73 , 74 , 76 , according to an embodiment of the invention.
Grid components include equivalent resistors 71 , 74 and 76 , equivalent capacitor 72 and current sink 73 that represent the resistances, capacitance and current consumption of various components of integrated circuit 20 .
Resistor 71 represents the (parasitic) resistance of a positive voltage supply element 44 that connects positive voltage supply input 62 to a certain internal point of integrated circuit 20 . Resistor 74 represents the resistance of grounding element 29 that is located between pin 61 (and reference point 33 ′) and sensing point 32 ′. Resistor 76 represents the resistance of a relatively highly resistive conductor that connects negative voltage supply input 63 to switch 89 of compensation circuit 90 . Capacitor 72 represents the equivalent capacitance of the integrated circuit as viewed between pin 61 and positive voltage supply input 62 . Current sink 73 represents the current consumption of one or more components of integrated circuit 20 , as viewed between pin 61 and positive voltage supply input 62 .
Capacitor 72 can represent a decoupling capacitor that is drained by excessive current that flows through grounding element 29 once the current consumption experiences a transient.
Compensation circuit 90 includes comparator 80 , switch 89 and a conductor that connects switch 89 to negative voltage supply input 63 . A non-inverting input 81 of comparator 80 is connected to sensing point 32 ′ (sensing point 32 ′ is graphically illustrated as being connected to the grounding element 29 adjacent to one end of capacitor 72 and one end of current sink 73 ). The other ends of capacitor 72 and current sink 73 are connected to the certain internal point of integrated circuit 20 . That certain internal point is connected to resistor 71 .
An inverting input 83 of comparator 80 is connected to ground voltage reference point (also referred to as reference point) 33 ′ that represents ground potential, which is not affected by the voltage elevation. Comparator 80 is connected in parallel to grounding element 29 thus is capable of detecting ground voltage elevation. It is noted that the detection can involve detecting a ground voltage elevation that exceeds a predefined value. A certain amount of current can flow through the grounding element 29 while causing ground voltage elevation, lower than the predefined level once a ground voltage elevation is detected, comparator 80 outputs a control signal via output 85 and opens switch 89 which is a MOSFET transistor. When switch 89 is opened, it connects the grounding element 29 to the negative voltage supply unit 48 (via negative voltage supply input 63 ) and allows input 63 to drain the excessive current. When switch 89 is opened it stops the discharge of capacitor 72 by providing the excess current drain path.
Conveniently, compensation circuit 90 is characterized by a response time that is relatively short in comparison to a development time of a substantially ground voltage elevation.
FIG. 4 is a flow chart of method 200 for compensating for a ground voltage elevation according to an embodiment of the invention.
Method 200 starts by optional stage 210 of defining or receiving a detection policy. The detection policy can mandate that the detection is performed in a continuous manner, according to a predefined detection pattern, in response to a reception of an alert that can represent expected current raise, and the like.
Each detection session can occur within a predefined measurement period, as well as within a dynamically changing measurement period. It is noted that the detecting can involve sampling the voltage developed over the grounding element.
Stage 210 is followed by stage 230 of detecting a ground voltage elevation resulting from a flow of excess current through a grounding element. Conveniently, the excess current flows through the grounding element due to an increment in a current consumption of a current consuming element of the device. Conveniently, the excess current is discharged through a decoupling capacitor.
Stage 230 is followed by stage 250 of connecting a negative voltage supply input to the grounding element in response to the detection.
Conveniently, stage 250 enables sinking of at least a portion of the excess current.
Conveniently, stage 250 includes connecting the negative voltage supply input via a relatively highly resistive conductor. The level of the negative supply voltage provided to the negative voltage supply input and a resistance of the relatively highly resistive conductor are designed to be matched such as to provide successful compensation and optimal overall circuit performance.
Conveniently, stage 250 of coupling includes closing a switch. Conveniently, the switch can be pulse width modulated. Conveniently, the switch is a transistor.
Conveniently, stage 250 at least partially reduces a discharge of a decoupling capacitor by the excess current.
Conveniently, various stages of method 200 can be executed concurrently by multiple compensation circuits that are mutually independent.
Stage 250 is followed by stage 270 of disconnecting the negative voltage supply from the grounding element. Stage 270 can be followed by stage 230 . Stage 250 can be followed by stage 270 once the compensation is completed. The compensation can be completed once a completion criterion is fulfilled. The completion criterion can relate to a reduction in the ground voltage elevation to an acceptable level.
Variations, modifications, and other implementations of what is described herein will occur to those of ordinary skill in the art without departing from the spirit and the scope of the invention as claimed. Accordingly, the invention is to be defined not by the preceding illustrative description but instead by the spirit and scope of the following claims.
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A method and a device, the device has ground voltage elevation compensation capabilities and includes: multiple current consuming components; a positive voltage supply input; a negative voltage supply input; and a compensation circuit, coupled to the negative voltage supply input and to a grounding element; wherein the compensation circuit is adapted to detect a ground voltage elevation resulting from a flow of excess consumption current through the grounding element, and in response couple the negative voltage supply input to the grounding element; wherein the excess current flows through the grounding element due to an increment in a current consumption of a current consuming element of the device.
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FIELD OF THE INVENTION
The present invention generally relates to devices designed to determine whether or not a flame, such as the flame of a pilot light, is present in a flame area. More specifically, the present invention relates to sensing the current conducted through a flame area to determine whether or not the current conducted is indicative of the presence of a flame.
BACKGROUND OF THE INVENTION
Many appliances, such as furnaces, use pilot lights for igniting the main burner of the appliance. For example, in a high efficiency furnace, a pilot light or igniting flame is ignited by a spark or electrically heated ignitor in response to a request for heat signal from a thermostat. This igniting flame provides the energy to ignite the fuel (e.g., natural gas) and air mixture at the combustion chamber of the furnace. However, it is important that the igniting flame is present before the fuel valve of the furnace is opened to provide fuel to the combustion chamber. Thus, the control system for the fuel valve must include a system for ensuring that an igniting flame is present when required to ignite the fuel-air mixture at the combustion chamber.
One way to sense the presence of a flame is to provide a voltage potential between two electrodes (e.g., flame hood and electrode near the tip of the flame), both located within a flame area (the area occupied by the ionized gases of a flame when a flame is present). The current flow within the flame area between the electrodes is monitored and will exceed a certain threshold when a flame is present due to the conductivity of the ionized gases in the flame area, By way of example, a typical furnace would apply 24 volts to the electrodes and a current of 50 or more nanoamps would indicate that a flame is present.
Electronics for accurately sensing currents in the range of 50 nanoamps can be relatively sensitive, since noise can substantially influence such sensing. Furthermore, circuits for flame current sensing in furnaces must be fail-safe for safety reasons. Accordingly, to provide reasonably priced fail-safe circuits for sensing flame current, circuits have been produced which only give a binary signal (flame present) based upon the presence or absence of a threshold flame current.
Flame current sensing circuits which only indicate that a flame is present or absent fulfill the primary need of flame detection; however, these circuits do not provide any information about the value of the flame current other than that it is above or below a setpoint.
For purposes of maintaining the electrodes of a flame current sensing circuit, and troubleshooting, it would be useful to have more information about the value of the flame current. For example, a typical problem with flame current sensing circuits is that the electrodes form a resistive layer over time due to oxidation and carbon deposits. When the resistance caused by such deposits becomes too great, the flame current is reduced and the circuit determines that a flame is not present, regardless of the presence of a flame, and prevents the furnace from operating. One solution to this problem is to clean the electrodes. However, this may only solve the problem temporarily if one or both of the electrodes were not sufficiently cleaned. Thus, it would be desirable to know how much the flame current exceeds the setpoint for purposes of checking electrode performance and predicting electrode cleaning schedules.
Accordingly, it would be useful to provide a simple, low-cost flame sensing circuit which could produce output signals representative of more than one flame current level and, preferably, output signals representative of a range of flame current levels.
SUMMARY OF THE INVENTION
The present invention provides for a flame detection circuit for detecting the presence of a flame between first and second electrodes. The impedance of the current path between the electrodes depends upon the presence of a flame between the electrodes, and with a given current supply, the current flow between the electrodes increases in the presence of a flame. The circuit includes a current sensing circuit coupled to the first and second electrodes. The current sensing circuit is configured to generate a first signal representative of a flame current above a first current level and a second signal representative of the flame current above a second current level greater than the first current level.
The present invention further provides a flame detection system. The system comprises an alternating current power source coupled to first and second electrodes and a signal generating circuit also coupled between the electrodes. The electrodes are disposed to rest within the flame of a furnace ignition device such as a pilot light. The signal generating circuit is configured to generate a first signal when the flame current exceeds a first predetermined amperage and a second signal when the flame current exceeds a second predetermined amperage, the first predetermined amperage being lower than the second predetermined amperage.
The present invention still further provides a flame detection system including a current amplifying circuit and a processor. The current amplifying circuit is coupled to an electrode disposed in the location of a pilot light flame, and generates an amplified current proportional to the flame current. The system also includes a capacitor coupled to the amplifying circuit and the processor. The capacitor is charged by the amplified current, where the rate of charge of the capacitor is proportional to the flame current and the voltage across the conductor increases at a rate proportional to the flame current. The processor is configured to discharge the capacitor when the voltage across the capacitor reaches a predetermined voltage, and measure a time required for the voltage across the capacitor to reach the predetermined voltage.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a circuit diagram for a first embodiment of a flame current sensing circuit usable within a furnace;
FIG. 2 is a graphical representation of a waveform plotted in the time and voltage domain; and
FIG. 3 is a circuit diagram for a second embodiment of a flame current sensing circuit.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1, a furnace 5 includes a flame current sensing circuit 10 which is coupled to a flame sensor (first electrode) 12 and a burner housing (second electrode) 14. Flame 16 emanates from housing 14. Electrode 12 is positioned so that when a flame 16 is present, electrode 12 is located within flame 16. Thus, flame 16 is in electrical contact with first and second electrodes 12 and 14, and the ionized gases of flame 16 reduce the resistance of the current path between electrodes 12 and 14 below the resistance of the path in the absence of a flame. In general, flame 16 is modeled as a resistance Rf and a diode Df. More specifically, flame 16 acts in part as a rectifying circuit, where the ratios of flame current in opposite directions along the current path in flame 16 are generally in the range of 1 to 5 depending upon the positioning of electrodes 12 and 14.
The present embodiment of circuit 10 is powered by the 24 VAC supply 18 of the type typically found in residential furnaces. Supply 18 includes a neutral lead 20 and a power lead 22. Lead 20 is coupled to electrode 14 and lead 22 is connected to electrode 12 by the series connection of a capacitor 24 and a resistor 26. The voltage of supply 18 was chosen since it is the voltage typically available at residential furnaces for use in furnace controls. However, depending upon the application the voltage of supply 18 may vary, and appropriate changes would be made in circuit 10 to accommodate such changes. For example, an advantage of increasing the voltage of supply 18 is that higher flame currents can be achieved, it typically being easier to monitor higher flame currents.
In addition to capacitor 24 and resistor 26, circuit 10 includes an LED 28, a resistor 30, an SCR 32, a resistor 34, a resistor 36, a microprocessor 38, a resistor 40, a transistor 42, a resistor 44, a diode 46, a resistor 48 and a capacitor 50. LED 28, resistor 30 and SCR 32 are connected in series between lead 22 and lead 20, where the anode of LED 28 is connected to lead 22 and the cathode of SCR 32 is connected to lead 20. The gate of SCR 32 is coupled to an I/O port 35 of processor 38 by resistor 34, and to lead 20 by resistor 36.
Resistor 40, transistor 42, diode 46 and capacitor 50 are connected in series between lead 22 and lead 20. In particular, the emitter of transistor 42 is connected to lead 22 by resistor 40, the collector is connected to the anode of diode 46 and the base is connected to the junction between capacitor 24 and resistor 26 by resistor 44. The cathode of diode 46 is connected to an I/O port 49 of processor 38 by resistor 48 and connected to lead 20 by capacitor 50. Processor 38 is grounded at lead 20.
By way of example only, processor 38 may be a Motorola XC68HC805C4CP, and the above-described components may have the following values:
______________________________________capacitor 24 .047 microfaradsresistor 26 4.7 MOhmsresistor 30 1.7 KOhmsresistor 34 4.7 KOhmsresistor 36 4.7 KOhmsresistor 40 470 KOhmsresistor 44 6.8 MOhmstransistor 42 PNP transistor with a gain greater than 100 at 1 microamp.resistor 48 2.2 KOhmscapacitor 50 .047 microfarads______________________________________
In general, circuit 10 operates to produce a voltage at capacitor 50 which increases with time at a rate generally proportional to the magnitude of the current passing from electrode 12 to electrode 14 (flame current). Processor 38 samples the status of port 49 once every cycle of the power source. For a 60 Hz power source, this would be once every 0.0167 seconds. If the status of port 49 goes from low to high (above 2 volts) within a predetermined number (N) of cycles (e.g. 8 cycles), processor 38 is programmed to determine that a flame is present between electrodes 12 and 14. In response, processor 38 will produce appropriate output signals applied to an associated fuel valve 52 which is coupled to a main burner 54 of furnace 5. This output signal causes valve 52 to open and the fuel at main burner 54 to be ignited by flame 16. After each N cycles, processor 38 controls port 49 to discharge capacitor 50.
In addition to the functions discussed above for processor 38, processor 38 is typically configured to control other functions of furnace 5, such as blower control.
One of the problems which is encountered with present electrodes 12 and 14 is an increase in surface resistance of the electrodes due to processes such as oxidation and carbon build up. When electrodes 12 and 14 develop a surface resistance which exceeds a particular threshold, circuit 10 will never sense a flame current regardless of whether a flame is present or not. Specifically, the surface resistance will be too high to allow sufficient current to flow through the flame to charge capacitor 50 within N cycles. As a result, the furnace associated with circuit 10 will not operate since processor 38 will not permit ignition of the main burner. A solution to this problem has been to clean electrodes 12 and 14. However, service personnel cannot typically determine how well the electrodes are cleaned. Accordingly, if electrodes 12 and 14 are marginally clean, the circuit 10 will sense a flame current and allow the furnace to operate for a short period of time until the surface resistance again increases beyond the threshold for sensing a flame current.
Circuit 10 is configured to determine more than just whether the flame current exceeds an acceptable minimum threshold which indicates with adequate certainty that a flame is present between electrodes 12 and 14. Circuit 10 also determines whether the flame current is above one or more amperage levels, and can provide an indication of the amount the flame current exceeds the minimum threshold. Accordingly, upon cleaning electrodes 12 and 14, a service person can operate the circuit 10 to determine whether or not the flame current is high enough to conclude that the electrodes have been adequately cleaned.
Referring to FIG. 2, the voltage across resistor 48 and capacitor 50 is graphically illustrated in reference to 16 cycles of AC power source 18, where processor 38 is programmed to discharge capacitor 50 every 8th cycle or on the cycle in which the signal at port 49 goes high, whichever occurs first. The generally truncated step shape of the voltage is the result of the use of an AC power source 18 and the circuit configuration which only allows charging of capacitor 50 during one-half of each cycle.
Curve 56 illustrates the increase in voltage across capacitor 50 over 8 cycles. Based upon curve 56, processor 38 will determine that the minimum threshold for flame current is met and that the flame current is at its lowest permitted level, since the full 8 cycles elapsed before the potential across resistor 48 and capacitor 50 reached the threshold of 2 volts. Curve 58 illustrates that the flame current is twice that of the threshold since only 4 cycles elapsed before the potential across resistor 48 and capacitor 50 reached the threshold of 2 volts. Circuit 10 is configured so that the time rate of Change of the voltage across capacitor 50 is a generally linear function for a substantially constant flame current. Accordingly, since the voltage across capacitor 50 is proportional to the flame current and the voltage is a linear function of time, the flame current is defined by the following function:
IF=K*8/M for M greater than 1 and less than or equal to 8;
where IF is the flame current, M is the number of cycles which elapse before the voltage across resistor 48 and capacitor 50 exceeds 2 volts, and K is a proportionality constant which is set based upon the flame current which is present when the potential across resistor 48 and capacitor 50 reaches 2 volts in eight cycles. For example, if a flame current of 50 nanoamps indicates that a flame is present, then K is 50 nanoamps. Thus, if processor 38 senses 2 volts at pin 49 in 2 cycles, the flame current is estimated at 200 nanoamps. Accordingly, this embodiment of circuit 10 produces flame current sensing at more than two levels or thresholds. More specifically, this embodiment provides M-1 flame current levels.
Referring now to the detailed operation of circuit 10, the resistance between electrodes 12 and 14 is typically above 100 Mohms when a flame is not present. In the absence of a flame, very little charge is accumulated on capacitor 24. Thus, transistor 42 remains non-conducting, and charge does not accumulate on capacitor 50. When a flame is present between electrodes 12 and 14, the charge on capacitor 24 goes above the forward voltage of transistor 42 (e.g. 0.6 volts) and base current will begin to flow. In response to the base current flow, a collector-to-emitter current will flow when lead 22 is positive. The collector-to-emitter current will cause a voltage drop across resistor 40 that will track changes in the charge of capacitor 24. During this time, the input impedance of transistor 42 will be approximately the product of the gain of the transistor and the value of resistor 40.
When lead 22 is negative, current flow does not occur through diode 46 or transistor 42. Therefore, the voltage on resistor 40 will not track the charge on capacitor 24. As a result, the input impedance of transistor 42 will be only the value of resistor 40 when the voltage on capacitor 24 is greater than 0.5 volts. Thus, the effective load on capacitor 24 will be the sum of resistors 40 and 44. Since resistor 44 has a much greater resistance than resistor 40, the load on capacitor 24 is the resistance of resistor 44 when lead 22 is negative and almost an infinite resistance when lead 22 is positive. Accordingly, the value of resistor 44 determines the amount of charge which accumulates on capacitor 24 for a given flame current. By way of example, based upon the present configuration of circuit 10, the voltage on capacitor 24 will be approximately the flame current IF times one-half the resistance of resistor 44.
When lead 22 is positive, transistor 42 operates as a constant current (I) source which charges capacitor 50, where the current I is defined by the following function:
I=(0.5*IF*R44-0.5)/R40,
where R40 and R44 are the resistances of resistors 40 and 44, respectively. When lead 22 is negative no current will flow, and the charging of C2 will be a ramp, followed by a constant voltage, followed by a ramp etc., as shown in FIG. 2.
As discussed above, when the voltage at port 49 exceeds a threshold (2 volts) within 8 cycles, processor 38 decides that a flame is present between electrodes 12 and 14. Upon the detection of a threshold voltage at port 49, or upon the occurrence of 8 cycles, whichever occurs first, processor 38 discharges capacitor 50. Resistor 48 is provided to protect processor 38 from excessive currents during the discharge of capacitor 50.
Circuit 10 is designed to include a number of features which make it fail-safe. One of these features is the programming of processor 38. In particular, the programming of processor 38 is completely run every cycle, where a cycle count is stored in processor 38 RAM. In the event that the program does not run error-free every cycle, the I/O ports which control the pilot light and main burner fuel valves are biased to cause these valves to close. Additionally, processor 38 is programmed to close all fuel valves if the voltage at port 49 reaches the threshold within one cycle, since it is assumed that such a charging rate at capacitor 50 is caused by a short in transistor 42. The failure of capacitor 50, either as an open circuit or short circuit, is also fail-safe in that in either mode of failure, the threshold voltage will not be produced at port 49 in the proper time period.
Referring to LED 28, processor 38 is programmed to drive port 35 high each time the threshold voltage is detected at port 49. Thus, the higher the flame current, the faster LED 28 will flash, and if the flame current is insufficient to charge capacitor 50 high enough within 8 cycles to produce the threshold voltage at 49, LED 28 will remain off. Further, processor 38 may be programmed to maintain SCR 32 conductive and thus keep LED 28 constantly illuminated as long as the threshold voltage at port 49 is obtained in a predetermined number of cycles less than 8, which indicates that the flame current is high enough to conclude that electrodes 12 and 14 are in good condition. Accordingly, LED 28 provides an indication of more than one flame current level in that it is constantly illuminated when the flame current is above a second level, it is flashed when the flame current is above a first level which is less than the second level, and it is off when the flame current is below the first level.
By way of modification, LED 28 may be replaced with an LCD display 29 and appropriate display driver coupled to processor 38. Display 29 would produce an alphanumeric display which would display the level at which the flame current was flowing. To refine the determination of the level of flame current, the frequency of sampling at port 49 could be increased by increasing the samples per cycle or the frequency of cycles.
In addition to producing an LED or LCD output representative of the level of flame current, processor 38 may be configured to communicate with other computers, and transmit data representative of the level of flame current to the other computers. For example, the main computer may utilize the flame current level data for the purpose of issuing a service message to the system operator. This message would be issued when the flame current is minimally above the threshold, but low enough to indicate that electrodes 12 and 14 may require servicing (e.g. cleaning) at the current time, or in the near future.
As a further modification to circuit 10, circuit 10 may be programmed to delay turning on main burner fuel valve 52 for a predetermined period of time (e.g. 5 or 10 seconds). This may be a desirable feature since the flame of burner 54 will alter the flame current when present and cause circuit 10 to sense an inaccurate flame current level. By providing the delay period, the circuit 10 has a period of time to accurately sense and display the flame current level. This feature is useful with certain indirect ignition applications.
A further modification of circuit 10 is shown in FIG. 3. In FIG. 3, the connection of the junction between the cathode of diode 46 and capacitor 50 is coupled to both port 49 and a second I/O port 60. Specifically, I/O port 60 is connected to port 49 by a resistor 62. In this embodiment, processor 38 is programmed to read port 49 at a given time period and determine whether or not a predetermined threshold voltage is exceeded. Processor 38 is also programmed to selectively ground port 60 during selected sampling of port 49. More specifically, when port 49 is above the predetermined threshold, port 60 is grounded to determine if port 49 remains above the predetermined threshold when the divider formed by resistors 48 and 62 is operative due to the grounding of port 60. Where the threshold is exceeded at port 49 when port 60 is not grounded, the flame current is considered to be minimally acceptable, but prompt servicing of electrodes 12 and 14 is advisable. If port 60 is grounded and port 49 is above the threshold, the flame current is considered to be sufficiently high to indicate that electrodes 12 and 14 are in good condition.
It will be understood that the above description is of the preferred exemplary embodiments of the invention, and that the invention is not limited to the specific forms shown. Various other substitutions, modifications, changes and omissions may be made in the design and arrangement of the elements of the preferred embodiment without departing from the spirit of the invention as expressed in the appended claims.
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A circuit for producing signals representative of at least two flame current levels is disclosed herein. The circuit includes two electrodes locatable in a flame, where a voltage potential is set up between the electrodes, and the current flow is measured therebetween (flame current). The circuit includes an amplifying portion for amplifying the flame current and applying a signal to a microprocessor. The microprocessor samples the signal and outputs a signal representative of the flame current level.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application No. 61/883,615, filed Sep. 27, 2013, hereby incorporated by reference in its entirety.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable.
THE NAMES OF THE PARTIES TO A JOINT RESEARCH AGREEMENT
Not applicable.
INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISC
Not applicable.
COPYRIGHT NOTICE AND PERMISSION
This document contains some material which is subject to copyright protection. The copyright owner has no objection to the reproduction with proper attribution of authorship and ownership and without alteration by anyone of this material as it appears in the files or records of the Patent and Trademark Office, but otherwise reserves all rights whatsoever.
BACKGROUND OF THE INVENTION
1. Technical Field
The present invention relates generally to methods and apparatus for controlled or regulated charging, discharging, or combined charging and discharging of power sources, such as batteries, and more particularly to where an internal such power source charges or operates an external second power source.
2. Background Art
In some manner, we have had electrical power stations nearly as long as we have had electrical power sources. Of present interest are electrical power stations that followed the addition of electrical starting and other electrical accessories in motor vehicles. Such power stations typically have had to meet the electrical requirements of their end application as well as be nominally portable to often be transported to such applications. For instance, a common application is to start an automobile where the owner has left the headlights on depleted the vehicle's battery. A power station suitable for this application must provide 12 volt direct current at sufficient amperes to operate the starter of the vehicle (typically while the vehicle's battery is still connected and presents an additional load as it recharges). Such a power station also usually must be portable to wherever a vehicle's owner parked when they left the headlights, typically a parking lot at their place of employment or at a store or restaurant.
The simplest power station for such an application is another vehicle that has a powerful enough battery, and a set of jumper cables. This simple solution, however, is not one that automotive and other service professionals are comfortable with. For example, a small service vehicle used to service large trucks in the field may not inherently come with or even be fit able with a large enough battery. Moreover, even when this can be done it is inefficient, in the small service vehicle when it is used for other tasks, and it is risky. Batteries become “weak” over time and use, and an aged or heavily used battery that starts a small service vehicle may embarrassingly not still be strong enough in a service application.
Most service professionals tend to prefer stand alone power stations. Historically, continuing mostly with automotive service scenarios but obviously extendable to aviation, nautical, and many other applications as well, a service profession would build or buy a power station with a large battery in an at least semi-portable housing, the a set of heavy cables terminated with suitable clams. In auto service stations one will frequently see such a power station today. It usually has two wheels, to permit easy limited movement, and it can be lifted into a service vehicle for field service calls.
Our society has increasingly come to rely on electrical power, and especially direct current power. Let us consider a few examples. Automobiles are now ubiquitous in some places, but so are cellular telephones and laptop computers. In fact many of us routinely use chargers for these devices that attach to a 12 volt DC power source in our automobiles. Many emergency and other specialty radios today can additionally be or are exclusively are powered with 12 VDC. Some televisions, small air compressors, lighting systems, and heating systems similarly can use 12 VDC. Ironically, an increasingly common electronic device today is power inverters, to convert 12 VDC to 120 or 240 volts, 60 cycle alternating current (AC) power.
Increasingly, people who are not service professionals, as well as ones who are but who want an appliance for personal use, are interested in power stations. These prospective new users want more than an expensive and awkward to handle box. They are willing to compromise on power to get economy, portability, and safety. Unlike service professionals, users here typically need a solution that can be stored between infrequent uses, that can be reliable when needed, and that is safe and easy. Thus, unlike professional service scenarios where lead technology batteries with their attendant their flammable hydrogen fumes, corrosive sulfuric acid, and expensive and environmentally threatening disadvantages may be manageable, a potential user here prefers a non lead-based power source or at least a very reliably sealed and storage-life optimized lead-based power source.
Moreover, these users typically have specific applications in mind and they want a power station that as flexibly as possible fulfills those applications as well as others that they may later encounter. These prospective new users often want sophistication in a power station. Many would like an air compressor and/or a power inverter integrated into a power station, but commercial offerings of such are not common.
Often unappreciated until needed, many such users (as well as many service professionals) would like a power station that provides lighting. There are only two basic ways hook two power sources, such as an automobile battery and a power station. When one cannot see what they are doing they will get it wrong 50% of the time, with great risk to safety and equipment. Service professionals appreciate this an strive to get it right, by also have a separate light source and using it (e.g., having an assistant hold a flash light, even if they have to wait for or go ask an assistant to do this). Lay users are not always so prepared in advance, or so patient, or will have read a power station's safety and usage instructions.
Accordingly, there is a growing market for economical power stations, but this market is not currently well served. Those who have tried to serve this market have tended to not study to scope of the market, and thus have tried to serve this market with offerings that retailers and end users find lacking.
Having mentioned retailers for the first time, let us consider their concerns. When a retailer has an adult in a suite or any adolescent buy a set of jumper cables the retailer cringes. In exchange for a relatively small profit, the retailer is taking a serious risk of litigation. Does an adult man or woman in a suit know how to work with lead-acid technology? For that matter does an adult in overalls know this? Has an adolescent enough life experience that a personal injury jury would find it reasonable to sell them jumper cables? Is such a retailer now willing to also stock and sell economical power stations? Clearly, such power stations must be as inherently safe and intuitively usable as possible.
Current economical-grade power stations offerings are jumper cables, already discussed at length; trickle chargers; and secondary battery-in-a-boxes. A trickle charger, in this context, is an AC powered battery charger. Its portability is limited to the length of extension cords that one can use to connect it to an AC power source. In general, trickle chargers put out such a small current (a “trickle) that connecting them incorrectly is relatively safe and at most damages the application or the trickle charger itself.
In contrast, a secondary battery-in-a-box is kludge, usually a minimalist make do solution. A battery-in-a-box is distinguishable from a professional-grade stand alone power station, and from the about to be disclosed invention, in that these other solutions are optimized for suitability for their anticipated users and their particular end applications. As the label “battery-in-a-box” implies, this usually consists of a box, often an ice chest or a container that markedly resembles one; a battery, very often a standard automotive lead-acid battery; and a set of cable clamps.
The ice-chest rebalance of battery-in-a-box devices can perhaps be attributed to a desire to evoke similar convenience in the minds of potential buyers. This is unfortunate, since a potential buyers should instead be considering if the device has drainage, if sulfuric acid exits the power source, or ventilation if hydrogen gas exits the power source. Potential purchasers of a battery-in-a-box are frequently enticed by claims of high power output and fast recharge ability, with these claims achieved by not “going cheap” on the standard automotive lead-acid battery and the charger used. This exacerbates sulfuric acid and hydrogen gas risks. Bigger battery-in-a-box devices often have wheels in the same manner as larger ice chests. Where manufactures of battery-in-a-box devices do sometimes do go cheap is on cable clamps. Copper is relatively expensive, hence savings can be had by using less of it. This can be done by using smaller gage wire in cables, providing shorter cables, and using little copper and more plastic in clamps.
Typically, battery-in-a-box devices are only a high current or ampere-hours solution, but the present inventor has recently observed one exception. Recently a Chinese-manufactured battery-in-a-box device has appeared in some U.S. automotive accessory stores that includes a 120/240 VAC power inverter.
BRIEF SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide a improved power station.
Briefly, a preferred embodiment of the present invention is an a power station suitable for portable use by a human user. Included is a current source, a light source, and a voltage source each having positive and negative polarity conductors. Further included is a control panel including controls to permit the user to selectively operate the current and light sources. A housing contains the sources and control panel, and is suitable to contain a main power source that has positionally fixed positive and negative power terminals. The housing has positionally fixed attachment posts to which the polarized conductors of the sources are electrically connected, and which is also suitable for electrical connection of the positive and negative power terminals of the main power source.
These and other objects and advantages of the present invention will become clear to those skilled in the art in view of the description of the best presently known mode of carrying out the invention and the industrial applicability of the preferred embodiment as described herein and as illustrated in the figures of the drawings.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING(S)
The purposes and advantages of the present invention will be apparent from the following detailed description in conjunction with the appended figures of drawings in which:
FIG. 1 is a schematic block diagram depicting how the functions of the portable modular power station are integrated together.
FIG. 2 is a perspective view of an exemplary power station in accord with the present invention.
FIG. 3 shows the control panel of the power station in FIG. 2 .
FIG. 4 shows the lighting panel of the power station in FIG. 2 .
FIG. 5 shows the back of the power station with the main power source being installed.
FIG. 6 also shows the back of the power station with some of the components of the control panel and the lighting panel being installed.
FIG. 7 shows the front of the power station with the rest of the control panel being installed.
FIG. 8 is an exploded view of the entire power station.
FIG. 9 is a cross-section view along section A-A in FIG. 2 .
FIGS. 10 a - b are schematic views showing how the same attachment posts can receive two alternated sizes of the main power source of the power station.
FIGS. 11 a - b are front and rear views, respectively, of an option module for use with the power station, here an air compressor module.
FIG. 12 shows how option modules are connected to the power station, in essence, being “piggy-backed” onto the back shell piece of the housing.
FIG. 13 is a stylized and basic schematic diagram of an electrical diagram for circuitry suitable for use in the inventive power station.
In the various figures of the drawings, like references are used to denote like or similar elements or steps.
DETAILED DESCRIPTION OF THE INVENTION
A preferred embodiment of the present invention is a portable modular power station. As illustrated in the various drawings herein, and particularly in the views of FIGS. 1-2 , wherein an embodiment of the invention is depicted by the general reference character 10 .
The present invention is termed a “portable modular power station” because it is portable (i.e., it can be easily moved about by a human adult) modularly assembled, yet provides a set of functions (functions 12 collectively and functions 12 a - d individually) that traditionally are found only in a stationary setting. For instance, the power station 10 may provide a heavy current sourcing function 12 a , a light sourcing function 12 b , an external device voltage sourcing function 12 c , and an optional module source function 12 d.
The current sourcing function 12 a of the power station 10 may particularly be used for jump starting vehicles and charging batteries, as well as for many other tasks that require high amperage direct current or high ampere-hours power. For instance, the power station 10 might be used to power heating cables wrapped around water pipes in a home during a cold spell or to power radio communications equipment in an emergency situation.
The light sourcing function 12 b of the power station 10 may be used for illumination and signaling. For instance, a very common problem when jump starting a vehicle is lack of illumination to correctly and safely connect jumper cables to the vehicle battery. Light as a signal can take many forms. Thus, for example, a user could set the power station 10 where it can be seen, say, to warn passing motorists to be cautious when driving by. Or a user could waive the power station 10 from side to side to both draw attention and to imply a safe direction for passing motorists to taken when driving by. Due to the already discussed high ampere-hours capability, the power station 10 can provide light for at least some hours.
The voltage sourcing function 12 c of the power station 10 include sourcing 12 VDC at a conventional automotive type accessory female plug (sometimes called a cigarette lighter plug) and sourcing 5 VDC at a conventional USB type-A female plug. The range of external devices that can be powered by or recharged from these two types of plugs and voltages is huge, including medium power devices like marine-band radios and low power devices like cellular telephones.
Finally, the module source function 12 d of the power station 10 can include any option that can use 12 VDC and for which there is a need. One embodiment described below includes an air compressor function. This permits inflating vehicle tires to their correct pressure, the repair of flats, inflating of inflatable boats, toys, etc. This can also be used as a source of compressed air for typical “shop uses,” such as blowing away dust, flushing sludge out of narrow hoses, etc. Another optional module for the power station 10 that the inventor is presently working on is a power inverter function, to convert 12 VDC to 120/240 VAC.
FIG. 1 is a schematic block diagram depicting how the functions 12 of the power station 10 are integrated together. The current sourcing function 12 a , light sourcing function 12 b , and voltage sourcing function 12 c are literally integrated within a housing 14 , whereas the optional module source function 12 d , when present, is physically attached to the exterior of the housing 14 .
FIG. 2 is a perspective view of an exemplary power station 10 in accord with the present invention. This power station 10 does not include an optional module source function, although one might be added. The major physical feature of the power station 10 is the housing 14 , that, in turn, has a front shell piece 16 , a back shell piece 18 , a handle unit 20 , and two base units 22 . The power station 10 here also has two large cable clamps 24 (a positive clamp 24 a and a negative clamp 24 b ) which are used in straightforward manner for the heavy current or power sourcing function.
As can also be seen in FIG. 2 , the front shell piece 16 of the housing 14 here includes a control panel 26 , a lighting panel 28 , and a face panel 32 . The control panel 26 permits a user of the power station 10 to controllably employ its features and to receive feedback about those features. The lighting panel 28 provides the lighting functionality of the power station 10 , and is controlled by the control panel 26 . The face panel 32 is a location where information about the power station 10 is typically put.
FIG. 3 shows the control panel 26 of the power station 10 in FIG. 2 . A rubber-like flip-up door 34 is provided to protect both an underlying automotive accessory plug 36 (a female plug able to source 12 VDC) and an underlying USB type-A plug 38 (a female plug able to source 5 VDC). A charge gauge 40 is provided to indicate the state of charge of the main power source inside the power station 10 . In the embodiment here the charge gauge 40 includes multiple light emitting diodes (LEDs) that are red, yellow, and two shades of green. Pressing a charge check button 42 completes a circuit with the charge gauge 40 and the main power source, permitting the LEDs to graphically and colorfully indicate the state of charge. A charging port 44 is provided to permit connection of an external charging unit (not shown) that can charge some versions of the main power source in straightforward manner. A lighting button 46 is provided to control the lighting panel 28 , discussed presently. And a main power switch 48 is provided to control connection of the terminals of the main power source to the cable clamps 24 .
FIG. 4 shows the lighting panel 28 of the power station 10 in FIG. 2 . Included here is a clear lens 52 that covers white-light LEDs 54 (three LEDs is preferred, but that quantity is not a limitation). Simple embodiments of the power station 10 can have the lighting button 46 permit toggling the white-light LEDs 54 on and off. More sophisticated embodiments can have the lighting button 46 permit cycling through the white-light LEDs 54 in various other useful manners.
FIG. 5 shows the back of the power station 10 with a main power source 56 being installed. As can be seen, the main power source 56 is contained fully in a compartment 58 in the back shell piece 18 of the housing 14 , behind a compartment door 60 . A subtle but very beneficial aspect of the power station 10 that can be appreciated here is that the main power source 56 is installed nearly last, after all of the other functional elements have been installed. Thus, all of the controls will have been installed into or inside of the housing 14 and the front shell piece 16 and the back shell piece 18 will have been assembled together before the main power source 56 is installed. This permits easy, modular, flexible, and robust assembly to be particular benefits of the power station 10 . A more detailed discussion of these benefits and the main power source 56 are provided, below.
FIG. 6 shows the back of the power station 10 with the handle unit 20 being installed. The handle unit 20 has end blocks 62 that engage with corresponding end openings 64 in the top of the front shell piece 16 . In a later assembly stage than shown in FIG. 6 (see e.g., FIG. 8 ), the back shell piece 18 which has similar end openings is added, thus capturing the end blocks 62 . When screws are inserted to attach the back shell piece 18 to the front shell piece 16 two such screws pass through the back shell piece 18 , into the end openings there, through the end blocks 62 of the handle unit 20 , into the end openings 64 of the front shell piece 16 , and part way into the front shell piece 16 . This particularly clamps the handle unit 20 securely in the finally assembled power station 10 .
FIG. 6 also shows the back of the power station 10 with some of the components of the control panel 26 and the lighting panel 28 being installed. The automotive accessory plug 36 and the USB type-A plug 38 are part of a device plug block 66 that is installed as a unit. Similarly, the main power switch 48 is installed as a unit. In alternate embodiments, the entire control panel 26 can be installed as a single pre-assembled a module. Two attachment posts 68 (a positive post 68 a and a negative post 68 b ) are also shown being installed here, and are discussed in more detail presently. Finally, the lighting panel 28 is installed here as a module.
FIG. 7 shows the front of the power station 10 with the rest of the control panel 26 being installed. Specifically, a cover plate block 72 is installed that will cover the device plug block 66 and the main power switch 48 . This cover plate block 72 also includes the flip-up door 34 , charge gauge 40 , charge check button 42 , charging port 44 , and lighting button 46 .
FIG. 8 is an exploded view of the entire power station 10 . In addition to providing a summary of aspects already discussed, the view here particularly helps to see some overall features of the power station 10 . For example, here it can be seen how the base units 22 engage over both the front shell piece 16 and the back shell piece 18 , to clamp and hold these together and thus make the overall housing 14 of the power station 10 much more robust. Returning briefly also to FIG. 7 , it can be seen that the front shell piece 16 has two wing pieces 74 (top wings 74 a ) and that the base units 22 each also have two wing pieces 74 (bottom wings 74 b ). When the power station 10 is not in use the cable clamps 24 each can have the cable portion wrapped around the wing pieces 74 and the clamp portion clamped onto a respective wing piece 74 , as shown (see also, FIGS. 2, 5 ).
Continuing with FIG. 8 , the use of screws in the final assembly of the power station 10 should be noted. Proceeding left to right, a first final screw set 76 comprises screws that attach the cover plate block 72 . A block screw set 78 comprises screws that assemble the cover plate block 72 , but at final assembly these are already installed as part of the cover plate block 72 . A third final screw set 80 comprises screws that attach the base units 22 to the front shell piece 16 and the back shell piece 18 of the housing 14 . Next to the right is a components screw set 82 that comprises screws that assemble components to the front shell piece 16 (for instance, the main power switch 48 ). At final assembly these are also already installed. A terminal screw set 84 comprises two screws, discussed in detail presently. A second final screw set 86 comprises screws to attach the back shell piece 18 to the front shell piece 16 . And a fourth final screw set 88 comprises screws to attach the compartment door 60 to the back shell piece 18 .
The block screw set 78 and the components screw set 82 will already be installed prior to final assembly. The first final screw set 76 will therefore typically be the first set of screws installed during final assembly. Then the back shell piece 18 and the front shell piece 16 are mated together and the second final screw set 86 is installed. The base units 22 are installed with the third final screw set 80 . Now, or at some later time, the main power source 56 is installed, with the terminal screw set 84 . And the compartment door 60 is mated with the back shell piece 18 and the fourth final screw set 88 is installed.
Next consider the orientation of the screws during assembly. The first final screw set 76 ultimately is at a downward angle relative to the power station 10 when finished, but during assembly the front shell piece 16 can simply be rotated as desired to facilitate installing the first final screw set 76 . Installing the block screw set 78 is even easier, since the cover plate block 72 can be rotated to face down and direct vertical and downward installation of the block screw set 78 can be used. The same manner of rotation to face down and direct vertical and downward installation of the components screw set 82 , terminal screw set 84 , second final screw set 86 , and fourth final screw set 88 can be employed. The installation of the third final screw set 80 (for the base units 22 ) then requires horizontal installation or another rotation.
FIG. 9 is a cross-section view along section A-A in FIG. 2 . Here a major safety feature of the power station 10 can be observed (see also, FIG. 5 ). The main power source 56 cannot be incorrectly installed (e.g., with the electrical polarity reversed). The main power source 56 has two power terminals 92 (a positive terminal 92 a and a negative terminal 92 b ) that are fixed in position. In particular, the terminals 92 a - b are much closer to the “front” of the main power source 56 . Inside the front shell piece 16 the attachment posts 68 are fixedly mounted in positions able to connect to the terminals 92 a - b only when they are close. Thus, for instance, putting the main power source 56 in “backwards” will result in the terminals 92 a - b being displaced away from and not being connectable with the attachment posts 68 . This is a substantial safety improvement over other systems that employ high-power automotive type batteries that can be incorrectly installed or incorrectly connected, e.g., due to the use of movable cables for connection.
FIGS. 10 a - b are schematic views showing how the same attachment posts 68 can receive two alternated sizes of the main power source 56 (shown in ghost outline). FIGS. 10 a - b show the same attachment posts 68 , and how they are mounted inside the front shell piece 16 ( FIG. 6 ) with mounting screws 94 holding them in place. The attachment posts 68 here are L-shaped brackets. Other shaped brackets may alternately be used, of course. For example, brackets that are L-shaped or angular in one plane but have a z-offset in another plane. The point in labeling these “posts” is to invoke a point like image of electrical connection points, one where positive electrical connection occurs and one where negative connection occurs. The attachment posts 68 each have wiring screws 96 that receive respective wires 98 , positive polarity wires 98 a to the positive post 68 a and negative polarity wires 98 b to the negative post 68 b . In keeping with the goal of modularity in the power station 10 , an effective minimum of wires 98 are employed (as described in more detail presently). The back shell piece 18 has openings that provide access from the compartment 58 to the attachment posts 68 , thus permitting connection of a main power source 56 to the attachment posts 68 with the terminal screw set 84 .
Continuing with the attachment posts 68 , the ones shown in the figures herein are nominally “L-shaped,” that is, they have the positions for the wiring screws 96 and the connection points 102 closer together rather than at opposed ends of I-shaped attachment posts 68 . This is not a requirement, for example, the attachment posts 68 could be straight (e.g., I-shaped or have another shape), but this L-shape permits an overall more compact construction of the power station 10 , as well as more subtle benefits like minimizing the areas of the openings from the compartment 58 to the interior of the power station 10 , etc.
In this manner the power station 10 can be fully assembled except for installation of the main power source 56 and closing the compartment 58 by installing the compartment door 60 with the fourth final screw set 88 . In particular, all operations related to installation, connection, disconnection, replacement, upgrade, etc. of the main power source 56 are compartmentalized.
The main power source 56 will typically be a 12 volt automotive type battery, but a one-use chemical power pack and fuel cells are potential alternates. The main power source 56 thus will necessarily require periodic access, and the power station 10 especially provides for and facilitates this in a manner that is easy and safe, and that does not require extensive disassembly (e.g., separating the front shell piece 16 and the back shell piece 18 , and/or tampering with other wiring or any internal parts).
FIG. 10 a shows a typical full or maximum size main power source 56 installed. One that will permit maximum capacity of the functions provided by the power station 10 . In contrast, FIG. 10 b shows a smaller size main power source 56 installed, with bridge bars 100 added. One that will provide a lesser capacity of the functions provided by the power station 10 . Embodiments of the power station 10 thus can be manufactured with one size of compartment 58 and be provided to end users with a variety of function capacities.
Many benefits are provided by this arrangement. The power station 10 can be manufactured and distributed without a main power source 56 installed. Then the party providing the power station 10 (e.g., a wholesaler providing to a retailer, or a retailer selling to an end user) can install a main power source 56 of a size and type as desired. One core model of the power station 10 can be stocked yet a variety of models can be provided to end users. Additionally, since the main power source 56 can be installed later, a larger single production run may be made and stocked without concern about the main power source 56 aging (i.e., discharging, degrading, corroding, etc.). A stock of the core power stations 10 can be keep for long periods, with fresh new main power sources 56 procured and installed only just before sale or use.
Another set of benefits peripherally relates to upgradability. A person can purchase a power station 10 with one type or size of the main power source 56 and easily change to another type or size of main power source 56 later. For instance, such a purchaser may be enticed by a lower price for a power station 10 that has a main power source 56 of the size (small) shown in FIG. 10 b , but then find that they use the power station 10 enough that they want the larger main power source 56 shown in FIG. 10 a . Or such a purchaser may obtain a power station 10 that has a main power source 56 that is a one-use chemical power pack, say, intending use only in an emergency, but find that they use their power station 10 enough that they want to install (upgrade to) a rechargeable 12 volt automotive type battery. Or a purchaser may obtain a power station 10 that has no optional modules (e.g., an air compressor module, power inverter module, high intensity lighting module, etc.) and then later purchase such a module and then also replace the original main power source 56 to one with a different type or size.
Another set of benefits relates to safety, both actual and perceived. As noted above in the discussion of FIG. 9 , the main power source 56 cannot be installed incorrectly. It cannot be installed with the electrical polarity reversed, which might damage the power station 10 itself or which could damage other equipment or injure a user. Thus, wholesalers, retailers, and end users can all handle the power station 10 safely and with confidence. The wholesalers and retailers can rest assured that any end user with the basic intelligence to avoid directly shorting two power terminals together should be able to safely handle maintenance and upgrade of the power station 10 with regard to the main power source 56 . And the end users can rest assured that their investment in the power station 10 can be long term and upgradeable, and that they themselves can perform maintenance and upgrades economically and safely.
Continuing with FIGS. 10 a - b , and summarizing, a key point of novelty in the power station 10 that permits its benefits is the modular and compartmentalized reduction of power routing between the main power source 56 and the rest of the power station 10 to simply two connection points 102 . This subtle aspect distinguishes the power station 10 over devices. Rather than have a hodge-podge of serial, parallel, and series-parallel wiring, forming a “rats-nest” that most end users would not dare to stick their hands into, the power station 10 keeps complexity in modules and has only minimal necessary complexity there. The compartmentalization of the main power source 56 is safe and minimally intimidating and the modularization of the overall power station 10 permits fast diagnosis and easy repair if any part of the power station 10 ever requires such.
FIGS. 11 a - b are front and rear views, respectively, of an option module for use with the power station 10 , here an air compressor module 104 . The air compressor module 104 is able to provide adequate pressure and volumetric capacity to inflate flat tires, inflatable boats, etc., or to provide pressurized air for many other uses. The air compressor module 104 here has an on/off switch 106 , a pressure gauge 108 , an air hose 112 with a nozzle 114 , and an accessory compartment 116 . The rear view ( FIG. 11 b ) particularly shows power wires 118 from the air compressor module 104 that will be connected to the power station 10 as wires 98 at the attachment posts 68 .
Of course, other optional modules may be constructed for use with the power station 10 . For example, the inventor is building a power inverter module to provide 120 and/or 240 volt alternating current (AC) that can be used to power many low to medium power AC devices, such as radios, televisions, hand power tools, etc. Another optional module might be a high intensity lighting module. Whereas the lighting panel 28 in most embodiments of the power station 10 is expected to provide 10-100 lumens of illumination, which is more than adequate for most tasks, an optional high intensity lighting module might provide 200-800 lumens and could additionally have a semi-rigid cable arm (sometimes termed a “goose neck” feature) that can be bend, wrapped, aimed, etc. as desired and to retain its position.
FIG. 12 shows how option modules are connected to the power station 10 , in essence, they are “piggy-backed” onto the back shell piece 18 of the housing 14 . The drawing, like FIGS. 5 and 8 , have so far shown the compartment door 60 in the back shell piece 18 as being plain, but the present inventor actually envisions that few instances of the power station 10 will have a plain compartment door 60 . Rather, it is expected that most instances of the power station 10 will be sold with an option module that uses the modified compartment door 60 a in FIG. 12 . As can be seen in FIG. 11 , the modified compartment door 60 a includes support and mounting holes for the air compressor module 104 and a hole 120 to permit the power wires 118 to be passed into the compartment 58 of the power station 10 and connected there to the attachment posts 68 .
FIG. 13 is a stylized and basic schematic diagram of an electrical diagram for circuitry suitable for use in the inventive power station 10 . The functions 12 , 12 a - 12 d , main power source 56 , controls and features 40 - 48 , and particularly the wires 98 , 98 a - b are shown. The modular nature of the power station 10 is stylistically emphasized here by how the wires 98 , 98 a - b connect at the two connection points 102 . As has been discussed herein, the use of only the two simple connection points 102 is more than just a coincidental matter. This promotes ease in manufacturing and repair, and particularly simplifies and increases safety in end user servicing.
While various embodiments have been described above, it should be understood that they have been presented by way of example only, and that the breadth and scope of the invention should not be limited by any of the above described exemplary embodiments, but should instead be defined only in accordance with the following claims and their equivalents.
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A portable power station including a current, light, and voltage sources as well as a control panel to permit a user to selectively operate the current and light sources. A housing contains the sources and is suitable to contain a main power source that has positionally fixed and polarized power terminals. The housing includes positionally fixed attachment posts to which the polarized conductors of the sources are electrically connected, and which are suitable for electrical connection of the polarized power terminals of the main power source.
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BACKGROUND OF THE INVENTION
[0001] Field of the Invention
[0002] This invention relates to optical apparatus, and in particular, it relates to a light source system, projection system and related methods.
[0003] Description of Related Art
[0004] Digital light processing (DLP) projection technology is gaining wide use, a core piece of which is digital micro-mirror device (DMD).
[0005] FIG. 1 a illustrates a conventional single chip DMD projection system. As shown in FIG. 1 , the system includes: excitation light source 100 , collection lens 101 , rotating color wheel 102 , light rod 103 , optical relay system 104 , DMD chip 105 , TIR (total internal reflection) prism 106 , and projection lens 107 . The excitation light source 100 is a semiconductor laser, and its emitted light is focused by the collection lens 101 onto the rotating color wheel 102 . The rotating color wheel 102 is coated with wavelength conversion materials (e.g. phosphors) on different color segments. FIG. 1 b is a plan view of the rotating color wheel with different color segments. As shown in FIG. 2 , a time sequence of three primary color lights red, green and blue is generated by the rotating color wheel 102 . The light is homogenized by the light rod 103 , and incident on the TIR prism 106 via the optical relay system 104 ; the light is reflected to the DMD chip 105 and modulated by it, and finally forms an output image by the projection lens 107 .
[0006] In conventional DMD projection system, the three primary color lights red, green and blue are inputted to the DMD sequentially in time, to be modulated; the monochromatic images are combined into a color image by the effect of persistence of vision of the human eyes. This system uses laser as the excitation light sources, which has the advantages of low etendue and high light efficiency. Conventional technology uses semiconductor laser devices to excite the different color segments of the color wheel to generate the red, green and blue primary lights. However, in this technology which uses semiconductor laser devices to excite phosphor materials in the color wheel, red phosphors have low conversion efficiency, leading to shortcomings in output image brightness and color gamut. This lowers the light efficiency and reliability of the system.
SUMMARY
[0007] Accordingly, the present invention is directed to a light source system, projection system and related methods which can improve the efficiency of red light generation, thereby improving the light efficiency and color saturation of the system.
[0008] To achieve these and/or other objects, the present invention provides a light source system, which includes:
[0009] a light source device, including least one group of excitation light sources generating an excitation light;
[0010] a light output device, which receives the excitation light and converts the excitation light to generate a converted light for output, wherein the light output device includes at least two different wavelength conversion materials, and wherein at least one of the wavelength conversion materials generates a converted light that is a multi-color light;
[0011] a light separation and combination device, which separates the multi-color light into a first light of a first wavelength range travelling along a first light path and a second light of a second wavelength range travelling along a second light path, wherein the first wavelength range and the second wavelength range are different, and wherein a combined light of all converted lights is a white light;
[0012] a first light modulation device, which modulates light that travels along the first light path; and
[0013] a second light modulation device, which modulates light that travels along the second light path.
[0014] Preferably, the converted light further includes a primary color light, wherein the light separation and combination device directs the primary color light to travel along the first light path of the second light path.
[0015] Preferably, the light output device is a color wheel, wherein the at least two different wavelength conversion materials are located on different segments of the color wheel.
[0016] Preferably, wherein the at least two different wavelength conversion materials absorb the excitation light from the light source device and emit at least two different multi-color lights. Preferably, the at least two different wavelength conversion materials are a cyan phosphor and a yellow phosphor, or a magenta phosphor and a cyan phosphor, or a magenta phosphor and a yellow phosphor.
[0017] Preferably, the light output device further comprises a multi-segment filter wheel which rotates coaxially with the color wheel, wherein the multi-segment filter wheel includes at least two different colored filter segments.
[0018] Preferably, the multi-segment filter wheel has a blue, a yellow and a green filter region, or a blue, a yellow and a red filter region, or a blue, a first yellow and a second yellow filter region.
[0019] Preferably, the light source device includes two groups of excitation sources.
[0020] Preferably, the light output device includes two color wheels respectively corresponding to the two groups of excitation light sources, wherein each color wheel has at least one wavelength conversion material, and wherein the wavelength conversion material of the two color wheels are non-identical.
[0021] Preferably, one of the two color wheels includes a blue or a cyan phosphor, and the other one includes a yellow phosphor and/or a green phosphor. Preferably, the light output device further includes: at least one multi-segment filter wheel which rotates coaxially with the color wheel, wherein the multi-segment filter wheel includes at least one different colored filter segments.
[0022] Preferably, the multi-segment filter wheel includes a yellow filter region and a green filter region.
[0023] Preferably, the two groups of excitation light sources are turned on and off alternatingly.
[0024] Preferably, the turn on time periods of one of the two groups of excitation light sources overlap with turn on time periods of the other one of the two groups of excitation light sources.
[0025] Preferably, two groups of excitation light sources are modulated by pulse width modulation.
[0026] Preferably, the light source system further includes a first filter plate and/or a second filter plate, where the first filter plate is disposed on a light path between the light separation and combination device and the first light modulation device, for filtering light travelling along the first light path, and wherein the second filter plate is disposed on a light path between the light separation and combination device and the second light modulation device, for filtering light travelling along the second light path.
[0027] In another aspect, the present invention provides a projection system, which includes: any of the above the light source system, and a projection lens, wherein the projection lens receives from the light source system the combined light after modulation, to form a projected image.
[0028] In another aspect, the present invention provides a projection method, which includes:
[0029] Providing at least one group of excitation light sources that emits an excitation light.
[0030] Receiving the excitation light, converting it to a converted light and outputting it, wherein the light output device includes at least two different wavelength conversion material, and wherein at least one of the wavelength conversion materials generates a converted light that is a multi-color light.
[0031] Separating the multi-color light into a first light of a first wavelength range travelling along a first light path and a second light of a second wavelength range travelling along a second light path, wherein the first wavelength range and the second wavelength range are different, and wherein the combined light of the converted lights is a white light.
[0032] Modulating light travelling along the first light path, and modulating light travelling along the second light path.
[0033] Conventional technologies use single DMD chip to simultaneously process the three primary color lights, or three DMD chips where each DMD processes a single primary color light. This way, the red, green and blue primary lights are input to the DMD in a time sequence to be modulated. The limitations of efficiency of red phosphors lower the output image brightness and reduces color gamut. In embodiments of the present invention, by exciting relatively high efficiency phosphors, a combined light containing two primary colors is generated, such as yellow light containing red light and green light; and then, using light separation method to distribute the two primary color lights to two DMDs for processing, the three primary color lights are distributed to two DMDs for processing. This way, the ratio of the three primary color lights can be adjusted, and the system can output multiple color lights including primary colors and intermediate colors. Thus, the color gamut of the light source is greatly increased, the light efficiency of the system is improved, the color gamut of the system is increased, and the cost is reduced.
BRIEF DESCRIPTION OF THE DRAWINGS
[0034] FIG. 1 a schematically illustrates the structure of a conventional single chip DMD projection system.
[0035] FIG. 1 b shows a plan view of rotating color wheel having different color segments in the conventional technology.
[0036] FIG. 2 schematically illustrates the structure of a light source system according to an embodiment of the present invention.
[0037] FIG. 3 schematically illustrates the structure of a projection system according to a preferred embodiment of the present invention.
[0038] FIG. 4 shows a plan view of a light output device of the embodiment of FIG. 3 .
[0039] FIG. 5 is a timing diagram showing the blue and yellow light sequence outputted from the light output device.
[0040] FIG. 6 illustrates the distribution of green and red lights after the light separation coating.
[0041] FIG. 7 a is a timing diagram of the reflected light from the first DMD.
[0042] FIG. 7 b is a timing diagram of the reflected light from the second DMD.
[0043] FIG. 8 shows a plan view of an improved light output device based on the projection system of the embodiment of FIG. 3 .
[0044] FIG. 9 is a timing diagram of the reflected light from the first DMD.
[0045] FIG. 10 is a timing diagram of the reflected light from the second DMD.
[0046] FIG. 11 shows a plan view of another improved light output device based o the projection system of the embodiment of FIG. 3 .
[0047] FIG. 12 a is a timing diagram of the reflected light from the first DMD.
[0048] FIG. 12 b is a timing diagram of the reflected light from the second DMD.
[0049] FIG. 13 a illustrates a color gamut.
[0050] FIG. 13 b illustrates another color gamut.
[0051] FIG. 14 schematically illustrates the structure of a projection system according to a preferred embodiment of the present invention.
[0052] FIG. 15 illustrates a color gamut.
[0053] FIG. 16 schematically illustrates the structure of a projection system according to a preferred embodiment of the present invention.
[0054] FIG. 17 shows a plan view of a light output device.
[0055] FIG. 18 is a timing diagram of the reflected light from the first and second DMDs when the light source devices are alternatingly turned on.
[0056] FIG. 19 shows a plan view of an improved light output device based on the projection system of the embodiment of FIG. 16 .
[0057] FIG. 20 is a timing diagram of the reflected light from the first and second DMDs when the light source devices are alternatingly turned on.
[0058] FIG. 21 is a timing diagram of the reflected light from the first and second DMDs when the turn on time of the light source devices are increased.
[0059] FIG. 22 is a timing diagram of the reflected light from the first and second DMDs when the light source devices are modulated using pulse width modulated.
[0060] FIG. 23 shows a plan view of an improved light output device based on the projection system of the embodiment of FIG. 16 .
[0061] FIG. 24 is a timing diagram of the reflected light from the first and second DMDs.
[0062] FIG. 25 is a flow chart showing a projection method according to a preferred embodiment of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0063] Embodiments of the present invention are described in detail below with reference to the drawings.
[0064] In conventional technologies, where a single DMD chip is used to simultaneously process the three primary color lights, or where three DMD chip are used where each DMD processes one of the three primary color lights, the red, green and blue lights are sequentially inputted to the DMDs for modulation. Limitations of the efficiency of the red phosphors decrease the output image brightness and reduce the color gamut.
[0065] Embodiments of the present invention use laser light to excite a phosphor having relatively high efficiency, to generate a converted light that contains two primary colors, such as a yellow light that contains red and green lights. Using a light separation method, the two primary color lights are separately inputted to two DMDs for processing. By distributing the three primary color lights according to desired ways to two DMDs for processing, the ratios of the three primary lights can be adjusted, which can achieve output of multiple colors including the primary colors and intermediate colors. Therefore, the color gamut that can be achieved is significantly increased, which increases the light efficiency of the system, increases the color gamut, and reduces cost.
First Embodiment
[0066] FIG. 2 schematically illustrates the structure of a light source system according to an embodiment of the present invention. As shown in FIG. 2 , the light source system includes: light source device 201 , light output device 202 , light separation and combination device 203 , first light modulation device 204 and second light modulation device 205 . The light source device 201 is a laser light source that generates at least one group of excitation light. The light output device 202 receives the excitation light and converts the excitation light to generate a converted light for output. The light output device includes at least two different wavelength conversion materials, and at least one of the wavelength conversion materials generates a converted light that is a multi-color light. The light separation and combination device 203 separates the multi-color light into a first light of a first wavelength range travelling along a first light path and a second light of a second wavelength range travelling along a second light path. The first light and second light cover different wavelength ranges, and the combined light of all converted lights is a white light. A multi-color light refers to a light that contains any two of the three primary colors. The primary lights include red light, green light and blue light. In this embodiment, a monochromatic light may be a primary color light; in other embodiment, it can be a monochromatic light of other wavelength ranges or a light having a certain spectral range. The first light modulation device 204 modulates the light that travels along the first light path, and the second light modulation device 205 modulates the light that travels along the second light path. The converted light also includes a primary color light, which is guided by the light separation and combination device 203 to travel along the first light path or the second light path.
[0067] In this embodiment, the light output device 202 is a color wheel, where at least two different wavelength conversion materials are respectively located on different segments of the color wheel. The two different wavelength conversion materials are wavelength conversion materials that absorb the excitation light and generate two different multi-color lights. These wavelength conversion materials, which absorb the excitation light from light output device 202 and generate two different multi-color lights, may be cyan phosphor and yellow phosphor, or magenta phosphor and cyan phosphor, or magenta phosphor and yellow phosphor.
[0068] More specifically, the multi-segment color wheel may be a two-segment color wheel having two different wavelength conversion materials. For example, the multi-segment color wheel may be a two-segment color wheel having a yellow segment and a blue segment, or a yellow segment and a cyan segment. The multi-segment color wheel may also be a three-segment color wheel having three different wavelength conversion materials. For example, the multi-segment color wheel may be a three-segment color wheel having a cyan segment, a green segment and a yellow segment. More specifically, when the light source is a blue laser source, the wavelength conversion materials that can absorb the excitation light from the light source and generate at least two multi-color lights may be a cyan phosphor and a yellow phosphor. When the light source is a UV source, the wavelength conversion materials that can absorb the excitation light from the light source and generate at least two multi-color lights may be a cyan phosphor and a yellow phosphor, a magenta phosphor and a cyan phosphor, or a magenta phosphor and a yellow phosphor. In this embodiment, because the yellow light may be separated to generate a red light and a green light, and the cyan light may be separated to generate a yellow light and a blue light, the wavelength conversion materials on the two-segment and three-segment color wheels are not limited to the color segments described above; as long as it can ultimately generate three primary color lights, all combinations are within the scope of this invention.
[0069] Further, to achieve a wider color gamut, the light output device 202 of this embodiment further includes: a multi-segment filter wheel which rotates coaxially with the color wheel, where the multi-segment filter wheel includes at least two different colored filter segments. For example, the multi-segment filter wheel may be one that has blue, yellow and green filter regions, or blue, yellow and red filter regions, or blue, first yellow and second yellow filter regions. The filter wheel is used to filter the output light generated by the multi-segment color wheel to obtain the three primary color lights including red, green and blue colors, thereby improving light efficiency and brightness.
[0070] Further, preferably, the light source device 201 includes two groups of excitation light sources. The light output device 202 includes two color wheels respectively corresponding to the two groups of excitation light sources. Each color wheel includes at least one wavelength conversion material, and the wavelength conversion materials of the two color wheels are not identical. Preferably, one of the two color wheels includes a blue phosphor, and the other one includes a yellow phosphor; or, one of the two color wheels includes a cyan phosphor, and the other one includes a yellow phosphor; or, one of the two color wheels includes a blue phosphor, and the other one includes a yellow and a green phosphor. The light output device 202 further includes at least one multi-segment filter wheel, which rotates axially with the color wheel, the multi-segment filter wheel including at least one different color filter region. The multi-segment filter wheel preferably includes a yellow filter region and a green filter region.
[0071] Further, preferably, the two groups of excitation light sources are alternatingly turned on and off, which improves the utilization efficiency of the first and second light modulation devices, and increases the brightness of the system. Or, the turn on time intervals of one of the two groups of excitation light sources partially overlap with the turn on time intervals of the other one of the two groups of excitation light sources. Or, the two groups of excitation light sources are modulated using pulse width modulation, which increases the color switching frequency, and can effectively solve the color breakup problem of projection display systems. In this embodiment, the light source system further includes a first filter plate and/or second filter plate, where the first filter plate is disposed on the light path between the light separation and combination device and the first light modulation device, for filtering the light travelling along the first light path, and the second filter plate is disposed on the light path between the light separation and combination device and the second light modulation device, for filtering the light travelling along the second light path. This can provide three purer primary color lights, and improve the light efficiency of the system.
[0072] In the light source system of this embodiment, by using at least one group of excitation light sources, the light output device sequentially outputs different lights based on the light of the excitation light sources. The light separation and combination device separates the different lights from the light output device into lights of different wavelength ranges which respectively travel along different light paths, and the light modulation devices modulate the different lights from the light separation and combination device that travel along the different light paths. This way, the three primary color lights can be distributed in specified ways to the two DMDs for processing, so that the color gamut of the system is greatly increased, and the light efficiency and reliability of the projection system is improved.
[0073] Improved projection systems based on the first embodiment, and their operating principles, are described below with reference to FIG. 3 to FIG. 24 . The second embodiment is an implementation based on modifying the wavelength conversion materials of the two-segment color wheel. The third embodiment is an implementation by changing the multi-segment color wheel from a two-segment color wheel to a three-segment color wheel. The fourth embodiment is an implementation that adds a three-segment filter wheel after a two-segment color wheel. The fifth embodiment is an implementation that adds filter plates before the light modulation devices. The sixth, seventh and eighth embodiments are implementations that add more excitation light sources and color wheel. The seventh embodiment is an implementation that adds more excitation light sources and color wheel, and further modifies the wavelength conversion materials of the color wheels. The eighth embodiment is an implementation that adds more excitation light sources and color wheel, and further modifies the turn on and turn off timing of the excitation light sources. The ninth embodiment is an implementation that changes the modulation method of the excitation light sources.
Second Embodiment
[0074] FIG. 3 schematically illustrates the structure of a projection system according to a preferred embodiment of the present invention. FIG. 4 shows a plan view of a light output device of the embodiment of FIG. 3 . FIG. 5 is a timing diagram showing the blue and yellow light sequence outputted from the light output device. FIG. 6 illustrates the distribution of green and red lights after the light separation coating. FIG. 7 a is a timing diagram of the reflected light from the first DMD. FIG. 7 b is a timing diagram of the reflected light from the second DMD. As shown in FIGS. 3 to 7 b , the projection system includes a light source system, which includes: light source device, light output device, light separation and combination device, first light modulation device and second light modulation device.
[0075] More specifically, the light source device includes: excitation light source (laser) 301 , and collection lens 302 . The light output device includes color wheel 303 . The light separation and combination device includes: light rod 304 , optical relay system 305 , TIR prism 306 , light separation and combination prism 307 and light separation film 310 . The first light modulation device includes a first DMD 308 a, and the second light modulation device includes a second DMD 308 b. Preferably, the projection system further includes a projection lens 309 .
[0076] More specifically, the excitation light source 301 may use a blue laser diode (LD). The blue light from the excitation light source 301 is focused by the collection lens 302 onto the color wheel 303 which is coated with phosphor materials. The color wheel 303 is a two-segment color wheel having a blue segment and a yellow segment, where the blue segment transmits the excitation light, and the yellow segment contains a yellow phosphor. Of course, the color wheel 303 may be a two-segment color wheel of other colors, such as a blue and cyan two-segment color wheel. The color wheel 303 outputs a blue light and a yellow light in a time sequence, as shown in FIG. 5 . The blue light and yellow light are homogenized by the light rod 304 , is collimated by the optical relay system 305 , and is then inputted to the TIR prism 306 and the light separation and combination prism 307 . A light separation film 310 is coated between the two prisms of the light separation and combination prism 307 . The light separation film 310 separates the yellow light in the input light into a red light and a green light. At the location of the light separation film 310 , one of the two lights is reflected and the other one is transmitted.
[0077] Thus, the light inputted to the first DMD 308 a and the second DMD 308 b are respectively green light, blue light and red light, or red light, blue light and green light. In other words, when the red light is reflected and the green light is transmitted, the light inputted to the first DMD 308 a is green light and blue light, as shown in FIG. 7 a , and the light inputted to the second DMD 308 b is red light, as shown in FIG. 7 b . Or, when the green light is reflected and the red light is transmitted, the light inputted to the first DMD 308 a is red light and blue light, and the light inputted to the second DMD 308 b is green light. The input lights are modulated by the first DMD 308 a and the second DMD 308 b, and are reflected and combined, and the combined light forms an image by the lens 309 .
Third Embodiment
[0078] FIG. 8 shows a plan view of an improved light output device of the projection system of the embodiment of FIG. 3 . FIG. 9 is a timing diagram of the reflected light from the first DMD. FIG. 10 is a timing diagram of the reflected light from the second DMD. As shown in FIGS. 8, 9 and 10 , compared to the second embodiment, this embodiment changes the color wheel of the second embodiment to a two-segment color wheel 303 a which has a cyan segment and a yellow segment, with other components remaining unchanged. The color wheel 303 a outputs a sequence of cyan light and yellow light, which is homogenized by the light rod 304 , collimated by the optical relay system 305 , and then inputted to the TR prism 306 and the light separation and combination prism 307 . A light separation film 310 is coated between the two prisms of the light separation and combination prism 307 . The light separation film 310 separates the yellow light in the input light into a red light and a green light, and separates the cyan light in the input light into a blue light and a green light. The blue light and the red light are inputted to one DMD (e.g. the first DMD 308 a ) for processing, as shown in FIG. 9 . The green light is inputted to the other DMD (e.g. the second DMD 308 b ) for processing, as shown in FIG. 10 . The input lights are modulated by the first DMD 308 a and the second DMD 308 b, and are reflected and combined, and the combined light forms an image by the lens 309 .
[0079] Compared to the second embodiment, in this embodiment, by using two DMDs, the cyan light is separated according to the time sequence to generate a green light, and the yellow light is separated according to the time sequence to generate a green light; this improves light utilization efficiency. Also, because the green component is enhanced, the brightness of the projection system is increased.
Fourth Embodiment
[0080] FIG. 11 shows a plan view of another improved light output device of the projection system of the embodiment of FIG. 3 . As shown in FIG. 11 , compared to the second embodiment, this embodiment adds a three-segment filter wheel 303 b that includes a blue, a green and a yellow segment, located downstream of the two-segment color wheel 303 that includes a blue and a yellow segment. The two-segment color wheel 303 and the three-segment filter wheel 303 b are mounted on the same rotation axis, and a common drive device is used to drive the two wheels to rotate synchronously. A part of the yellow light generated by the color wheel 303 is filtered by the green filter plate of the three-segment filter wheel 303 b into a green light, and another part of the yellow light is filtered by the yellow filter plate of the three-segment filter wheel 303 b and remains a yellow light. FIG. 12 a is a timing diagram of the reflected light from the first DMD. FIG. 12 b is a timing diagram of the reflected light from the second DMD. As shown in FIGS. 12 a and 12 b , in the light sequences from the two DMDs, two kinds of green light are obtained, so the three primary color lights now become four primary color lights of blue, green 1, green 2 and red. FIG. 13 a illustrates a color gamut. As shown in FIG. 13 a , the color gamut is increased.
[0081] Preferably, the green filter plate of the three-segment filter wheel may be changed to a red filter plate. Thus, red 1 and red 2 lights are obtained from the second DMD, thereby obtaining four primary color lights of blue, green, red 1 and red 2. Or, without adding the three-segment filter wheel 303 b, the two-segment color wheel 303 with blue and yellow segments may be changed to a two-segment color wheel with cyan and yellow segments, which can produce four primary color lights of blue, green 1, green 2 and red. Or, the two-segment color wheel 303 may be changed to a three-segment color wheel with blue, green and yellow segments, which can also produce four primary color lights of blue, green 1, green 2 and red. Or, still using the two-segment color wheel 303 with blue and yellow segments, the three-segment filter wheel 303 b is changed to a three-segment filter wheel having blue, yellow 1 and yellow 2 segments, to obtain two different yellow lights. Yellow 1 and yellow 2 lights are separated at the light separation and combination prism 307 into green 1, red 1, green 2 and red 2 lights, thereby obtaining five primary lights of blue, green 2, green 2, red 1 and red 2. FIG. 13 b illustrates another color gamut. As shown in FIG. 13 b , the color gamut obtained this way is broader. Or, without using the three-segment filter wheel 303 b, the two-segment color wheel 303 may be changed to a three-segment color wheel that includes cyan, green and yellow segments, to obtain five primary color lights if blue, green 1, green 2, green 3 and red. Or, the two-segment color wheel 303 may be changed to a three-segment color wheel that includes blue, yellow 1 and yellow 2 segments, which can also provide five primary colors of blue, green 1, green 2, red 1 and red 2.
[0082] It should be noted that the implementations of this embodiment are not limited to the above, and further modifications may be made. For example, by adding excitation light sources, changing the colors of various segments of the multi-segment color wheels, adding more DMDs, etc., multiple color output including primary colors and intermediate colors can be generated. More specifically, by increasing the color gamut that can be obtained from the excitation lights, a color gamut having more primary colors can be obtained, in order to satisfy requirements of various image standards and to enhance the color gamut of the system.
Fifth Embodiment
[0083] FIG. 14 schematically illustrates the structure of a projection system according to a preferred embodiment of the present invention. As shown in FIG. 14 , a first filter plate 1401 and a second filter plate 1402 are respectively provided in front of the two DMDs, and are respectively a green filter plate and a red filter plate. FIG. 15 illustrates a color gamut. As shown in FIG. 15 , after filtering of the green light and the red light by the first filter plate 1401 and the second filter plate 1402 respectively, the red light and green light inputted to the two DMDs are purer, thereby providing three primary colors with broader color gamut.
Sixth Embodiment
[0084] FIG. 16 schematically illustrates the structure of a projection system according to a preferred embodiment of the present invention. FIG. 17 shows a plan view of a light output device. This embodiment is based on the second embodiment, and changes the color wheel 303 to two color wheels including the first color wheel 1603 and the second color wheel 1604 . As shown in FIGS. 16 and 17 , the excitation light sources include an excitation light source 1601 and an excitation light source 1602 . In practice, the excitation light sources may be, for example, blue LD modules. FIG. 18 is a timing diagram of the reflected light from the first and second DMDs when the light source devices are alternatingly turned on. As shown in FIG. 18 , the turn on time periods of the excitation light source 1601 and the excitation light source 1602 correspond to the light sequence of the light output from the first DMD 308 a and the second DMD 308 b. The first excitation light source 1601 and the second excitation light source 1602 are alternatingly turned on; the blue light and red light are input to the first DMD 308 a, and the green light is input to the second DMD 308 b. The light output from the first excitation light source 1601 and the second excitation light source 1602 are focused by the collection lenses 302 onto the color wheel 1603 and the color wheel 1604 , respectively, as shown in FIG. 17 . The color wheel 1603 and the color wheel 1604 are respectively a single-segment blue light scattering wheel and a single-segment yellow phosphor wheel. The light output from the color wheels are respectively homogenized by the light rods 304 and collimated by the optical relay systems 305 , and inputted to a filter plate 1605 which transmits blue light and reflects yellow light, so that the blue light and the yellow light are combined by the filter plate 1605 . The combined light is input to the TIR prism 1606 , and then directed by the light separation and combination prism 1607 to the first DMD 308 a and the second DMD 308 b. The lights reflected by the DMDs are ultimately imaged via the projection lens 309 to form the image. Of course, this invention is not limited to the above; for example, the red light and the green light may be swapped.
Seventh Embodiment
[0085] FIG. 19 shows a plan view of an improved light output device of the projection system of the embodiment of FIG. 16 . As shown in FIG. 19 , this embodiment is based on the fifth embodiment, and changes the color wheel 1603 to a cyan phosphor color wheel 1603 a. The other components remain unchanged. FIG. 20 is a timing diagram of the reflected light from the first DMD 308 a and the second DMD 308 b when the light source devices are alternatingly turned on. As shown in FIG. 20 , the turning on times of the first excitation light source 1601 and the second excitation light source 1602 correspond respectively to the light sequences of the light from the first DMD 308 a and the second DMD 308 b. This method improves the utilization efficiency of the first DMD 308 a and the second DMD 308 b and increases the brightness of the system.
Eighth Embodiment
[0086] Based on the sixth and seventh embodiments, the eighth embodiment increases the turning on time duration of the first excitation light source 1601 , so that the first excitation light source 1601 and the second excitation light source 1602 are both turned on during certain time periods, i.e. they overlap. As a result, during the overlapping time periods, a multi-color light is obtained from the two DMDs which process the different multi-color lights; for example, blue and red lights can be combined into a magenta light, and blue and green lights can be combined into a cyan light. FIG. 21 is a timing diagram of the reflected light from the first DMD and the second DMD when the turning on time of the light source devices are increased. As shown in FIG. 21 , depending on whether the color wheel 1603 is a single-segment blue color wheel or a single-segment cyan color wheel, the time sequence of the output light from the second DMD 308 b has two situations. During the time period when both excitation light sources are turned on, the combined light formed by the lights from the two DMDs is a combined light of magenta and green, or a combined light of cyan and red, both of which result in a white combined light. This greatly increased the brightness of the system.
Ninth Embodiment
[0087] Based on the sixth and seventh embodiments, the ninth embodiment treats the lights output by the pair of color wheels, i.e. blue light and yellow light respectively outputted by the single-segment blue color wheel and the single-segment yellow color wheel, or cyan light and yellow light respectively outputted by the single-segment cyan color wheel and the single-segment yellow color wheel, as two light sources, and applies pulse width modulation (PWM) to their excitation light sources. FIG. 22 is a timing diagram of the reflected light from the first and second DMDs when the light source devices are modulated using pulse width modulated. As shown in FIG. 22 , the pulse sequences of the first excitation light source 1601 and the second excitation light source 1602 correspond respectively to the light sequences of the light from the first DMD 308 a and the second DMD 308 b. Using PWM can increase the switching frequency between the different colors, and can effectively solve the color breakup problem of projection display systems.
Tenth Embodiment
[0088] Based on the sixth embodiment, the tenth embodiment changes at least one of the two single-segment color wheels to a multi-segment color wheel. FIG. 23 shows a plan view of an improved light output device of the projection system of the embodiment of FIG. 16 . As shown in FIG. 23 , this embodiment uses a two-segment color wheel 1604 a that has a yellow segment and a green segment, and a single-segment blue color wheel 1603 . FIG. 24 is a timing diagram of the reflected light from the first DMD 308 a and second DMD 308 b. FIG. 24 shows the turn on sequences of the two excitation light sources and the corresponding light sequences of the two
[0089] DMD. This embodiment is not limited to this particular design of color wheels; any color wheel design is within the scope of this embodiment so long as: it provides three primary colors, i.e. of the two DMDs, one DMD processes one primary color and the other DMD sequentially processes the other two primary colors, and it allows combination of colors during some time periods, such as combining blue and red lights into magenta light, or combining blue and green lights into cyan light.
[0090] Further, this embodiment is not limited to using multi-segment color wheels; it can also use a single-segment color wheel, or a two-segment or a multi-segment color wheel, and add a filter wheel that rotates synchronously with the color wheel. This can also meet the above conditions of providing three primary color lights to two DMDs. In this embodiment, either or both of the single-segment color wheels can be changed to multi-segments color wheels, so the embodiment may use a combination of a two-segment color wheel and a single-segment color wheel, or a combination of two two-segment color wheels, etc. All of such combinations are within the scope of this embodiment. This embodiment can ensure brightness and at the same time ensure a broad color gamut.
Eleventh Embodiment
[0091] FIG. 25 is a flow chart showing a projection method according to a preferred embodiment of the present invention. As shown in FIG. 25 , the method includes:
[0092] Step S 1011 : Providing at least one group of excitation light sources (laser sources) that emits an excitation light.
[0093] Step S 1012 : Receiving the excitation light, converting it to a converted light and outputting it, wherein the converted light includes at least one multi-color light.
[0094] Step S 1013 : Separating the multi-color light into a first light of a first wavelength range travelling along a first light path and a second light of a second wavelength range travelling along a second light path, wherein the first wavelength range and the second wavelength range are different, and wherein the combined light of the converted light is a white light.
[0095] Step S 1014 : Modulating the light travelling along the first light path, and modulating the light travelling along the second light path.
[0096] In the projection method according to this embodiment, by providing at least one group of excitation light sources, the light output device sequentially outputs different lights based on the excitation light emitted by the excitation light sources. The light separation and combination device separates the different lights from the light output device into lights of different wavelength ranges travelling along different light paths. The light modulation devices modulate the different lights from the light separation and combination device that travel along different light paths. This way, the three primary color lights are distributed to two DMD for processing, which increases the color gamut of the light source system and improves the light efficiency and reliability of the system.
[0097] It will be apparent to those skilled in the art that various modification and variations can be made in the light source system and related method of the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention cover modifications and variations that come within the scope of the appended claims and their equivalents.
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A light source system including: a light source device emitting excitation light; an light output device receiving the excitation light and converting it into converted light, wherein the light output device includes at least two different wavelength conversion materials, the converted light of at least one wavelength conversion material being a multi-color light; a light splitting and combining device splitting the multi-color light into a first and a second color light propagating respectively along a first and a second optical channel, wherein the first and second color lights have different wave spectrum coverage ranges; and a first and a second light modulation device respectively modulating the light propagating over the first and second optical channels, wherein the light of three primary colours can be allocated to two DMDs for processing. This results in improved colour gamut of the light source and the light efficiency and reliability of the system.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present invention is a continuation-in-part of U.S. application Ser. No. 12/109,766 filed on Apr. 25, 2008 entitled “THERMAL TREATMENT OF TRIGLYCERIDES”, which is hereby incorporated by reference in its entirety.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] None.
FIELD OF THE INVENTION
[0003] The present invention relates generally to the thermal cracking of impurities in triglyceride feedstock and the conversion of such feedstock to fuel range hydrocarbons.
BACKGROUND OF THE INVENTION
[0004] There is a national interest in the discovery of alternative sources of fuels and chemicals, other than from petroleum resources. As the public discussion concerning the availability of petroleum resources and the need for alternative sources continues, government mandates will require transportation fuels to include, at least in part, hydrocarbons derived from sources besides petroleum. As such, there is a need to develop alternative sources for hydrocarbons useful for producing fuels and chemicals.
[0005] One possible alternative source of hydrocarbons for producing fuels and chemicals is the natural carbon found in plants and animals, such as for example, oils and fats. These so-called “natural” carbon resources (or renewable hydrocarbons) are widely available, and remain a target alternative source for the production of hydrocarbons. For example, it is known that oils and fats, such as those contained in vegetable oil, can be processed and used as fuel. “Bio Diesel” is one such product and may be produced by subjecting a base vegetable oil to a transesterification process using methanol in order to convert the base oil to desired methyl esters. After processing, the products produced have very similar combustion properties as compared to petroleum-derived hydrocarbons. However, the use of Bio-Diesel as an alternative fuel has not yet been proven to be cost effective. In addition, Bio-Diesel often exhibits “gelling” thus making it unable to flow, which limits its use in pure form in cold climates.
[0006] Unmodified vegetable oils and fats have also been used as additives in diesel fuel to improve the qualities of the diesel fuel, such as for example, the lubricity. However, problems such as injector coking and the degradation of combustion chamber conditions have been associated with these unmodified additives. Since cetane (C 16 H 34 ), heptadecane (C 17 H 36 ) and octadecane (C 18 H 38 ) by definition have very good ignition properties (expressed as cetane rating), it is often desired to add paraffinic hydrocarbons in the C 16 -C 18 range, provided that other properties of the additive (such as for example, viscosity, pour point, cloud point, etc.,) are congruent with those of the diesel fuel). Processes for converting vegetable oil into hydrocarbons have been achieved, such as, for example, contacting a diesel/vegetable oil mixture with a hydrotreating catalyst. However, oftentimes, vegetable oils can contain significant amounts of impurities such as such as phospho-lipids, proteins, gums, and other metal containing compounds (such as alkali metals, alkaline earth metals). These impurities can cause catalyst deactivation and plugging of the reactor catalyst bed.
[0007] As such, development of a new and simple process for removing impurities such as phospho-lipids, proteins, gums, metal containing compounds (such as alkali metals, alkaline earth metals) from vegetable oils would be a significant contribution to the art.
SUMMARY OF THE INVENTION
[0008] In one embodiment of the present invention, there is a process disclosed comprising thermal cracking a triglyceride feedstock in a thermal cracking zone wherein the temperature in the thermal cracking is in the range of from about 100° C. to about 540° C. to form a thermally cracked feedstock.
[0009] In another embodiment of the present invention, there is a process disclosed comprising passing a feedstock mixture comprising a hydrocarbon boiling in the temperature range of from about 25° C. to about 760° C. and a triglycerides feedstock through a thermal cracking zone, wherein the temperature in the thermal cracking zone is in the range of from about 100° C. to about 540° C.
[0010] In yet another embodiment of the present invention, a process is disclosed comprising contacting the thermally cracked feed from any one of the previous embodiments with a hydrotreating catalyst in a reaction zone under a condition sufficient to produce a reaction product containing diesel boiling range hydrocarbons, wherein the condition includes a pressure of less than about 2000 psig and a temperature in the range of from about 260° C. to about 430° C.
[0011] In accordance with the current disclosure, the triglycerides feedstock is selected from the group consisting of vegetable oil, soybean oil, yellow grease, animal fats and mixtures thereof.
[0012] In accordance with the current disclosure, the triglycerides feedstock further comprises elements selected from the group consisting of phospho-lipids, proteins, gums, metal containing compounds (such as, alkali metals, alkaline earth metals), and combinations thereof.
[0013] In accordance with the current disclosure, the hydrocarbon is selected from the group consisting of gasoline, naphtha, jet fuel, kerosene, diesel fuel, light cycle oil, vacuum gas oil, atmospheric gas oil, atmospheric tower bottom, and combinations of any two or more thereof.
[0014] The major advantage of this invention is the ability to clean the feedstock in situ. This ability allows the use of a variety of low cost feedstock and reduce reactor fouling tendency. The process also reduces the use of chemicals required for conventional clean up processes such as degumming
[0015] Other objects, advantages and embodiments of the invention will be apparent from the following detailed description of the invention and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] None
DETAILED DESCRIPTION OF THE INVENTION
[0017] Turning now to the detailed description of the embodiments of the present invention. It should be understood that the inventive features and concepts may be manifested in other arrangements and that the scope of the invention is not limited to the embodiments described or illustrated. The scope of the invention is intended only to be limited by the scope of the claims that follow.
[0018] Triglycerides or fatty acids of triglycerides, or mixtures thereof, may be converted to form a hydrocarbon mixture useful for liquid fuels and chemicals. The term, “triglyceride,” is used generally to refer to any naturally occurring ester of a fatty acid and/or glycerol having the general formula CH 2 (OCOR 1 )CH(OCOR 2 )CH 2 (OCOR 3 ), where R 1 , R 2 , and R 3 are the same or different, and may vary in chain length. Vegetable oils, such as for example, canola and soybean oils contain triglycerides with three fatty acid chains. Useful triglyceride feedstock in the present invention include, but are not limited to, triglycerides that may be converted to hydrocarbons when contacted under suitable reaction conditions. Examples of triglycerides useful in the present invention include, but are not limited to, vegetable oils including soybean and corn oil, peanut oil, sunflower seed oil, coconut oil, babassu oil, grape seed oil, poppy seed oil, almond oil, hazelnut oil, walnut oil, olive oil, avocado oil, sesame, oil, tall oil, cottonseed oil, palm oil, ricebran oil, canola oil, cocoa butter, shea butter, butyrospermum, wheat germ oil, illipse butter, meadowfoam, seed oil, rapeseed oil, borange seed oil, linseed oil, castor oil, vernoia oil, tung oil, jojoba oil, ongokea oil, algae oil, jatrothea oil, yellow grease (for example, as those derived from used cooking oils), and animal fats, such as poultry grease, beef fat (tallow), and milk fat, and the like and mixtures and combinations thereof.
[0019] Triglyceride Feedstock may be processed alone or in combination with other hydrocarbons. The hydrocarbons generally boil at a temperature of from about 25° C. to about 760° C. Examples of suitable hydrocarbons include middle distillate fuels. Middle distillate fuels generally contain hydrocarbons that boil in the middle distillate boiling range in the range from about 150° C. to about 400° C. Typical middle distillates may include for example, jet fuel, kerosene, diesel fuel, light cycle oil, atmospheric gas oil, and vacuum gas oil. If a middle distillate feed is employed in the process of the present invention, the feed generally may contain a mixture of hydrocarbons having a boiling range (ASTM D86) of from about 150° C. to about 400° C. In addition, the middle distillate feed may have a mid-boiling point (ASTM D86) of greater than about 175° C.A middle distillate feed employed in one embodiment of the present invention is diesel fuel. In addition, one or more triglycerides can mix with a middle distillate feed.
[0020] In addition to middle distillate fuels, other suitable hydrocarbons include, but are not limited to, gasoline, naphtha, and atmospheric tower bottom.
[0021] Generally, the hydrocarbon can contain a quantity of sulfur. The amount of sulfur in the hydrocarbon can generally be greater than about 20 parts per million by weight (ppmw) sulfur. In one embodiment of the present invention, sulfur is present in an amount in the range of from about 100 ppmw to about 50,000 ppmw sulfur. In another embodiment of the present invention, sulfur is present in the range of from about 150 ppmw to 4,000 ppmw. As used herein, the term “sulfur” denotes elemental sulfur, and also any sulfur compounds normally present in a hydrocarbon stream, such as diesel fuel. Examples of sulfur compounds which may be contained in the hydrocarbon through in the present invention include, but are not limited to, hydrogen sulfide, carbonyl sulfide (COS), carbon disulfide (CS) mercaptans (RSH), organic sulfides (R—S—R), organic disulfides (R—S—S—R), thiophene, substituted thiophenes, organic trisulfides, organic tetrasulfides, benzothiophene, alkyl thiophenes, dibenzothiophene, alkyl benzothiophenes, alkyl dibenzothiophenes, and the like, and mixtures thereof as well as heavier molecular weights of the same, wherein each R can be an alkyl, cycloalkyl, or aryl group containing 1 to about 10 carbon atoms.
[0022] Generally, the triglyceride feedstock may be present in an amount in the range of from about 0.1 to about 99.9 percent, based on the total weight percent of the feed. The triglyceride feedstock can also be present in an amount in the range of from about 50 weight percent to about 99.9 weight percent based on the total weight of the mixture. The triglyceride feedstock can also be present in the feed in an amount of 100 weight percent.
[0023] Generally, the triglyceride feedstock contains amounts of impurities. The elements that the triglyceride contains are generally selected from the group consisting of phospho-lipids, proteins, gums, metal containing compounds (such as alkali metals, alkaline earth metals), and combinations thereof. The amounts of these compounds are generally in the range of from about 0 ppmw to about 10,000 ppmw.
[0024] The degumming of triglycerides involves contacting the triglycerides with a water wash. In the present invention, the triglycerides can either be degummed or not degummed prior to being thermal cracked in the thermal cracking zone.
[0025] In one embodiment of the present invention, the triglyceride feedstock or its mixture with hydrocarbon may be contacted with a co-feed gas in the thermal cracking zone. Generally, the co-feed gas is selected from the group consisting of hydrogen, nitrogen, helium, carbon monoxide, and carbon dioxide. In one embodiment, the co-feed gas can be hydrogen or nitrogen.
[0026] The processes according to various embodiments of the present invention comprises thermal cracking a triglyceride feedstock only or in the mixture of hydrocarbon feed in a thermal cracking zone to form a thermally cracked feed.
[0027] Thermal cracking process generally refers to heating a material in the absence of oxygen or air. Thermal cracking generally results in decomposition of thermally unstable components of the feedstock in this case these are the impurities such as phospho-lipids, proteins, gums, and other metal containing compounds. The thermally unstable material decomposes and deposits in the thermal cracking zone and leaves cleaner triglycerides unaffected and hence suitable for further reaction in downstream equipment
[0028] The temperature in the thermal cracking zone is generally in the range of from about 100° C. to about 540° C. The temperature in the thermal cracking zone can also be in the range of from about 120° C. to about 430° C., and the temperature in the thermal cracking zone can also be in the range of from about 200° C. to about 400° C.
[0029] Generally, a thermally cracked feed from any one of the previous embodiments can be contacted with a catalyst composition under a condition sufficient to produce a reaction product containing diesel boiling range hydrocarbons. Useful catalyst compositions in the present invention include catalysts effective in the conversion of triglycerides to hydrocarbons when contacted under suitable reaction conditions. Examples of suitable catalysts include hydrotreating catalysts. The term “hydrotreating” as used herein, generally describes a catalyst that is capable of utilizing hydrogen to accomplish saturation of unsaturated materials, such as aromatic compounds. Examples of hydrotreating catalysts useful in the present invention include, but are not limited to, materials containing compounds selected from Group VI and Group VIII metals, and their oxides and sulfides. Examples of hydrotreating catalysts include but are not limited to alumina supported cobalt-molybdenum, nickel sulfide, nickel-tungsten, cobalt-tungsten and nickel-molybdenum.
[0030] The metal of the catalyst useful in the present invention is usually distributed over the surface of a support in a manner than maximizes the surface area of the metal. Examples of suitable support materials for the hydrogenation catalysts include, but are not limited to, silica, silica-alumina, aluminum oxide (Al 2 O 3 ), silica-magnesia, silica-titania and acidic zeolites of natural or synthetic origin. The metal catalyst may be prepared by any method known in the art, including combining the metal with the support using conventional means including but not limited to impregnation, ion exchange and vapor deposition. In an embodiment of the present invention, the catalyst contains molybdenum and cobalt supported on alumina or molybdenum and nickel supported on alumina
[0031] This process in accordance with an embodiment of the present invention can be carried out in any suitable reaction zone that enables intimate contact of the thermally cracked feed and control of the operating conditions under a set of reaction conditions that include total pressure, temperature, liquid hourly space velocity, and hydrogen flow rate. The catalyst can be added first to the reactants and thereafter, fed with hydrogen. If desired, the thermally treated feed can pass through a filter before passing to the reaction zone. In the present invention, either fixed bed reactors or fluidized bed reactors can be used. As used herein, the term “fluidized bed reactor” denotes a reactor wherein a fluid feed can be contacted with solid particles in a manner such that the solid particles are at least partly suspended within the reaction zone by the flow of the fluid feed through the reaction zone and the solid particles are substantially free to move about within the reaction zone as driven by the flow of the fluid feed through the reaction zone. As used herein, the term “fluid” denotes gas, liquid, vapor and combinations thereof.
[0032] Generally, the reaction conditions at which the reaction zone is maintained include a temperature in the range of from about 260° C. to about 430° C. Preferably, the temperature is in the range of from about 310° C. to about 370° C.
[0033] In accordance with the present invention, regardless of whether a fixed or fluidized bed reactor is used, the pressure is generally in the range of from about 100 pounds per square inch gauge (psig) to about 2000 psig. Generally, in a fixed bed reactor, the pressure is in the range of from about 100 psig to about 1500 psig. In a fixed bed reactor, the pressure can also be about 600 psig. In a fluidized bed reactor, the pressure is generally in the range of from about 400 psig to about 750 psig, and can also be about 500 psig.
[0034] The following examples are presented to further illustrate the present invention and are not to be construed as unduly limiting the scope of this invention.
Example 1
[0035] Undegummed vegetable oil was diluted in an undesulfurized diesel fuel to provide a mixture containing 10% vegetable oil. The mixture was mixed with either hydrogen or nitrogen and was fed into a heated ¼-inch diameter tube. The feed was exposed to a temperature of 348° C. for about 20 seconds. This run was done with hydrogen as a co-feed, and another with nitrogen as a co-feed. The feed and product metal concentrations are shown in Table I, below.
[0000] TABLE I Thermal Cracking of Vegetable Oil Description Feed Product 1 Product 2 Treatment Temperature, ° C. 348 348 Treatment Pressure, psig 200 200 Co-feed Gas H 2 N 2 ICP metal, ppm Potassium 18.9 1.6 1.6 Calcium 7.6 1.0 1.0 Magnesium 7.4 0.9 1.1 Phosphorus 47.6 10.5 13.6 Total 81.5 14.1 17.3
The result of example 1 demonstrated the total metals and phosphorus removal of about 80%.
Example 2
[0036] A mixture of soybean oil and diesel was fed into a heated tube operated at a temperature of about 330° C. and a pressure of 700 psig (there was no co-feed gas present). The mixture was then passed through a filter and sent to a hydrotreating reactor containing a hydrotreating catalyst. Table 2 below shows that the hydrotreating reactor experienced no pressure drop, unlike when the same mixture is fed through a hydrotreating reactor without the pre-treatment.
[0000]
TABLE 2
Heated
Hydrotreating
Tube/Filter/
Reactor Configuration
Reactor Only
Hydrotreating Reactor
Time On-Stream, hrs
50
100
Reactor Pressure
100
None
Drop, psig
[0037] In closing, it should be noted that the discussion of any reference is not an admission that it is prior art to the present invention, especially any reference that may have a publication date after the priority date of this application. At the same time, each and every claim below is hereby incorporated into this detailed description or specification as an additional embodiment of the present invention.
[0038] Although the systems and processes described herein have been described in detail, it should be understood that various changes, substitutions, and alterations can be made without departing from the spirit and scope of the invention as defined by the following claims. Those skilled in the art may be able to study the preferred embodiments and identify other ways to practice the invention that are not exactly as described herein. It is the intent of the inventors that variations and equivalents of the invention are within the scope of the claims while the description, abstract and drawings are not to be used to limit the scope of the invention. The invention is specifically intended to be as broad as the claims below and their equivalents.
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A triglyceride or a triglyceride/hydrocarbon combination can be thermally cracked to remove its impurities in situ prior to be upgraded to fuel range hydrocarbon. This process allows the use of a variety of low cost feedstock and reduce reactor fouling tendency. The process also reduces the use of chemicals required for conventional clean up processes such as degumming.
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TECHNICAL FIELD
The present invention relates to rotary machines comprising a stator housing two rotors, respectively male and female, driven in opposite rotations in either controlled or non-controlled manner. The object of the invention relates to the technical field of machines of the aforesaid type of which the rotors have complementary helical teeth creating, by their intermeshing, cells of variable volume, which, by developing along a direction parallel to the rotors rotation axis, set up a flow of gaseous fluid between an admission or induction orifice and an expelling orifice.
The object of the invention concerns machines of the aforesaid type working as compressors or vacuum-pumps.
PRIOR ART TECHNIQUE
In the machines of the aforesaid type, the rotation of the rotors inside their housings, when it is caused by the controlled rotation of one rotor driving the other in rotation, is performed with interposition of a liquid, generally oil, then achieving sealing between the teeth of the rotors and the housings of the stator, lubrication between rotor and stator, and cooling of the compressed gaseous fluid.
The screw-type rotors, known from application GB-A-1 342 287, have tooth tips in wedge form. With this particular construction, the presence of the sealing, lubricating and cooling liquid causes an important loss of power, due to the phenomenon whereby the liquid molecules are wedged between the tip of the teeth of the male and female rotors and the housings of the stator containing them. Said wedging phenomenon generates high pressures exerting radial forces which are harmful to the rotors and to the bearings supporting them. Said radial forces are amplified, on the one hand, by the centrifuging of the liquid in concentration near the top of the teeth, due to the high rotation of the rotors, and on the other hand, by the flowing of said liquid from the delivery plane toward the induction plane, caused by the difference of pressure between said two planes.
It is to be noted that a similar phenomenon occurs also in cases where the rotors are driven in gear-synchronized controlled rotations. In such cases, there is no lubricant fluid provided. The formation is however noted, for each tip of the teeth, of a wedge of high pressure air which is responsible for overheating and loss of power.
It is the object of the invention to propose new profiles for male and female rotors, seeking to reduce, altogether, the importance and extent of phenomenon of wedging of the molecules either of the sealing, lubricating or cooling liquid of the gaseous fluid, or of said gaseous fluid.
SUMMARY OF THE INVENTION
In order to reach the aforesaid object, the invention proposes cutting profiles, characterized in that they involve, at least for the teeth of the male rotor, an apex:
offset by an angle in the direction of rotation,
a chamfer making an angle open in the direction of rotation and defined between, on the one hand, a tangent to the apex, perpendicular to a straight line joining said apex to the center of rotation of the male rotor and, on the other hand, a straight line tangent to the apex and perpendicular to a straight line joining said apex to the instantaneous center of rotation.
Various other characteristics will emerge from the following description with reference to the accompanying drawings which show, by way of example and non-restrictively, embodiments of the object of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross-section of a rotary machine according to the invention.
FIG. 2 is an elevational view of an axial section taken substantially along line II--II of FIG. 1.
FIG. 3 is a cross-section showing, on a larger scale, the embodiment of the profiles according to the invention.
FIGS. 4 to 10 are diagrammatical views, similar to FIG. 1, illustrating various characteristic phases of operation of the object of the invention.
FIGS. 11 and 12 are cross-sections showing two variants of embodiment of one of the means of the invention.
DESCRIPTION OF PREFERRED EMBODIMENT
FIGS. 1 and 2 show a rotary machine 1 comprising a body or stator 2 defining two bores 3 and 4 which have parallel and secant axes. The stator 2 is closed laterally by two plates 5 and 6 defining respectively, an induction orifice 7 which communicates with a vestibule 8 in communication with the upper part of the bores 3 and 4, and a delivery orifice 9 which communicates with a delivery chamber 10 connected with the lower part of the bores 3 and 4. The chambers 7 and 9 have their openings situated on either side of a plane P passing through the axes of the rotors.
Plates 5 and 6 are provided with bearings, although this is not shown in the drawings, for supporting two rotors, respectively male 11 and female 12, housed in the bores 3 and 4. One of the rotors, such as for example rotor 11, is called driving rotor, because of its being driven in rotation in the direction of arrow f 1 by a driving member not shown. The female rotor 12 is called driven rotor, on account of the fact that its rotation, according to f 2 , is caused by that of rotor 11.
In known manner, rotors 11 and 12 are provided with complementary helical teeth 13 and 14, intermeshing successively, during the rotations in the direction of arrows f 1 and f 2 , in the intersection of bores 3 and 4. In conventional manner, teeth 13 and 14 are defined in cross-section perpendicular to the axis of rotation, by profiles comprising, for each tooth, several curve segments joined one to the other in succession while being determined in such a way that, when two complementary teeth intermesh in the intersection of the bores 3 and 4, the rotations, according to arrows f 1 and f 2 , create, in the transversal induction plane, a cell A of progressively decreasing volume, which, because of the helical form of the teeth, evolves according to an axial displacement from the transversal induction plane toward the opposite transversal plane corresponding to the delivery plate 6.
Such a working principle, which is due to the geometry of the teeth, is not the object of the invention and is not described in more detail hereinafter, given that knowledge of this principle and of the means for carrying it into effect are accessible to any one skilled in the art, from many available publications.
As recalled hereinabove, the rotation of rotors 11 and 12 causes the creation of a film sealing, lubricating and cooling liquid over the whole internal surface of the bores 3 and 4. In order to eliminate the phenomenon of wedging of the molecules of this film, or of the molecules of the conveyed gaseous fluid, between the bores and the apices of the teeth 13 and 14, the invention proposes to confer, at least to the teeth 13, a cross-sectional profile as described hereafter.
FIG. 3 shows that each tooth 13 of the rotor 11 is designed so as to comprise an apex SM offset in the direction of rotation of an angular value γM comprised between, on the one hand, a straight line DM joining the center of rotation CM of the male rotor 11 to the apex SM and, on the other hand, the straight line D 1 M joining the center CM to the center CF of the female rotor 12. The angle γM can be between 1° and 30° and preferably has a value equal to 7°.
The apex SM is joined to the downstream profile segment according to rotatin direction f 1 by a chamfer 13a materialized by a straight line dM tangent to the apex SM and perpendicular to a straight line D 2 M joining the apex SM to the instantaneous center of rotation CI. The straight line dM forms an angle αM with the tangent TM passing through the apex SM and perpendicular to straight line DM. The angle αM can be between 1° and 36° and its value determines, by construction, the value of angle γM, the distance between the axes of the bores 3 and 4 and their diameters, being given values.
FIG. 3 also shows that each tooth 14 of the female rotor can also be designed so as to have, in cross-section, a profile such that a chamfer 14a is created from apex SF, which chamfer is inclined in the direction of rotation f 2 . Said chamfer 14a is produced in such a way that the straight line dF which materializes it forms an angle αF with the tangent TF passing through apex SF and perpendicular to the straight line DF joining the apex to the center of rotation CF of the female rotor 12. The angle αF, open in the direction of rotation f 2 , can be between 1° and 90° and preferably has a value ranging between 10° and 30°.
An examination of FIG. 3 reveals that the chamfers 13a and 14a, opening according to angles αM and αF, are responsible for the definition with respect to the peripheral surfaces of bores 3 and 4, of wedge-shaped volumes. During the rotation in the directions of arrows f 1 and f 2 , the role of said chamfers is to force back the sealing, lubricating and cooling liquid or even, the conveyed gas, without subjecting it to a laminating and wedging effect, as this occurs when the apices SM and SF are tangentially joined.
Shaping of the profiles, as indicated hereinabove, permits:
a reduction of the frictions at the apices of the teeth, due to the fact that the sealing, lubricating and cooling liquid is no longer confined between the apices of the rotor teeth and the bores of the stator,
a reduction of leakages of the forced back liquid or compressed gas toward the induction, due to the fact that said liquid is forced back by the chamfers instead of being absorbed or swallowed by the gradual shape of the tangentially joined profiles,
a reduction of the areas undergoing frictions, due to the reduction of the mass of liquid driven back toward the induction,
an improvement of the mechanical performance and of the thermal efficiency by simultaneous reduction of the stray sources of overheating caused by heating and by the leaks of liquid and gas (or of gas alone), which actually reduces the quantity of heat to be expelled by the cooling fluid.
In the example of embodiment of the teeth 13 illustrated in FIG. 3, the shape conferred to said teeth alters the design of the delivery chamber 10 which coincides with the location of the contact points of the male and female rotors in the corresponding transverse plane. To achieve total draining out of variable-volume cell A, it is advantageous, as illustrated in FIG. 3, to provide on the transversal face of the male rotor 11, corresponding to the plane of the delivery chamber 10 and for each one of the teeth 13, a communication 20 between the profile segment preceding chamfer 13a in the direction of rotation of the rotor and a zone adjacent the instantaneous center of rotation CI. Such a communication may be formed by a recess provided in the transversal face or else by a duct formed in set-off relationship with respect to said face, from the tooth profile, and reaching into said tooth through a communicating hole.
Communication 20 makes it possible, as can be seen on examining FIGS. 4 to 10, to keep up a communication between the delivery cell A defined between two intermeshing teeth, and the delivery chamber 10, and this throughout the end of the delivery action.
The object of the invention is described in relation with rotors having teeth with asymmetrical profile. But it is understood that the dispositions of the invention can be used with symmetrical profiles.
The various advantages afforded by the object of the invention are all re-grouped in the case of constructions in which the rotors are both driven in synchronized controlled rotations by two pinions external to the bores of the male and female rotors and respectively made fast with one rotor. In such a case, the presence of the sealing, lubricating and cooling liquid is not necessary, and the advantage then afforded by the disposition according to the invention is to the reduction of gaseous fluid leaks between the delivery phase and the induction phase, as well as the reduction of overheating of such a fluid.
FIG. 11 shows a variant embodiment whereby the apices SF of the teeth 14 of the female rotor 12 are situated beyond the working diameter DP of said rotor. In such a case, the apex SF of each tooth is offset, in the direction of rotation f 2 , of a positive angular value γF. The apex SF further comprises, as previously indicated, a chamfer 14a which is materialized by a straight line dF passing through the apex SF and perpendicular to a straight line D 2 F joining the apex SF to the instantaneous center of rotation CI. The straight line dF forms, with the tangent TF to the apex SF, perpendicular to a straight line DF joining the apex SF to the center CF, an angle γF.
FIG. 12 shows another variant corresponding to an embodiment whereby each apex SF is situated within the working diameter DP. In such a case, the angle γF is negative with respect to the direction of rotation.
In the two examples illustrated in FIGS. 11 and 12, γM is dependent both on the positive or negative difference between the radius of the tooth apex and the working radius of the tooth 14 and of angle F which may be between 1° and 90° and preferably has a value between 10° and 30°. If the radius of the tooth apex is equal to the working radius, γF is nil, whatever αF, as is the case in FIG. 3.
POSSIBLE INDUSTRIAL APPLICATIONS
The object of the invention finds a particularly advantageous application in the field of compressors or vacuum pumps.
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The present invention provides an improved rotary machine of the type having male and female rotors with complementary intermeshing helical teeth. The improvement relates to the profile of the teeth, particularly the teeth of the male rotor, so that there is a reduction of the phenomenon of wedging of the sealing, lubricating or cooling liquid molecules and a reduction of the wedging of the molecules of gaseous fluid between the bores and apices of the teeth. The improved profile of the teeth and the resulting reduction of the wedging phenomenon prevents a loss of power which is typical in the prior art screw-type rotary machines.
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BACKGROUND OF THE INVENTION
[0001] Many of the medical care garments and products, protective wear garments, mortuary and veterinary products, and personal care products in use today are partially or wholly constructed of thermoplastic nonwoven web materials. Examples of such products include, but are not limited to, medical and health care products such as surgical drapes, gowns and bandages, protective workwear garments such as coveralls and lab coats, and infant, child and adult personal care absorbent products such as diapers, training pants, swimwear, incontinence garments and pads, sanitary napkins, wipes and the like. For these applications nonwoven materials provide tactile, comfort and aesthetic properties which can approach those of traditional woven or knitted cloth materials. Nonwoven web materials are also widely utilized as filtration media for both liquid and gas or air filtration applications since they can be formed into a filter mesh of fine fibers having a low average pore size suitable for trapping particulate matter while still having a low pressure drop across the mesh.
[0002] Nonwoven web materials have a physical structure of individual fibers or filaments which are interlaid in a generally random manner to form a fibrous web material. The fibers may be continuous or discontinuous, and are frequently produced from thermoplastic polymer or copolymer resins from the general classes of polyolefins, polyesters and polyamides, as well as numerous other polymers. Blends of polymers or conjugate multicomponent fibers may also be employed. Nonwoven materials formed by melt extrusion processes such as spunbonding and meltblowing, and formed by dry-laying processes such as carding or air-laying of staple fibers are well known in the art. In addition, nonwoven materials may be used in composite materials in conjunction with other nonwoven layers as in a spunbond/meltblown (SM) and spunbond/meltblown/spunbond (SMS) laminate materials, and may also be used in combination with thermoplastic films.
[0003] Nonwoven materials may be topically treated to impart various desired properties, depending on end-use application. For example, some applications such as components for diapers and other incontinence products and feminine hygiene products call for nonwoven materials which are highly wettable and will quickly allow liquids to pass through them. For these applications it is desirable to treat the nonwoven materials with surfactants or other chemicals to impart hydrophilicity. On the other hand, for applications such as surgical drapes and gowns, and other protective garments, liquid barrier properties are highly desirable, and specifically desirable are nonwoven materials which have a high degree of repellency to low surface tension liquids such as alcohols, aldehydes, ketones and hydrophilic liquids, such as those containing surfactants. Repellency to low surface tension liquids may be achieved by treating the nonwoven material with chemicals such as fluorochemical compounds known in the art. Topical treatments are available to impart other properties as well, such as antistatic treatments for example.
[0004] Topical treatments are typically applied to fibrous web materials such as nonwoven materials in the form of a treatment chemical carried in a liquid, often aqueous, medium as a solution, suspension or emulsion. Once the treatment has been applied to the nonwoven material it is generally necessary to remove the excess moisture in the nonwoven material sheet by drying. Conventionally, the moisture is removed by blowing heated air on the nonwoven material or by running the nonwoven material over and in contact with heated surfaces such as rollers or cans until it is dry or nearly dry. However, a wetted nonwoven material generally will not dry in all places at the same rate; therefore with conventional drying techniques certain areas of the nonwoven material will become completely dry while other areas still contain moisture, and these areas which dry first will experience continued and excessive heat from the drying process while the entire sheet of material is dried to a satisfactory level of residual moisture. This additional heating of the nonwoven material can deleteriously affect the material and degrade material properties such as by causing heat shrinkage of the material, reducing material tensile strength, causing the material to become embrittled and/or surface glazed and thereby unpleasant to the touch, and decreasing barrier properties in SMS laminate materials.
[0005] Consequently, there remains a need for an efficient treatment method that provides treated thermoplastic nonwoven materials without unduly negatively impacting the material and material properties compared with methods heretofore known.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] [0006]FIG. 1 is a schematic illustration of an exemplary process for topically treating fibrous webs in accordance with the invention.
SUMMARY OF THE INVENTION
[0007] The present invention provides a method for treating a fibrous web material including the steps of providing a fibrous web material, treating the web material with a topical treatment which includes a treatment chemical and a liquid carrier medium, partially drying the treated web material such that after the partial drying step the web material has less than about 40 percent and at least about 10 percent by weight residual moisture and then passing the web material through a radio frequency energy field to further dry the web. After passing through the radio frequency energy field the web has less than about 5 percent by weight residual moisture, desirably less than about 2 percent, more desirably less than about 1 percent, and still more desirably less than about 0.5 percent by weight residual moisture.
[0008] The partial drying step may be performed by applying vacuum or external heat to the fibrous web material, and the fibrous web material may desirably be thermoplastic nonwoven web material or thermoplastic nonwoven barrier laminate material. The topical treatment may desirably be a liquid-repellent treatment, a hydrophilic treatment or an anti-static treatment. In certain embodiments, the web after partial drying has about 20 percent to about 10 percent by weight residual moisture. The radio frequency energy field may have a frequency ranging from about 10 megahertz to about 50 megahertz. Also provided are fibrous web materials obtained in accordance with embodiments of the method of the invention.
Definitions
[0009] As used herein and in the claims, the term “comprising” is inclusive or open-ended and does not exclude additional unrecited elements, compositional components, or method steps.
[0010] As used herein the term “polymer” generally includes but is not limited to, homopolymers, copolymers, such as for example, block, graft, random and alternating copolymers, terpolymers, etc. and blends and modifications thereof. Furthermore, unless otherwise specifically limited, the term “polymer” shall include all possible geometrical configurations of the material. These configurations include, but are not limited to isotactic, syndiotactic and random symmetries.
[0011] As used herein the term “fibers” refers to both staple length fibers and continuous filaments, unless otherwise indicated.
[0012] As used herein the term “monocomponent” fiber refers to a fiber formed from one or more extruders using only one polymer extrudate. This is not meant to exclude fibers formed from one polymer to which small amounts of additives have been added for color, anti-static properties, lubrication, hydrophilicity, etc. These additives, e.g. titanium dioxide for color, are generally present in an amount less than 5 weight percent and more typically about 2 weight percent.
[0013] As used herein the term “multicomponent fibers” refers to fibers which have been formed from at least two component polymers, or the same polymer with different properties or additives, extruded from separate extruders but spun together to form one fiber.
[0014] Multicomponent fibers are also sometimes referred to as conjugate fibers or bicomponent fibers. The polymers are arranged in substantially constantly positioned distinct zones across the cross-section of the multicomponent fibers and extend continuously along the length of the multicomponent fibers. The configuration of such a multicomponent fiber may be, for example, a sheath/core arrangement wherein one polymer is surrounded by another, or may be a side by side arrangement, an “islands-in-the-sea” arrangement, or arranged as pie-wedge shapes or as stripes on a round, oval, or rectangular cross-section fiber. Multicomponent fibers are taught in U.S. Pat. No. 5,108,820 to Kaneko et al., U.S. Pat. No. 5,336,552 to Strack et al., and U.S. Pat. No. 5,382,400 to Pike et al. For two component fibers, the polymers may be present in ratios of 75/25, 50/50, 25/75 or any other desired ratios.
[0015] As used herein the term “nonwoven web” or “nonwoven material” means a web having a structure of individual fibers or filaments which are interlaid, but not in an identifiable manner as in a knitted or woven fabric. Nonwoven webs have been formed from many processes such as for example, meltblowing processes, spunbonding processes, air-laying processes and carded web processes. The basis weight of nonwoven fabrics is usually expressed in grams per square meter (gsm) or ounces of material per square yard (osy) and the fiber diameters useful are usually expressed in microns. (Note that to convert from osy to gsm, multiply osy by 33.91).
[0016] The term “spunbond” or “spunbond nonwoven web” refers to a nonwoven fiber or filament material of small diameter fibers that are formed by extruding molten thermoplastic polymer as fibers from a plurality of capillaries of a spinneret. The extruded fibers are cooled while being drawn by an eductive or other well known drawing mechanism. The drawn fibers are deposited or laid onto a forming surface in a generally random manner to form a loosely entangled fiber web, and then the laid fiber web is subjected to a bonding process to impart physical integrity and dimensional stability. The production of spunbond fabrics is disclosed, for example, in U.S. Pat. No. 4,340,563 to Appel et al., U.S. Pat. No. 3,802,817 to Matsuki et al. Typically, spunbond fibers or filaments have a weight-per-unit-length in excess of 2 denier and up to about 6 denier or higher, although finer spunbond fibers can be produced. In terms of fiber diameter, spunbond fibers generally have an average diameter larger than 7 microns, and more particularly between about 10 and about 25 microns.
[0017] As used herein the term “meltblown fibers” means fibers or microfibers formed by extruding a molten thermoplastic material through a plurality of fine, usually circular, die capillaries as molten threads or fibers into converging high velocity gas (e.g. air) streams which attenuate the fibers of molten thermoplastic material to reduce their diameter. Thereafter, the meltblown fibers are carried by the high velocity gas stream and are deposited on a collecting surface to form a web of randomly dispersed meltblown fibers. Such a process is disclosed, for example, in U.S. Pat. No. 3,849,241 to Buntin. Meltblown fibers may be continuous or discontinuous, are generally smaller than 10 microns in average diameter and are often smaller than 7 or even 5 microns in average diameter, and are generally tacky when deposited onto a collecting surface.
[0018] The term “staple fibers” refers to discontinuous fibers, which typically have an average diameter similar to that of spunbond fibers. Staple fibers may be produced with conventional fiber spinning processes and then cut to a staple length, typically from about 1 inch to about 8 inches. Such staple fibers are subsequently carded or airlaid and thermally or adhesively bonded to form a nonwoven fabric.
[0019] As used herein, “thermal point bonding” involves passing a fabric or web of fibers or other sheet layer material to be bonded between a heated calender roll and an anvil roll. The calender roll is usually, though not always, patterned in some way so that the entire fabric is not bonded across its entire surface. As a result, various patterns for calender rolls have been developed for functional as well as aesthetic reasons. One example of a pattern has points and is the Hansen Pennings or “H&P” pattern with about a 30% bond area with about 200 bonds/square inch as taught in U.S. Pat. No. 3,855,046 to Hansen and Pennings. The H&P pattern has square point or pin bonding areas wherein each pin has a side dimension of 0.038 inches (0.965 mm), a spacing of 0.070 inches (1.778 mm) between pins, and a depth of bonding of 0.023 inches (0.584 mm). The resulting pattern has a bonded area of about 29.5%. Another typical point bonding pattern is the expanded Hansen and Pennings or “EHP” bond pattern which produces a 15% bond area with a square pin having a side dimension of 0.037 inches (0.94 mm), a pin spacing of 0.097 inches (2.464 mm) and a depth of 0.039 inches (0.991 mm). Other common patterns include a diamond pattern with repeating and slightly offset diamonds and a wire weave pattern looking as the name suggests, e.g. like a window screen. Typically, the percent bonding area varies from around 10% to around 30% of the area of the fabric laminate web. Thermal point bonding imparts integrity to individual layers by bonding fibers within the layer and/or for laminates of multiple layers, point bonding holds the layers together to form a cohesive laminate.
[0020] As used herein, the term “hydrophilic” means that the polymeric material has a surface free energy such that the polymeric material is wettable by an aqueous medium, i.e. a liquid medium of which water is a major component. The term “hydrophobic” includes those materials that are not hydrophilic as defined. The phrase “naturally hydrophobic” refers to those materials that are hydrophobic in their chemical composition state without additives or treatments affecting the hydrophobicity. It will be recognized that hydrophobic materials may be treated internally or externally with surfactants and the like to render them hydrophilic.
DETAILED DESCRIPTION OF THE INVENTION
[0021] The present invention provides a method for topically treating fibrous web materials such as thermoplastic nonwoven materials and nonwoven barrier laminate materials. The method includes providing the fibrous web material, topically treating the fibrous web material with a liquid-carried treatment chemical, partially drying the fibrous web material and then further drying the fibrous web material utilizing a radio frequency energy field.
[0022] Conventional topical treatment methods for fibrous webs include brushing or spraying liquid chemical treatment on the web, dipping or saturating the web in a liquid treatment bath and foaming a liquid chemical treatment and applying the foam to the web material.
[0023] The invention will be more fully described with reference to FIG. 1. Turning to FIG. 1, there is illustrated in schematic form an exemplary process line 10 which demonstrates an embodiment of the method of treating fibrous web materials. Fibrous web material 20 is shown being transported through process line 10 . Fibrous web material 20 may desirably be a thermoplastic nonwoven web material or laminate material including thermoplastic nonwoven web materials such as for example spunbonded materials, bonded carded webs, high-loft spunbond and through-air dried nonwovens, spunbond-meltblown-spunbond (“SMS”) laminates or spunbond-film-spunbond (“SFS”) laminates. As shown in FIG. 1, fibrous web material 20 is topically treated at treatment station 30 . Treatment station 30 may desirably be one or more means of applying topical treatment as are known in the art such as for example a brush treater, spray treater, foam treater, or, as shown, a saturation treater such as a dip and squeeze bath.
[0024] For the purpose of describing the advantages of the invention, FIG. 1 and process line 10 will be described with reference to fibrous web material 20 being a nonwoven barrier laminate material such as for example a spunbond-meltblown-spunbond laminate or “SMS” laminate material which may be produced in accordance with U.S. Pat. No. 4,041,203 to Brock et al., incorporated herein by reference in its entirety. Because of their liquid barrier properties, SMS laminate materials are highly suitable as protective fabrics and are used as or as part of surgical suite wear such as patient drapes and surgical gowns, and also may be used in protective or industrial workwear. However, in order to more fully protect the wearer from harmful exposure to contaminants the laminate material should have a high degree of repellency to low surface tension liquids such as surfactant containing aqueous solutions, alcohols, aldehydes and ketones. Repellency to low surface tension liquids may be imparted to the laminate material by use of a treatment chemical such as for example fluorocarbon compound treatments as are disclosed in U.S. Pat. No. 5,149,576 to Potts et al. and U.S. Pat. No. 5,178,931 to Perkins et al., both incorporated herein by reference in their entireties, and fluorocarbon compound treatments are available commercially.
[0025] To impart repellency to low surface tension liquids, treatment station 30 may desirably be a dip and squeeze station as is known in the art and which contains a bath of an aqueous emulsion of fluorocarbon compound. The fibrous web material 20 travels a path which immerses the web in the bath to saturate it with the treatment emulsion. Web material 20 continues through nip rollers 32 and 34 which squeeze off the excess treatment bath emulsion. Despite having the excess bath removed by nip rollers 32 and 34 , the web material 20 will typically have about a 100 percent “wet pick up” upon exiting treatment station 30 . That is, a web material of approximately 70 gsm when dry will weigh approximately 140 gsm after exiting treatment station 30 and nip rollers 32 and 34 , and must be dried prior to storage of the material. The web material should contain as little residual moisture as is practicable, desirably less than about 5 percent moisture by weight, more desirably less than about 2 percent by weight, and still more desirably less than about 1 percent or even 0.5 percent by weight residual moisture.
[0026] A conventional method well known in the art for drying treated webs is the use of steam canisters, such as the steam canisters 40 , 50 and 60 which are incorporated as part of the treatment process shown in FIG. 1. Fibrous web 20 travels between and in tensioned contact with canisters 40 , 50 and 60 which are heated with steam to heat the web material and drive off moisture via evaporation. Typically, the number and/or temperature of the steam canisters will be adjusted to match the amount of drying needed in order to fully or nearly fully dry the fibrous web material. However, this has several drawbacks. Because the planar surfaces of the web material are in direct contact with the heated canisters, the outer surfaces of web material will tend to become fully dry well before the center of the material, which will result in the surfaces of the material being exposed to overheating. Further, certain areas of a moving web material, often the edges and the transverse middle portion of the web, will be under more tension than other areas of the web and be pressed against the heated canisters with more force than the other areas of the web material, resulting in these higher tension areas becoming dry before the other areas and therefore being exposed to overheating. Because the web materials are made with thermoplastic resins, overheating of the web material surfaces and overheating of other high tension areas results in undesirable heat-glazing (that is, a slight to moderate melting) of the material surfaces, making the material stiff and making the material surfaces harsh and unappealing to the touch. Also, overheating of the web material generally causes heat shrinkage of the material, often resulting in web width losses of 5 percent or even greater.
[0027] In order to alleviate the overheating problems caused by attempting to fully dry the fibrous web material 20 with external heat, FIG. 1 and process line 10 further include a radio frequency station 70 which generates a radio frequency energy field through which fibrous web 20 passes. In the practice of the invention, rather than fully drying the fibrous web material with the externally applied heat of the steam canisters, the web material is only partially dried until it retains about 40 percent by weight or less of residual moisture. Depending on equipment available and the particular web to be dried, it may be advantageous to partially dry the web until it has only about 20 percent or only about 10 percent by weight of residual moisture. As explained below, to avoid overheating the web material it is important that the web still retain some moisture after the partial drying step. Further drying is accomplished by the radio frequency energy at radio frequency drying station 70 .
[0028] As known in the art, radio frequency energy or dielectric is an alternating electromagnetic field which causes susceptible molecules to attempt to orient the molecular poles alternatingly to follow the alternating electromagnetic field. Molecules susceptible to the dielectric field include polar molecules such as the water molecule and other polar liquid solvents in which treatment chemicals are typically dissolved, suspended or emulsified. As the molecules in the liquid continue to alternatingly reorient themselves they “vibrate” and thereby gain frictional heat energy and cause evaporation of the liquid. However, because conventional thermoplastic resins useful for fibrous nonwoven web materials are generally non-polar molecules they are not susceptible to the radio frequency energy field, and are therefore not heated by the radio frequency energy. In this manner the fibrous web material may be further dried until it has less than about 5 percent by weight moisture, and desirably until is has less than about 2 percent moisture, without any dried portions of the web being contacted by external heat sources in excess of 100 degrees Celsius and thereby avoiding the deleterious effects of overheating. Radio frequency “ovens” are commercially available which produce radio frequency energy fields at frequencies of from about 1 megahertz (MHz) to about 80 megahertz, typically from about 10 to about 50 megahertz, and commonly available radio frequency units are available at 13, 27 and 40 MHz. Although not shown in FIG. 1, radio frequency drying station 70 may desirably also include a vent or vacuum system suitably attached to evacuate the water vapor produced by drying the web.
[0029] As shown in FIG. 1, as the fibrous web material 20 exits the radio frequency drying station 70 it may be wound up as a roll of dried web material on winding roll 80 . As an alternative to taking the dried fibrous web material up on winding roll 80 , the material may be directed to various finishing steps such as web slitting, stretching or further treating, or may be directed immediately to various converting or integrated product forming operations.
[0030] As another example, the fibrous web material 20 may be a lofty nonwoven material such as a bonded carded staple fiber web, or as a spunbond web material made with crimped multicomponent or bicomponent fibers in side-by-side or eccentric sheath-core arrangement. Such crimped multicomponent fibers and lofty webs are described in U.S. Pat. No. 5,382,400 to Pike et al., incorporated herein by reference in its entirety. Lofty nonwoven web materials find extensive use in personal care absorbent products, and for many such uses it is desirable for the nonwoven web materials to be wettable. Wettability may be imparted by topically treating the web with, for example, surfactant treatments as are known in the art by saturation dipping at treatment station 30 , or alternatively by such well known methods as brush treating, spraying or foaming. The partial drying step may be accomplished by the steam canisters as shown in FIG. 1. Alternatively, because lofty nonwoven webs typically have much higher air permeability than the barrier laminate materials previously discussed, it would also be useful to employ means such as a vacuum or through air drying using heated air to partially dry the web until it retains less than about 40 percent by weight residual moisture as stated above. Then, the remainder of the moisture may be evaporated by radio frequency heating of the water without overly heating the web.
[0031] Where steam canisters are the means used for partial drying of the lofty nonwoven web, the use of a radio frequency energy field to remove the residual moisture in the web can be particularly advantageous for helping to retain the loft of the web. For example, in order to hold the lofty nonwoven web against the steam canister as the web travels over the canister there must be tension on the web, which can result in some compression forces pushing the web against the canister, decreasing the loft of the web. Where these compression forces are still being applied at the point in the process when the web is completely dry and beginning to be overheated, overheating can “set” the web structure, resulting in permanent loss of loft. Also, as mentioned above with regard to barrier laminate materials, continued contact with the hot surface of the steam canisters after the surface of the lofty web is fully dried can result in heat glazing of the surface, making it stiff and harsh to the touch.
[0032] Other webs may suitably be treated and dried by use of the invention. For example, nonwoven webs made by the spunbonding method are frequently used for liners and coverstock material for personal care absorbent garments, and are therefore often treated to impart hydrophilicity to assist the absorbent garment in accepting and absorbing bodily fluid exudates from the wearer. Where topical liquid surfactant application is desired, as by spray treater, a vacuum source is generally applied to the liner materials to remove the excess liquid treatment. Still, after vacuum removal of excess treatment the webs contain substantial moisture, which can lead to undesirable microorganism growth on the webs if the webs are stored in this moist condition. However, liner and coverstock materials are meant to be used in close contact with intimate portions of the user's anatomy, and prior to treatment these materials will already have undergone at least one heat-intensive processing step such as thermal point bonding. Therefore the method described herein, utilizing vacuum to partially dry the web materials and utilizing radio frequency energy to further dry the web to a fully or nearly fully dry state is an advantageous way to avoid unnecessary additional heating of the webs. The vacuum extraction may additionally be used in combination with the external heat partial drying as described above.
[0033] Polymers suitable for the fibrous web materials include the known polymers suitable for production of nonwoven webs and materials such as for example polyolefins, polyesters, polyamides, polycarbonates and copolymers and blends thereof. However it should be noted that certain commercially available polymers and staple-length fibers which have abundant dipoles or which have had other radio frequency susceptible added to the polymer are susceptible to radio frequency heating, such as for example the CoPET-A “Kodel 410 ” binder fibers available from the Eastman Chemical Company. These types of polymers and fibers should not be use unless it is specifically desired to heat bond or partially heat bond the fibrous web material while performing the further drying step in the radio frequency drying station.
[0034] Numerous other patents have been referred to in the specification and to the extent there is any conflict or discrepancy between the teachings incorporated by reference and that of the present specification, the present specification shall control. Additionally, while the invention has been described in detail with respect to specific embodiments thereof, it will be apparent to those skilled in the art that various alterations, modifications and/or other changes may be made without departing from the spirit and scope of the present invention. It is therefore intended that all such modifications, alterations and other changes be encompassed by the claims.
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The present invention provides an efficient method for topically treating and drying fibrous web materials such as nonwoven web materials and nonwoven laminate materials without unduly damaging the materials due to excessive heating during drying.
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CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims priority under 35 U.S.C. §119(e) to U.S. Provisional Patent Application Ser. No. 61/715,367, filed Oct. 18 2012, entitled JET PUMP REPAIR FOR A NUCLEAR POWER PLANT.
BACKGROUND
[0002] 1. Field
[0003] The present invention relates to a method for repairing a jet pump and more particularly to a method for repairing the slip joint between an inlet mixer and a diffuser of a jet pump with particular benefit to jet pumps employed in boiling water reactors.
[0004] 2. Related Art
[0005] As can be appreciated from FIG. 1 , in conventional boiling water reactors 10 , jet pump assemblies 18 are located in the reactor vessel's annulus region 12 , between the core shroud 14 and a wall of the reactor vessel 16 . The primary function of the jet pump is to pump coolant below the reactor core where the coolant then flows up through the fuel assemblies to extract heat from the fuel assemblies. The jet pumps are also relied upon to maintain two-thirds of the water level height in the reactor core during postulated accident conditions. For these reasons, the jet pump assemblies 18 are considered safety related components.
[0006] In a typical arrangement, twenty jet pumps are paired in ten assemblies 18 , as illustrated in FIG. 2 . Each jet pump assembly 18 is driven by flow from a common riser pipe 22 . Jet pump flow is then directed to the lower plenum region 24 below the core supported within the shroud 14 . Jet pump flow is roughly one-third driven by the reactor coolant system pump flow through the riser pipe 22 , and the last two-thirds of jet pump flow is due to venturi action of the jet pump suction inlet that pulls in fluid from the annulus region 12 . The jet pump assemblies 18 are circumferentially spaced around the shroud 14 , supported on a shroud support ledge 20 near the bottom of the shroud.
[0007] Industry operating experience has encountered numerous instances of damage or accelerated wear to critical components of the jet pump assemblies 18 which has affected a large population of boiling water reactors both in the United States and globally. The most common jet pump components to experience damage are the main wedge and rod 26 , restrainer bracket pad in the restrainer bracket 28 , riser pipe 22 welds and riser brace 30 , all of which components can be observed in FIG. 3 , which shows an enlarged perspective view of a jet pump assembly 18 . These common types of damage are all in critical supporting structures or features of the jet pump assemblies. Damage and wear are largely attributable to flow induced vibration due to normal operation. In addition to flow induced vibrations, many plants experience excessive leakage in the slip joint region 32 , which can exacerbate the vibration experienced in the jet pump assemblies 18 . This leakage can greatly accelerate the degradation and damage done to the jet pumps.
[0008] Plants that have shown signs of accelerated wear and component movement, both indicators of flow induced vibration issues, have historically attempted to address the problem by adding additional hardware to help support the jet pump components and reinforce the components against flow induced vibration. These solutions have generally been in the area of the restrainer bracket 28 and include larger main wedges 26 , supplemental auxiliary wedges, and slip joint clamps. These solutions do not address the root cause of flow induced vibrations, have been ineffective for some plants, and their effectiveness overall is questionable.
[0009] In addition to these typical solutions, a few boiling water reactor plants have added labyrinth seals to the inlet mixer 34 original equipment manufacturer design. These labyrinth seals are intended to reduce bypass flow in the slip joint region 32 of the jet pumps; however, it appears that under certain operating conditions in some plants these seals have been ineffective and the seal geometry has been damaged on the inlet mixer's outer diameter and has caused damage to the inner diameter of the collar 38 on the diffuser 36 .
[0010] In the slip joint region 32 , the inlet mixer 34 is unsupported or floats, allowing the mixer to thermally expand along its length during plant startup and shutdown. The inlet mixer's bottom section fits into the collar 38 of the diffuser assembly 36 , forming a slip joint. The inlet mixer 34 is laterally supported by a three-point contact at the restrainer bracket 28 . This three-point contact is maintained with a sliding (main) wedge 26 and two set screws that are tack welded in place. The main wedge 26 is held in place by gravity, theoretically resulting in three-point contact. The very upper portion of the inlet mixers are supported by a pre-tensioned beam bolt assembly 40 that presses down on the inlet mixer 34 where it is seated in the transition seat 42 .
[0011] Because of how the inlet mixers 34 are supported, small lateral loads on the bottom of the inlet mixer (within the slip joint 32 ) can create large reaction moments at the restrainer bracket 28 . As previously mentioned, the main wedge 26 is held in place by its weight, typically about eight pounds, which can be overcome and lifted by small lateral forces. Since the inlet mixer 34 weighs significantly more than the wedges 26 , its mass can easily overcome the holddown force of the main wedge 26 with small lateral displacements at the outlet of the inlet mixer 34 within the diffuser collar 38 . Once the wedge is temporarily displaced, three-point contact is lost, and, in severe cases, the bottom of the inlet mixer may hammer against the inside of the diffuser collar 38 . This hammering of the inlet mixer 34 and diffuser 36 can also be excited at particular frequencies of vibrations, potentially caused by drive flow or bypass flow in the slip joint 32 .
[0012] Thus, a new solution to flow induced vibrations is desired that will address the root cause of the vibrations.
[0013] Furthermore, a solution to the flow induced vibration wear is desired that will minimize such wear and require little or no disassembly of the jet pump assembly 18 .
[0014] Further, such a repair is desired that can be performed remotely, under water.
SUMMARY
[0015] These and other objects are achieved by employing a new method of repairing a slip joint on a jet pump assembly between an inlet mixer and a diffuser that has an opening that receives the inlet mixer with a given spacing between an outside diameter of the inlet mixer and an inside diameter of the opening in the diffuser forming an annulus; with the given spacing a product of manufacture and vibration wear. The method comprises the steps of remotely accessing the annulus and narrowing a radial dimension of the annulus.
[0016] In one embodiment, the method includes the step of measuring a dimension of the outside diameter of the inlet mixer that fits within the slip joint. A clamp is then fabricated having a generally circular collar clamp opening with a design diameter that is larger than the outside diameter of the inlet mixer and smaller than a maximum extent of the inside diameter of the diffuser opening. A collar clamp is then fitted around the inlet mixer and at least partially over and above the diffuser opening with the collar clamp supported by the diffuser. The collar clamp is then attached to a portion of the diffuser housing below the diffuser opening. Preferably, the measuring step measures dimensions around the diffuser opening in addition to the outsider diameter of the inlet mixer. In one embodiment, the diffuser has guides spaced circumferentially around a housing of the diffuser, with the guides extending above the opening in the diffuser that receives the inlet mixer. In the latter embodiment, the method includes the steps of forming notches in an underside of the collar clamp, in line with the guides; and fitting the notches over the guides wherein the guides restrain rotation of the collar clamp. In these embodiments, the collar clamp effectively optimizes the insertion depth of the inlet mixer within the diffuser opening. Desirably, the collar clamp is fabricated in at least two circumferential sections with each of the sections fastened together to form the generally circular opening. In this embodiment, the attaching step clamps the collar clamp to the portion of the diffuser housing, which is preferably a radially outwardly extending collar on the diffuser housing. In this latter arrangement, the collar clamp has at least two radially, outwardly extending segments that extend out radially further than the diffuser collar and the outwardly extending segments have a vertical opening therethrough. A tie bar having a radially, inwardly extending lip at a lower end positioned under the diffuser collar and a second end of the tie bar extending through one of the openings in the segments is captured on another side of the opening in the segments to tighten the collar clamp down against the diffuser collar. Preferably, the attaching step clamps the collar clamp to the portion of the diffuser housing at a plurality of discrete circumferential locations around the housing. In this arrangement, the method does not require the step of removing the inlet mixer from the diffuser.
[0017] In still another embodiment, the collar clamp has an axially extending convergent surface that faces an outer surface of the inlet mixer when the collar clamp is fitted around the inlet mixer and the collar clamp rests on a lip of the diffuser opening. In one arrangement, the collar clamp has an annular circumferential groove adjacent the generally circular clamp opening, the groove having a generally “L” shape in the radial direction with one leg of the “L” extending in a horizontal direction and resting on a lip of the diffuser opening. Preferably, the second leg of the “L” contacts an outer wall of the diffuser. The method may also insert a gasket between the collar clamp and a lip of the diffuser opening to minimize leakage.
[0018] In still another embodiment, the step of narrowing the radial dimension of the annulus comprises the step of removing the inlet mixer from the diffuser. Then, the inside surface of the diffuser opening is machined and material damage on the inlet mixer outer surface that is to be inserted into the diffuser opening is resurfaced. The method then inserts an internal collar having an outside diameter substantially equal to an inside diameter of the machined inside surface of the diffuser opening and has an inside diameter that narrows the annulus gap when the inlet mixer is inserted into the diffuser opening so that the annulus has a radial dimension that is less than the given spacing. Preferably, the internal collar is fabricated to have an axially convergent contour on a surface that opposes the outer surface of the inlet mixer.
[0019] In each of the foregoing embodiments, the radial dimension of the annulus is narrowed to be equal to or smaller than a corresponding original equipment manufacturer specification.
[0020] Alternately, in a separate embodiment, the step of narrowing the radial dimension of the annulus includes the step of cutting a collar portion of the diffuser that surrounds the inlet mixer from the remainder of the diffuser. The collar portion of the diffuser is then removed from the rest of the diffuser and the inlet mixer. A spool piece is then fabricated having a replacement opening with a desired inside diameter to replace the collar portion of the diffuser; and the spool piece is secured to the rest of the diffuser with an end of the inlet mixer within the replacement opening.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] A further understanding of the invention claimed hereafter can be gained from the following description of the preferred embodiments when read in conjunction with the accompanying drawings in which:
[0022] FIG. 1 is a perspective view of a boiling water reactor with the reactor vessel cut away to show the core shroud and the general placement of the jet pump assemblies;
[0023] FIG. 2 is a perspective view of the core shroud of FIG. 1 with a better view of the placement of the jet pump assemblies;
[0024] FIG. 3 is an enlarged perspective view of one of the jet pump assemblies illustrated in FIGS. 1 and 2 ;
[0025] FIG. 4 is a close-up perspective view of a prior art slip joint;
[0026] FIG. 5 is a close-up perspective view of a slip joint incorporating one embodiment of this invention;
[0027] FIG. 6 is a cross section of a slip joint incorporating the embodiment illustrated in FIG. 5 showing the optimization of insertion depth of the inlet mixer;
[0028] FIG. 7 is a perspective view of the clamp employed in the embodiment shown in FIG. 5 ;
[0029] FIG. 8 is a close-up perspective view of a portion of the collar clamp employed in the embodiment of FIG. 5 supported on a lip of the diffuser opening adjacent an outer surface of the inlet mixer showing an axially convergent interface of one form of the embodiment shown in FIG. 5 ;
[0030] FIG. 9 is a perspective view of a diffuser collar illustrating another embodiment of this invention;
[0031] FIG. 10 is a sectional view of the embodiment shown in FIG. 9 ;
[0032] FIG. 11 is a perspective view of a third embodiment of this invention; and
[0033] FIG. 12 is a sectional view of the embodiment shown in FIG. 11 .
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0034] FIG. 4 shows a close-up perspective view of the slip joint region 32 with the diffuser 36 having a radially outward projecting shoulder 44 just below the diffuser collar 38 that defines the opening 46 in the diffuser in which the inlet mixer 34 is inserted. The diffuser collar 38 has guides (sometimes referred to as ears) that extend radially outward and upward from the opening 46 to guide the inlet mixer 34 into the opening 46 . According to one embodiment of the present invention, the current inlet mixer 34 and diffuser collar 38 are supplemented by stacking an additional collar clamp 48 on top of the diffuser, over and around the diffuser collar 38 as shown in FIG. 5 . In addition to other benefits, the collar clamp 48 optimizes the overall insertion depth for the slip joint 32 . The insertion depth of the inlet mixer 34 into the diffuser 36 has been recognized as one of several critical parameters that lead to the onset of inlet mixer vibration. In another embodiment, the collar clamp 48 is structured to create an axially convergent slip joint geometry relative to the diffuser and/or inlet mixer.
[0035] Rather than replace the existing inlet mixer, the design of the present embodiment retains and creates a new slip joint region 32 by the addition of hardware onto the top of the diffuser 36 . The present invention addresses flow induced vibration issues by either: (1) using a convergent slip joint design, (2) optimizing the effective insertion depth, or (3) both using a convergent slip joint design and optimizing the effective insertion depth. FIG. 5 shows this design concept developed according to one embodiment of the invention. The embodiment shown in FIG. 5 allows for any existing damage to both the mixer and the diffuser to be left in place. A new slip joint area is created directly above the old slip joint (see FIG. 6 ). This design approach has the following advantages: (i) it is able to be installed in situ with no inlet mixer removal required; (ii) does not require surface repairs; (iii) provides tight tolerance control of the slip joint gap; (iv) creates an optimal insertion depth; (v) reduces overall repair time and costs; (vi) enables a convergent slip joint configuration; and (vii) provides a flow-induced vibration solution that addresses a root cause.
[0036] Generally, there are two basic options for implementing an axially convergent slip joint design onto the existing diffuser components. The first option entails modifying the exiting diffuser surface by removing or adding material on its collar 38 . The second option entails adding additional hardware and creating a new slip joint area above the old slip joint area, e.g., as described with respect to FIG. 5 . The present invention contemplates both options. FIG. 6 is a cross section of the embodiment shown in FIG. 5 ; i.e., the second option mentioned above. Bracket A on the right shows the original insertion depth prior to the collar clamp 48 being installed. Bracket B, just to the left of bracket A shows the original slip joint area. Bracket C on the left shows the new improved slip joint area achieved by adding the collar clamp 48 .
[0037] FIG. 7 shows one embodiment of the collar clamp 48 that is created from two semi-circular segments 52 and 54 which are joined by dovetail joints 56 and 58 , though it should be appreciated that other means of joining the segments are available and the clamp 48 may be constructed out of two or more such segments. Each segment has a radially outwardly extending arm 60 and 62 through which holes 64 and 66 are formed that will be used to clamp the collar clamp 48 to the diffuser housing 36 as will be described hereafter. FIG. 8 is an enlarged partial sectional view of the inlet mixer 34 , the diffuser 36 and the collar clamp 48 embodiment shown in FIG. 5 , uncovering the convergent slip joint at the intersection between collar clamp segments. The design utilizes a convergence geometry, i.e., the inner face of the collar clamp 48 that faces the outer surface of the inlet mixer 34 converges toward the outer surface of the inlet mixer as one progresses from the upper and lower ends to the center of the inside face of the collar clamp 48 . The convergence geometry works off an unmodified inlet mixer original equipment manufacturer outer surface design. The actual dimensions and angles can be fine tuned for each slip joint (since the existing slip joint geometry is left in place and new differential pressure conditions are created in the slip joint).
[0038] According to one embodiment of this invention, digital measurements are taken and three D models rendered of the inlet mixer 34 and diffuser collar slip joints 32 , for example, using a three-D laser scanner. These measures are taken since the as-found conditions of the diffuser and mixer may differ between jet pumps (i.e., components will vary dimensionally from one another, and actual as-built dimensions are unknown). Also, the tight tolerance for the slip joint gap requires the added hardware to have high tolerance requirement for fit-up. The three-D laser scanner technology provides very accurate measurements, approximately plus/minus 0.005 inch (0.013 cm). Also, the rendered three-D model may be saved as a compatible AutoCAD file type, which allows a machine shop to use the CAD file to automatically program CNC mills and lathes to machine from hardware blanks which meet these tight tolerances.
[0039] According to the current embodiment, the collar clamp configuration uses two stack halves 52 , 54 that interlock the dovetail joints 56 , 58 formed at their circumferential ends; see FIG. 7 . To ensure the collar clamp 48 cannot be raised up off of the diffuser upper lip, two tie bars 70 , 72 clamp down on the collar clamp 48 ; leveraging off of the bottom edge of the diffuser shoulder 44 . Each tie bar has a laterally inwardly extending projection 74 that seats under the diffuser shoulder 44 against which the tie bars 70 , 72 react to maintain the collar clamp 48 pressed against the upper lip of the diffuser opening 46 ( FIG. 5 ). The upper portion of the tie bars is threaded so that nuts can tighten down the tie bars, applying a slight preload. Preferably, these nuts are crimped in place by crushable material built in to the nut or collar clamp 48 .
[0040] A crushable gasket may be employed if needed between the diffuser stack 48 and the diffuser lip to ensure there is no leakage at their interface. In order to prevent the collar clamp from rotating, the diffuser guides 50 are used as support surfaces. The diffuser guides (often called ears) purpose is to help align and aid in the insertion of the inlet mixer 34 during jet pump reassembly. Notches 76 are formed in the underside of the collar clamp that allow the external collar clamp 48 to fit over the ears 50 and down onto the diffuser lip. These notches also prevent the collar from rotating. The ear recesses in the collar clamp may allow some leakage, but only small amounts of bypass flow are likely.
[0041] The hardware shown in the embodiment illustrated in FIG. 5 is light enough that the two stack halves can be delivered remotely using tool poles. Much of the tooling necessary for installation exists, and minimal if any new hardware handling tooling is required. While the current embodiment illustrates one design for clamping the stack halves together, it should be appreciated by those skilled in the art that this invention is not limited to this particular embodiment.
[0042] FIG. 9 illustrates another embodiment for repairing damaged jet pump surfaces and/or reducing/eliminating flow induced vibration. According to the embodiment shown in FIG. 9 , damaged material on the inside diameter of the diffuser is resurfaced. FIG. 10 is a sectional view of the embodiment shown in FIG. 9 . A new internal collar 78 is inserted into the diffuser collar 38 , restoring it to at least its original designed inside diameter, or even narrowing the annular gap between the inlet mixer and the diffuser collar. The originally engineered manufactured tolerance gap for the slip joint between the inlet mixer outside diameter and the diffuser collar is very tight, plus/minus 0.010 inch diametrically. It should be appreciated that the new internal collar may also be structured to form a convergent geometry relative to the outside diameter of the inlet mixer.
[0043] According to another embodiment of the present invention, the inlet mixer is left in place, but the diffuser collar portion 38 of the diffuser is cut and removed. A new casting or spool piece 80 is then secured to the diffuser 36 ( FIGS. 11 and 12 ). This allows the slip joint geometry to be tightly controlled. This spool piece can be a single section (which may require the removal of the inlet mixer for installation) or multiple sections (i.e., like a clam shell) which may allow for the inlet mixer to in situ install. Again, the geometric relationship between the inlet mixer and the diffuser can be structured such that the inlet mixer outside diameter surface and the diffuser inside diameter surface converge.
[0044] While specific embodiments of the invention have been described in detail, it will be appreciated by those skilled in the art that various modifications and alternatives to those details could be developed in light of the overall teachings of the disclosure. Accordingly, the particular embodiments disclosed are meant to be illustrative only and not limiting as to the scope of the invention which is to be given the full breadth of the appended claims and any and all equivalents thereof.
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A method of repairing a slip joint on a jet pump assembly between an inlet mixer and a diffuser, with the diffuser having an opening that receives the inlet mixer with a given spacing between an outside diameter of the inlet mixer and an inside diameter of the opening in the diffuser forming an annulus whose spacing is a product of manufacture and vibration wear. The method comprises the steps of remotely accessing the annulus and narrowing a radial dimension of the annulus.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority to provisional application No. 61/447,096, filed on Feb. 27, 2011, which application is incorporated herein by reference.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not Applicable.
REFERENCE TO SEQUENCE LISTING, A TABLE, OR A COMPUTER PROGRAM LISTING COMPACT DISC APPENDIX
Not Applicable.
BACKGROUND OF THE INVENTION
The present invention relates to a wind blocking device for a convertible automobile and particularly suited for a C6 convertible CORVETTE (model years 2005-present) and a C5 convertible CORVETTE (model years 1997-2004) as manufactured by General Motors. Several wind blocking devices have been manufactured for convertibles and for the C5 and C6 CORVETTE. However, due to deficiencies in the design of the wind blocking panel and its related mounting system, all other wind blocking devices for the C5 and C6 CORVETTE require the wind blocking device to be removed in order to operate the convertible top between the open and closed positions. The present invention, on the other hand, is unique in that it is designed and mounted in such a way that the convertible top can be opened and closed without disturbing the wind blocking device and the present invention also incorporates text or art work which may be abraded onto a solid transparent or translucent wind blocker and then illuminated for dramatic effect.
BRIEF SUMMARY OF THE INVENTION
The present invention provides a wind blocker for a convertible automobile which allows the convertible top to be opened and closed without the necessity of removing the wind blocker. In a preferred embodiment, the wind blocker is made of a transparent or translucent material which is abraded with text or art work and illuminated for a dramatic artistic effect.
The present invention provides a device which comprises a solid panel, bends in the panel to follow the contour of the interior of a convertible C5 OR C6 CORVETTE as manufactured by General Motors, and a means for attaching the panel to such convertible. In one embodiment of the invention, the panel is of a transparent or translucent material with abrasions on the face of the panel and a means of illumination. The subject device is installed in a convertible automobile such that it projects upwards beyond a seat belt tower of the automobile and provides a customized artistic presentation while redirecting airflow through the passenger compartment of the automobile.
BRIEF DESCRIPTIONS OF THE DRAWINGS
FIG. 1 is a preferred embodiment of the panel of the wind blocker.
FIG. 2 is a preferred embodiment of the panel of the wind blocker with various details identified.
FIG. 3 depicts one of the bends in the panel of the wind blocker.
FIG. 4 depicts another of the bends in the panel of the wind blocker.
FIG. 5 illustrates the panel and a portion of a mounting assembly that is used to secure the panel to the convertible automobile.
FIG. 6 further illustrates the panel and a preferred embodiment of the mounting assembly that is used to secure the panel to the convertible automobile.
FIG. 7 illustrates a frame bracket for a convertible automobile.
FIG. 8 illustrates several views of an anchor that is used to secure the frame bracket to the convertible automobile.
FIG. 9 illustrates the panel bracket which is used to secure the panel to the frame bracket.
FIG. 10 illustrates a panel bracket plate which is used to secure the panel to the panel bracket.
FIG. 11 further illustrates the panel bracket which is used to secure the panel to the frame bracket.
FIG. 12 illustrates the method of attaching the anchor to the convertible automobile.
FIG. 13 further illustrates the method of attaching the anchor to the convertible automobile.
FIG. 14 illustrates the method of attaching the frame bracket to the convertible automobile.
FIG. 15 illustrates a modified frame bracket for a convertible automobile.
DETAILED DESCRIPTION OF THE INVENTION
A convertible automobile wind blocking device comprising a solid panel 20 which projects upwards beyond a seat belt tower 18 of the convertible automobile, and that has a face 1 , two first bends 2 an equal distance from a centerline of the panel, two second bends 3 an equal distance from the centerline of the panel, an edge 4 , two sets of mounting holes 5 , a means of attaching the panel 20 to the automobile, an abrasion 19 in the face 1 and a means of illumination. Additionally, the panel has two cutouts 34 arranged to provide clearance for a seat latch of a convertible automobile.
The wind blocking device is made in the following manner. In the preferred embodiment, the panel 20 is made from an acrylic plastic. In the preferred embodiment, the panel 20 is cut and bent into a predetermined shape to fit behind seats of a convertible automobile and generally follow the contour of a rear passenger compartment of the automobile. In the preferred embodiment, the first bends 2 and the second bends 3 are 52 degrees and 48 degrees, respectively. However, it should be understood that any number of angles could be accommodated by the present invention to allow the panel 20 to follow the contour of the rear passenger compartment of the automobile. In the preferred embodiment, the abrasion 19 is customized text and/or an artistic design which is formed in the face 1 of the panel 20 by water pressure, sand blasting or laser etching, which allows each wind blocking device to be custom designed based upon a customer's requirements.
In the preferred embodiment, a means of illumination is a strip of light emitting diodes (LEDs) which are readily known in the art and which are affixed to the edge 4 of the panel 20 . Affixing the LED strip to the edge 4 of the panel 20 allows light to pass through the panel 20 and become diffused at the abrasion 19 such that the abrasion 19 is illuminated to observers. In the preferred embodiment, the means of attaching the panel 20 to the convertible automobile comprises a panel bracket plate 6 , a panel bracket 8 , a frame bracket 12 , an anchor 15 , four screws 9 , two nuts 30 and a bolt 10 . The panel bracket plate 6 comprises a flat metal plate with mounting bosses 7 arranged in such a way as to align with one set of the holes 5 in the panel 20 . The panel bracket 8 comprises a stamped sheet metal plate comprising a bottom tab 23 , a front tab 24 and a side tab 25 , with holes 16 in the front tab 24 arranged in such a way as to align with the mounting bosses 7 of the panel bracket plate 6 and holes 21 arranged in such a way as to align with threaded studs 26 the frame bracket 12 . In the preferred embodiment, the bottom tab 23 and the side tab 25 form an angle of approximately 90 degrees and the bottom tab 23 and the front tab 24 form an angle of approximately 102 degrees. However, it should be understood that any number of angles could be accommodated by the present invention to allow the panel bracket 8 to align with both the panel 20 and the frame bracket 12 . The panel bracket 8 is installed onto the panel 20 by attaching the panel bracket 8 to a front side of the panel 20 with the holes 16 of the panel bracket 8 aligned with one set of the holes 5 of the panel 20 . The panel bracket plate 6 is installed onto the panel 20 by attaching the panel bracket plate 6 to a rear side of the panel 20 opposite the panel bracket 8 with the mounting bosses 7 of the panel bracket plate 6 aligned with one set of the holes 5 of the panel 20 . Screws 9 are affixed to the mounting bosses 7 by installing the screws 9 through the holes 16 in the panel bracket and the corresponding set of holes 5 in the panel 20 . A seat belt tower trim 17 is removed from a seat belt tower 18 pursuant to the manufacturer's directions. An anchor 15 is inserted into an existing slot 27 on the seat belt tower 18 as depicted in FIG. 7 . The seat belt tower trim 17 is then reinstalled on the seal belt tower 18 . The frame bracket 12 comprises a sheet metal stamping which is bent to fit the contours of the seat belt tower 18 of the automobile, two tabs 13 , a hole 22 , a spacer 14 and two threaded studs 26 . The frame bracket 12 is attached to the automobile by placing the frame bracket 12 over the seat belt tower 18 and pressing it down onto the seat belt tower 18 until the tabs 13 engage an edge of the seatbelt tower 18 . A bolt 10 is inserted through the hole 16 and affixed to the anchor 15 . The anchor 15 is adapted to fit snugly inside the existing slot 27 in the seat belt tower 18 . Inserting the bolt 10 into the anchor 15 causes flanges 28 on the anchor 15 to press firmly against inside edges of the existing slot 27 in the seat belt tower 18 . Raised lips 29 on the flanges 27 prevent the removal of the anchor 15 from the existing slot in the seat belt tower 18 without first removing the bolt 10 . The panel bracket 8 is attached to the frame bracket 12 by aligning the holes 21 with the threaded studs 26 and tightening bolts 30 onto the threaded studs 26 such that the panel bracket is situated between the frame bracket 12 and the bolts 30 .
The present invention can be easily adapted to another a-convertible automobile by modifying the frame bracket 12 . A preferred embodiment of the invention for another convertible automobile the is the same as the previous embodiment except that the anchor 15 is not used and the a modified frame bracket 31 is used in place of the frame bracket 12 . The modified frame bracket 31 comprises a sheet metal stamping which is bent to fit the contours of a frame member 11 of a convertible automobile, and two threaded studs 32 . The modified frame bracket 31 is attached to the convertible automobile by attaching two sided high bonding strength tape which is known by one knowledgeable in the art to a bottom 33 of the modified frame bracket 31 and placing the modified frame bracket 31 over the frame member 11 and pressing it down firmly onto the frame member 11 . The panel bracket 8 is attached to the modified frame bracket 31 in the same fashion as the panel bracket 8 is attached to the frame bracket 12 .
Although a preferred embodiment uses a transparent or translucent acrylic panel, it should be understood that the panel 20 of the wind blocking device can be manufactured from any number of materials capable of redirecting air flow through the passenger compartment of the Corvette and which are known in the art, i.e., ABS plastic, plexi-glass, lexan, aluminum, screen mesh, and so forth. Additionally, while the preferred embodiment utilizes an LED strip for illuminating a transparent or translucent panel 20 , it should also be understood that the means of illuminating the abrasion 19 could be any number of means of illumination known in the art and such illumination can be white, a single color, or multi-colored. The means of illumination can be powered by its own independent power source or powered by the automobile's power system. In either case, the means of illumination can utilize its own switch to control the flow of electricity. However, if powered by the automobile's power system, the means of illumination can also be connected to the automobile's electrical system such that the automobile's electrical system controls the flow of electricity such that the means of illumination may be always on, on when the vehicle's ignition switch is in the “accessory” or “on” position, or on when one or more of the automobile's lights are on, such as the parking lights, brake lights or head lights.
Although it is anticipated that the abrasion 19 will be formed by water pressure, sand blasting or laser etching, it should also be understood that the invention is not dependent on any particular manner of forming the abrasion 19 . The formation of the abrasion 19 can be accomplished by any number of methods known to one skilled in the art.
It should be understood that the geometry of the panel 20 in FIG. 1 is based upon the contours of a particular convertible automobile. The geometry of the panel 20 can be manufactured with a wide range of geometries capable of fitting behind passenger seats of the convertible automobile by one skilled in the art. FIG. 5 through FIG. 14 depict the preferred embodiment of the means for affixing the panel 20 to a convertible automobile.
Although the invention has been described in detail with reference to a particular embodiment, it is to be understood that variations or modifications may be made within the spirit and scope of the invention as defined in the appended claims.
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The wind blocker allows the simple and inexpensive manufacture of a wind blocker for the convertible C5 and C6 Corvette which utilizes illuminated text and/or artwork. The design of the wind blocker allows such text or artwork to be quickly and inexpensively applied based on customer requirements. The use of computer aided etching techniques allow the wind blocker to be cost effectively manufactured with custom artwork in quantities as low as one item. This allows the end customer to utilize any artistic design desired to create a completely custom, one-of-a-kind accessory for the customer's C5 or C6 Corvette.
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This is a continuation application of Ser. No. 07/997,824 filed Dec. 29, 1992, now abandoned.
TECHNICAL FIELD
The present invention is generally directed to apparatus and methods of freezing food using a liquid refrigerant. The food is contacted with the refrigerant under conditions generating a turbulent flow to provide more efficient freezing and better separation of the individual pieces of food.
BACKGROUND OF THE PRIOR ART
The freezing of food using a liquid refrigerant, such as liquid nitrogen, has been practiced on a commercial scale for several years. A typical commercial freezing process begins by placing the food onto a continuous conveyor. The conveyor travels into a bath of the liquid refrigerant in a manner which immerses the food in the liquid refrigerant. The frozen food is removed from the bath by the conveyor and sent for further freezing, processing and packaging.
Processes by which food is immersed in a relatively fixed bath of liquid refrigerant are disadvantageous because the food product in the form of individual pieces of food tend to be frozen together. This requires a mechanical separation procedure which can damage the food, particularly delicate food products such as shrimp, scallops, clams and the like.
Such processes are also disadvantageous because large loses of the liquid refrigerant result from the passage of the conveyor into and out of the bath. The conveyor is continuously being cooled upon entry into the bath and warmed upon exiting the bath. As a result, large quantities of the liquid refrigerant are consumed in the process adding significantly to the cost of freezing.
Another method of freezing food employs a tunnel freezer. The food product is placed onto a continuous conveyor which enters a thermally insulated box equipped with fans. Liquid refrigerant is injected into the insulated box and vaporizes thereby cooling the interior of the insulated box. The fans within the insulated box circulate the cold vapor and convectively freeze the food.
Tunnel freezers of the type described above are disadvantageous because the convective cooling process is relatively slow. In addition, a relatively large insulated box is needed, increasing the cost of the freezer and occupying valuable processing area.
Tunnel freezers are also disadvantageous because like the immersion freezers described above, if the pieces of food are not separated prior to entering the freezer, they must be mechanically separated after the freezing operation. In addition, wet and delicate food products such as shrimp, scallops, clams and the like tend to stick to the conveyor, requiring mechanical removal thereof. The implementation of mechanical devices to separate pieces of food from each other and/or from the conveyor may cause damage to delicate food products.
More recently, methods of freezing have been disclosed, particularly for freezing liquids such as creams, liquid egg and the like, in which a liquid refrigerant flows through inclined channels provided by a trough.
Peter H. Gibson et al., U.S. Pat. No. 4,479,363 disclose a process for freezing a liquid in which the liquid is passed into or onto a stream of liquified gas along an inclined channel. The stream of liquified refrigerant is characterized by a laminar flow and the patent states that turbulent flow is to be avoided.
Peter H. Gibson, U.S. Pat. No. 4,843,840 discloses a process for freezing liquid food products using a channeled conduit to convey the liquid refrigerant. A smooth, non-turbulent flow of the liquid refrigerant is required to achieve uniformity in and control over both the size of product and the extent to which the food product is cooled.
Despite the benefit achieved by these methods, there is still the need for processes of freezing food which at least substantially reduce the freezing of solid pieces of food together and which freezes the food product in an even more cost efficient manner.
SUMMARY OF THE INVENTION
In accordance with the present invention it has been discovered that a freezer comprising at least one inclined channel formed by a trough is particularly adapted for the freezing of food, especially hard and soft solid food, when a liquid refrigerant is transported along the channel(s) under turbulent flow conditions.
The present invention is generally directed to an apparatus and method for freezing food products in the form of individual pieces of food using a liquid refrigerant in which the food is frozen in a more efficient manner and the individual pieces of food do not stick together as they proceed through the freezing operation. In accordance with the invention, there is provided, in its broadest aspect, a continuous method of freezing food, especially solid pieces of food, comprising supplying the individual pieces of food to a conveyor means, contacting the pieces of food on the conveyor means with a liquid refrigerant under conditions of turbulent flow to thereby freeze at least the outer surface of the food product, and separating the individual frozen pieces of food from the liquid refrigerant.
The apparatus is constructed to insure that the liquid refrigerant contacts the food product under turbulent flow conditions. As used herein the term "turbulent flow" shall mean that the velocity of the flow of liquid refrigerant at a given point varies erratically in magnitude and direction over time. Laminar flow, which is typical of prior art processes, provides a streamline non-erratic flow at a given point over time.
The manner in which the turbulent flow is provided can vary. For example, the conveyor means may be provided with an uneven surface in the direction of the flow path of the liquid refrigerant. This uneven surface may be in the form of spaced apart raised ridges. In addition, or alternatively, the conveyor means may comprise a plurality of individual conveyors arranged in the form of a tier in which the liquid refrigerant falls from the forward end of one conveyor to the rear end of the conveyor next below it. The force under which the liquid refrigerant contacts the rear end of each conveyor being sufficient to generate a turbulent flow through at least a portion of the flow path within the freezer.
Other methods of creating a turbulent flow may be employed in the present invention and include, for example, causing the liquid refrigerant to enter the freezer under turbulent flow or by feeding the food product to the freezer in a manner which creates a turbulent flow in the liquid refrigerant.
Turbulent flow provides several benefits over freezing food products using a stationary bath of liquid refrigerant or using a laminar flow of liquid refrigerant. First, turbulent flow mixes the food product with the liquid refrigerant in a manner which achieves more uniform freezing. Second, turbulent flow at least substantially reduces the incidence of individual pieces of food sticking together. Third, turbulent flow increases the rate of freezing which improves the quality of the food product and reduces the cost of freezing including reducing the size of the freezer.
BRIEF DESCRIPTION OF THE DRAWING
The following drawings are illustrative of embodiments of the invention and are not intended to limit the invention as encompassed by the claims forming part of the application.
FIG. 1 is a schematic view of one embodiment of the invention employing a single conveyor for freezing individual pieces of food under turbulent flow conditions;
FIG. 2A is a side view of the conveyor shown in FIG. 1 having spaced apart elevated ridges adapted to create a turbulent flow of the liquid refrigerant;
FIG. 2B is a plan view of the conveyor shown in FIG. 1;
FIG. 2C is a front view of the conveyor shown in FIG. 1;
FIG. 2D is a front view of a conveyor having multiple channels;
FIG. 3 is a partial schematic view of the separation section of the embodiment shown in FIG. 1;
FIG. 4 is a top view of the conveyor used in the separation section shown in FIG. 3; and
FIG. 5 is a schematic view of another embodiment of the invention employing multiple conveyors arranged in a tier for freezing individual pieces of food under turbulent flow conditions.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the drawings and particularly to FIG. 1, there is shown an embodiment of the freezer of the present invention using a single conveyor in the form of a trough having a single channel for contacting the food product in the form of individual pieces of food with the liquid refrigerant. The freezer 2 includes a food entry section 4, a liquid refrigerant entry section 6, a freezing section 8, a separation section 10 where the liquid refrigerant and frozen food are separated and a frozen food exit section 12 where the frozen food is discharged from the freezer 2.
The food entry section 4 includes a conveyor means which may be, for example, a conveyor belt 14 for transporting individual unfrozen pieces of food from a source (not shown) to an entry port 16 opening into the freezer 2. The pieces of food are transported by the conveyor belt 14 and fall off the end 18 thereof onto a trough 20 having a rear end 22 for receiving the food product and a forward end 24 defining a channel 21 (see FIG. 2C) for transporting the liquid refrigerant and the food product as it undergoes freezing. The distance from the entry port 16 to the trough 20 is preferably sufficient so that the impact of the food product on the liquid refrigerant contained in the trough 20 is sufficient to generate a turbulent flow. Typically, the distance from the entry port 16 to the trough 20 is from about 6 to 24 inches.
The trough is adapted to house a flow of liquid refrigerant and the food product as the food product becomes frozen and to transport the same to the separation section 10.
Primary freezing of the food product, where at least the outer surface of the food is frozen, occurs in the trough 20. Secondary freezing of the interior portions of the food product may occur in the trough 20 or in an additional freezer (not shown) after the food passes out of the exit section 12 of the freezer 2.
The extent to which the individual pieces of food are frozen is dependent on the residence time of the food product in the liquid refrigerant, the depth of the liquid refrigerant and the temperature of the food entering the freezer.
The residence time of the food product within the liquid refrigerant is dependent on the length of the trough and its angle of inclination θ. The longer the trough, the greater the time the food product will be in contact with the liquid refrigerant and, therefore, the greater the extent of freezing. Conversely, as the angle of inclination θ increases, the time the food product is in contact with the liquid refrigerant decreases resulting in a lesser degree of freezing. The preferred angle of inclination is from about 0.5° to 5.0°.
The depth of the liquid refrigerant is also a factor in the freezing of the food product. The depth of the liquid refrigerant should be sufficient to allow all sides of the food product to be in contact with the liquid refrigerant for a time sufficient to freeze at least the outer surface thereof. It is desirable to maintain the depth of the liquid refrigerant within the range of from 0.5D to 2.0D, preferably 0.5D to 1.5D, where D is the maximum thickness of the food product.
The temperature of the food product entering the freezer 2 is another factor when considering the freezing of a food product in accordance with the present invention. The higher the temperature of the food product entering the freezer 2, the greater the heat which must be removed to freeze at least the outer surface thereof. Accordingly, foods at relatively high temperatures, e.g. at least 50° F., require a greater length of time in contact with the liquid refrigerant than food products entering the freezer at lower temperatures.
By way of example, a food product having a temperature of 30° to 50° F. and a maximum thickness of from about 0.25 to 0.75 inch (e.g. diced chicken) can be frozen, in accordance with the present invention, in a trough having a length of from about 5 to 15 feet, an angle of inclination of about 0.5° to 5°, and a depth of liquid refrigerant of from about 0.125 to 1.5 inches.
In accordance with the present invention, the flow of liquid refrigerant within the trough 20 is turbulent which improves the efficiency of cooling and keeps the individual pieces of food separated. Turbulent flow may be obtained by providing the base 30 of the trough 20 with an uneven surface. In this regard, the base 30 may be provided with a plurality of spaced apart ridges 34 extending between the opposed walls 26, 28 and transverse the flow path of the liquid refrigerant. One such design which accomplishes this purpose is shown by reference to FIGS. 2A-2C where the ridges 34 are comprised of a front side 36 facing the flow of liquid refrigerant and a rear side 38. The front side 36 is angled with respect to the base 30 and rises to an apex 40 while the rear side 38 is substantially perpendicular to the base 30. The flow of the liquid refrigerant over the ridge creates turbulence when the liquid refrigerant hits the base 30 after dropping from the apex 40. Other means of modifying the flow path along the base 30 to create turbulent flow would be obvious to one of ordinary skill in the art.
The ridges 34 are spaced apart to generate the turbulent flow of the liquid refrigerant. It is preferred that the distance between the ridges 34 be in the range of from about 5.0D to 15.0D, where D is the maximum thickness of the food product as shown best in FIG. 2B.
In another embodiment of the invention, as shown in FIG. 2D, multiple channels 21a and 21b are provided which are separated by a divider 35. Multiple channels 21a and 21b are desirable when different types of products or different sizes of the same food product are to be frozen and must remain separated at least through the freezing process. For example, multiple channels may be employed when freezing different sized shrimp. It is understood that the separation of the shrimp into different sizes may occur prior to their transportation to the freezer of the present invention.
Liquid refrigerant is supplied to the trough 20 at its rear end 22 from a sump 42 located beneath the separation section 10 which is used to capture reclaimed liquid refrigerant as explained hereinafter. A pump 44 transfers liquid refrigerant from the sump 42 through a conduit 46 into a reservoir 48 which is located proximate to the rear end 22 of the trough 20.
The reservoir 48 is separated from the rear end 22 of the trough 20 by a wall 50. As the liquid refrigerant is delivered to the reservoir 48, it overflows the wall 50 and falls into the trough 20. The height of the wall 50 can be set to provide for a sufficient drop of the liquid refrigerant to create a turbulent flow in the trough 20. The height of the front wall 50 for creating a turbulent flow is typically within the range of from about 3 to 12 inches.
The separation section 10 is adapted to separate the liquid refrigerant and the frozen food obtained from the forward end 24 of the trough 20. As shown best in FIGS. 3 and 4, the separation section 10 includes a conveyor belt 52 having a base 54 with perforations 56 therein (shown best in FIG. 4) extending from a rear end 58 to a forward end 60.
The rear end 58 lies below the forward end 24 of the trough 20 and therefore is adapted to receive the liquid refrigerant and frozen pieces of food from the trough 20. The perforations 56 in the base 54 are sufficiently large to enable the liquid refrigerant to pass therethrough, yet small enough so that the individual pieces of food remain on the base 54. The liquid refrigerant, therefore, passes through the conveyor belt 52 into the sump 42 for recirculation.
The frozen pieces of food remaining on the conveyor belt 52 are transferred to the frozen food exit section 12 comprised of an opening 62 within the freezer 2 remote from the entry port 16. The frozen food is conveyed through the opening 62 for further processing, freezing, and/or packaging (not shown).
During the freezing process, some of the liquid refrigerant contained within the trough 20 will boil off which may require replacement of the liquid refrigerant during its travel from the rear end 22 to the forward end 24 of the trough 20. Referring to FIG. 1, the replacement liquid refrigerant may be supplied from a liquid refrigerant tank 65 via a conduit 64 through a flow control valve 66. The liquid refrigerant is distributed along at least a portion of the length of the trough 20 by a header 68 comprising a plurality of spaced apart outlets 70 through which the liquid refrigerant passes into the trough 20.
The header 68 is preferably spaced apart from the base 30 of the trough 20 by a distance such that entry of the replacement liquid refrigerant into the trough 20 will create a turbulent flow therein. The distance between the header 68 and the base 30 to create turbulent flow of the liquid refrigerant is typically about 2 to 6 inches.
The opening and closing of the flow control valve 66 is controlled by a sensor 72 which detects the level of the liquid refrigerant in the sump 42 such as through the use of a float 74. When the level in the sump 42 decreases, the sensor 72 detects the downward movement of the float 74 and transmits an electrical signal through an electrical connection (not shown) to the valve 66 which moves to the open position. This allows supplemental liquid refrigerant to be supplied to the trough 20 from the tank 65 until the sensor 72 detects a termination in the decrease of the level of liquid refrigerant in the sump 42.
There will be some loss of liquid refrigerant due to boil off caused by the freezing of the food product at various sections of the freezer. The losses of liquid refrigerant during the freezing process can be made up by adding liquid refrigerant to the sump 42 and/or the header 68 from the tank 65 or other source of liquid refrigerant.
The type of food which may be frozen in accordance with the present invention is generally unlimited and includes both solid and liquid foods including chicken parts, diced chicken meat, fruits, vegetables, diced clams, shrimp, scallops and oysters and the like.
The type of liquid refrigerant which may be used must meet safety requirements for processing of food. Liquid nitrogen is the preferred liquid refrigerant because of its relatively low cost.
In another embodiment of the invention, turbulent flow is provided by employing multiple conveyors within the freezer section such that the liquid refrigerant and processed food "drop" from one conveyor to another.
Referring to FIG. 5, there is shown a freezer 80 having a series of three troughs 82a-82c each angled downwardly by an angle θ of about 0.5° to 5° to create a flow of both liquid refrigerant and food product from the rear end 84 of an upper trough (i.e. trough 82a) to the rear end 86 of the next trough (i.e. 82b) in sequence until the liquid refrigerant and the frozen food product are passed into a separation section 88. As described in connection with FIG. 1, the separation section 88 includes a conveyor belt 90 having a base 92 with perforations 94 therein (see FIG. 4) allowing the liquid refrigerant to pass into a sump 96 and the frozen food to proceed out of the freezer through the exit 95.
The liquid refrigerant is supplied from the sump 96 to the rear end 84 of the topmost trough 82a via a pump 98, through a conduit 100 and through a spray header 102. the latter device creates a spray of the liquid refrigerant of sufficient force to create a turbulent flow in the trough 82.
The pieces of food to be frozen enter the freezer 80 through an opening 104 from a conveyor (not shown) as previously described in connection with FIG. 1. The distance the pieces of food fall through the opening 104 and into the trough 82 may create a turbulent flow where the pieces of food contact the liquid refrigerant. The distance from the opening 104 to the trough 82a is typically from about 6 to 24 inches.
One or more of the troughs 82a-82c may be provided with spaced apart ridges, as shown and described in connection with FIGS. 1 and 2A-2D, to generate a turbulent flow or to maintain the turbulent flow generated by the multiple troughs 82a-82C.
EXAMPLE 1
Diced chicken measuring approximately one-half inch on all sides is fed to a freezer of the type shown in FIG. 1. The freezer has the capacity to freeze 1,000 pounds of diced chicken per hour. The pump 44 connected to the sump 42 must deliver a flow rate of liquid refrigerant (e.g. liquid nitrogen) of approximately 40 gallons per minute.
The trough 20 measures 10 feet in length from the rear end 22 to the forward end 24. The trough 20 is provided with ridges 34 at 5 inch intervals. The ridges measure 0.5 inch in height (see FIG. 2C).
The heat removed from the chicken is approximately 25 BTUs per pound and the flow rate of make up liquid nitrogen is approximately 333 pounds per hour which is supplied to the sump 42 from a source of liquid nitrogen.
EXAMPLE 2
The same chicken product used in Example 1 is sent to a freezer of the type shown in FIG. 5. The chicken product was fed to the freezer at the rate of 1,000 pounds per hour requiring a flow rate of liquid nitrogen of approximately 40 gallons per minute.
Each of the troughs 82a-82c are 10 feet long and the passage of the chicken along the three troughs results in a heat loss from the chicken of 50 BTUs per pound. The flow rate of liquid nitrogen to make up lost refrigerant is approximately 666 pounds per hour.
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Method and apparatus for continuously freezing a food product in which the food product is contacted on a conveyor with a liquid refrigerant under conditions of turbulent flow to thereby freeze at least the outer surface of the food product. The frozen food product and the liquid refrigerant are thereafter separated.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to mounting arrangements for electronic equipment to be mounted in a rack mounting system and more particularly, to such systems suitable for mounting data communication devices.
2. Description of the Prior Art
Communication devices are typically constructed so as to be mounted in standard size racks. Each rack includes first and second vertical supports which are spaced by a standard opening width. For example, the racks commonly used by the telephone companies have a width of 23 inches, whereas the racks typically used by end users of telephone services have a rack opening of 19 inches.
Various communication equipment is typically constructed so as to fit between and be mounted within one of the standard size racks.
Additionally, the prior art includes various shelves constructed to fit within a standard rack, wherein the shelf has various slots defined therein for receiving equipment.
Also, it is commonly known to mount an item of electrical communication equipment on a vertical surface, such as a vertical wall of the phone terminal room of an end user.
It would be desirable to have a mounting system for data communication devices that would provide improved flexibility and allow the equipment to be mounted in multiple modes in each of the environments mentioned above
SUMMARY OF THE INVENTION
The present invention, in a first embodiment, provides a data communication system constructed to be mounted in a rack having a rack width defined between first and second supports. The system includes first and second equipment boxes, each box having a box width less than one-half of the rack width. The first and second boxes are structurally connected together to form a two box structure having a combined width less than the rack width. First and second mounting brackets are connected to the first and second boxes, respectively, for attaching the two box structure to the first and second supports of the rack.
The mounting brackets have two alternative mounting positions which allow the two box structure to be selectively mounted in either of the two alternative rack widths.
Additionally, either one of the boxes may be mounted on a vertical surface such as a wall utilizing the two mounting brackets.
Further flexibility is provided by the alternative use of a second set of mounting brackets which allows a single one of the boxes to be mounted within a standard rack.
In another embodiment, the invention includes a data communication apparatus which includes a battery box having a hinged front door. A chassis is mounted on the door of the battery box. The chassis has a face oriented transversely to the door. The face includes an opening for receiving a plurality of data communication cards therein. Access to the data communication cards can be achieved when the battery box is mounted on a wall in close proximity to other devices, by pivoting the door to swing the chassis away from the other devices.
In another embodiment of the invention, an enclosure for data communication equipment is provided which includes a six sided rectangular box. Two oppositely facing sides of the box include a plurality of mounting holes, which plurality of mounting holes includes a first pattern for mounting the box on a planar surface, a second pattern for mounting the box in a rack, and a third pattern for mounting a power supply on the box.
In yet another embodiment of the invention, a system is provided for mounting one or more electrical equipment enclosures in a plurality of alternative arrangements. The system includes at least one electrical equipment enclosure and a plurality of alternative mounting brackets which provide numerous alternative arrangements. A first bracket selection and arrangement provide side by side dual mounting of two enclosures within a first rack having a first rack width. A second bracket selection and arrangement provides side by side dual mounting of two enclosures within a second rack having a second rack width greater than the first rack width. A third bracket selection and arrangement provides a single mounting of one enclosure in the first rack. A fourth bracket selection and arrangement provides a single mounting of one enclosure in the second rack. A fifth bracket selection and arrangement provides a single mounting of one enclosure on a planar surface.
In another embodiment of the invention, a lockable communications device enclosure is provided, which includes an enclosure having a face with one or more openings defined therein for receiving a plurality of communication cards therein. The face has a first engagement surface defined thereon. A retaining structure retains the communication cards within the enclosure. The retaining structure extends across the one or more openings and includes a second engagement surface defined thereon complementary to the first engagement surface so that the first and second engagement surfaces can interlock. A tool actuated fastener detachably connects the retaining structure to the enclosure with the first and second engagement surfaces in interlocked position.
It is therefore, an object of the present invention to provide improved alternative mounting arrangements for data communication devices.
Another object of the present invention is the provision of a mounting system wherein first and second boxes, structurally connected together to form a two box structure, can be mounted within a standard rack.
And another object of the present invention is the provision of a system wherein such a two box structure has two alternative mounting positions in either of two alternative standard rack widths.
And another object of the present invention is the provision of a data communication apparatus including a chassis mounted on a hinged front door of a battery box, whereby access to devices contained in the chassis can be achieved by pivoting the door to swing the chassis away from other devices mounted adjacent the battery box.
And another object of the present invention is the provision of a lockable communications device enclosure apparatus including improved means for retaining data communication devices within an enclosure.
Other and further objects, features and advantages of the present invention will be readily apparent to those skilled in the art upon a reading of the following disclosure when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic illustration of a single box data communications system connected between a network and end user devices, such as telephones.
FIG. 2 is a perspective view of a single data communication card which could be received within the single box structure like that of FIG. 1 .
FIG. 3 is an exploded perspective view of the single box structure of FIG. 1 .
FIG. 4 is a plan view of a first mounting bracket having a shorter leg and a longer leg.
FIG. 5 is an elevation view of the shorter leg of the bracket of FIG. 4 .
FIG. 6 is an elevation view of the longer leg of the bracket of FIG. 4 .
FIG. 7 is a plan view of alternative mounting bracket utilized to mount a single box within a standard rack mount system.
FIG. 8 is an elevation view of the longer leg of the bracket of FIG. 7 .
FIG. 9 is an elevation view of the shorter leg of the bracket of FIG. 7 .
FIG. 10 is a front elevation view of a two box structure mounted within the standard 19 inch wide rack.
FIG. 11 is a front elevation view of a two box structure mounted within a standard 23 inch width rack.
FIG. 12 is a side elevation view taken along line 12 — 12 of FIG. 10 .
FIG. 13 is a front elevation view of a single box structure mounted within a standard rack of either dimension.
FIG. 14 is an elevation view of a single box structure mounted on a vertical surface such as a wall.
FIG. 15 is a perspective view of a single box structure mounted on a vertical hinged door of a battery box which is in turn mounted on a vertical wall.
FIG. 16 is a perspective view of a locking bar.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 illustrates in schematic form a data communications system 10 having a single box enclosure 11 for data communication equipment, such as data communication cards 12 , 14 , 16 and the like.
The data communication system 10 is typically connected to public communications network 18 by communications line 20 which may, for example, be a standard T 1 line. The data communication system 10 will in turn be connected by a plurality of telephone lines 22 to individual telephones 24 at the user's facility. It will be understood that the data communication system 10 might also be connected to other devices at the user's facility.
One of the communication cards, such as card 12 is shown in perspective view in FIG. 2 .
The present invention deals primarily with the construction of the enclosure 11 in combination with various arrangements of mounting brackets which allow one or two of the enclosures 11 to be mounted in a plurality of ways.
For example, FIG. 10 shows side by side mounting two enclosures, which have been designated as 11 A and 11 B, within a rack 26 having a rack width 28 . The rack 26 is constructed of two vertical members 30 and 32 . The rack 26 illustrated in FIG. 10 may, for example, be a standard communications device rack having a width 28 of 19 inches, such as is commonly utilized by end users of communications equipment. The enclosures 11 A and 11 B are mounted within the rack 26 by first and second brackets 34 and 36 which are further described below with regard to FIGS. 4-6.
FIG. 11 illustrates a second mounting arrangement for the two enclosures 11 A and 11 B between vertical members 40 and 42 of a rack 38 having a rack width 44 which is greater than the rack width 28 . Rack 38 may for example be a standard 23 inch wide rack such as is conventionally used by telephone companies. As will be further described below, the same two brackets 34 and 36 are utilized in FIG. 11, but in a different orientation than they were utilized in FIG. 10 .
In still another possible mounting arrangement for one of the enclosures 11 , as shown in FIG. 13, the same may be mounted within either of the racks 26 or 38 in a single enclosure arrangement utilizing a different set of brackets 46 and 48 which are further described below with regard to FIGS. 7-9. By choice of the dimensions of brackets 46 and 48 , a single box mounting arrangement may be utilized in either the narrower rack 26 or the wider rack 38 of FIGS. 10 and 11, respectively.
Finally, FIG. 14 illustrates still another mounting arrangement for a single one of the enclosures 11 wherein the same is mounted on a vertical surface, such as wall 50 , by use of the first and second brackets 34 and 36 .
The details of construction of one of the enclosure boxes 11 is shown in the exploded view of FIG. 3 . The enclosure 11 can be described as a six sided rectangular box, two oppositely facing sides 52 and 54 of which include a plurality of mounting holes as best seen on side 52 in FIG. 3 . As will be further described below, those mounting holes are arranged in a plurality of patterns to provide for alternative mounting of the enclosure on various support structures. The first and second sides 52 and 54 may be referred to as the left and right lateral sides when the enclosure 11 is mounted in a horizontal manner as shown in FIG. 10 . The enclosure box 11 further includes a front side 56 , a rear side 58 , a top side 60 and a bottom side 62 .
The rear side 58 receives a backplane board 64 having slots such as 66 for receiving the plug-in connectors of the communications card such as 12 in a conventional manner. The rear side 58 is closed by a rear cover 68 and an access panel 70 .
The front side 56 , which may also be referred to as a face 56 , is generally open to and defines a plurality of opening slots, such as 72 and 74 , for receiving data communication cards such as 12 , 14 , 16 and the like therein.
Referring now to FIGS. 4, 5 and 6 , the details of construction of mounting bracket 34 are shown. The mounting bracket 36 is identical.
As shown in the plan view of FIG. 4, the bracket 34 is constructed in a right angle shape having an apex 76 and having a shorter leg 78 and a longer leg 80 .
As seen in FIG. 5, the shorter leg 78 has two oval shaped bolt holes 82 and 84 defined therein which can be described as a rack bolt pattern 82 , 84 . As can be seen, for example, in FIG. 10, the short leg 78 engages the vertical member 30 of rack 26 and the bracket 34 is attached to the rack 26 by bolts (not shown) extending through the oval shaped bolt holes 82 and 84 .
The short leg 78 also includes three smaller bolt holes 86 , 88 and 90 which can be described as a box bolt pattern 86 , 88 , and 90 which will be utilized to bolt the short leg 78 to the box 11 when the bracket 34 is reoriented in the manner shown in FIG. 11 .
Similarly, the longer leg 80 shown in FIG. 6 includes a rack bolt pattern made up of oval bolt holes 92 and 94 which are utilized to bolt the bracket 34 to the vertical member 40 of rack 38 when in the orientation shown in FIG. 11 . The longer leg 80 also includes a box bolt pattern made up of three smaller bolt holes 96 , 98 and 100 which are utilized to bolt the longer leg 80 to the box structure 11 when the bracket 34 is in the orientation shown in FIG. 10 .
As can be seen in FIGS. 5 and 6, each of the box bolt patterns made up of three smaller bolt holes are spaced identical distances 102 and 104 from the apex 76 . As is also apparent in comparing FIGS. 5 and 6, the rack bolt patterns of the shorter and longer legs 78 and 80 are spaced different distances 102 and 106 from the apex 76 . The different between distances 102 and 106 is equal to one-half of the difference between the two alternative rack widths 28 and 44 . Thus, if the rack widths are 19 and 23 inches, as would be the case for two commonly used standard racks as previously described, then the difference between distance 102 and 106 would be two inches.
Furthermore, as seen in FIG. 6, the longer leg 80 includes four additional bolt holes 108 , 110 , 112 and 114 which can be described as an alternative box bolt pattern 108 , 110 , 112 , 114 for allowing one of the boxes 11 to be mounted on a planar surface such as wall 50 with the first and second mounting brackets 34 and 36 . The use of this alternative box bolt pattern can be better understood with reference to FIG. 3, and an examination of the various bolt holes found in the left side wall 52 of box 11 .
Each of the left and right side walls 52 and 54 of box 11 can be described as including a plurality of mounting holes, which plurality of mounting holes includes a first pattern made up of mounting holes 116 , 118 , 120 and 122 for mounting the box 11 on a planar surface, such as wall 50 .
The plurality of mounting holes of the left side 52 further includes a second pattern made up of mounting holes 116 , 118 and 132 for mounting the box 11 in one of the racks of FIG. 10 or 11 .
The left side wall 52 further includes a third pattern of mounting holes including holes 134 , 136 , 138 and 140 for mounting a power supply 142 (see FIG. 15) on the box 11 .
The long leg 80 of bracket 34 can be mounted on left side wall 52 with the short leg 78 oriented flush with the bottom wall 62 and with the bolt holes 108 , 110 , 112 and 114 aligned with corresponding bolt holes 116 , 118 , 120 and 122 . The bracket 34 will of course, be attached to the side wall 52 by bolts or machine screws fitted through the bolt hole patterns just described. With brackets 34 and 36 mounted on either side wall 52 and 54 of the box 11 in the manner just described, the box 11 can then be mounted on a planar surface, such as vertical wall 50 in a manner shown in FIG. 14, wherein wall bolts would extend through the oval holes 82 and 84 of brackets 34 and 36 .
Referring again to FIG. 10, the structure illustrated therein can be described as a data communication system constructed to be mounted in the rack 26 having the width 28 defined between the first and second supports 30 and 32 . The data communications system includes first and second equipment boxes 11 A and 11 B. Each box has a box width, such as 122 less than one-half of the rack width 28 . The first and second boxes 11 A and 11 B are structurally connected together by a pluarality of screws (not shown), which extend through aligned threaded holes such as 127 , 129 , 131 and 133 seen in FIG. 3 . The screws are inserted from inside one enclosure 11 A and threaded through the holes into the corresponding holes of the adjacent enclosure 11 B. Thus, the first and second boxes 11 A and 11 B are structurally connected together to form a two box structure having a combined width less than the rack width 28 . The first and second mounting brackets 34 and 36 are then connected to the first and second boxes 11 A and 11 B, respectively, for attaching the two box structure to the first and second supports 30 and 32 of the rack 26 .
As is apparent in viewing both FIGS. 10 and 11, the mounting brackets 34 and 36 have two alternative mounting positions which allow the two box structure 11 A, 11 B to be selectively mounted in either of the two alternative racks 26 or 38 having rack widths 28 or 44 , respectively.
The mounting brackets 46 and 48 utilized to mount a single box structure within one of the standard rack arrangements are shown in greater detail in FIGS. 7-9. FIG. 7 is a plan view showing the mounting bracket 46 having a shorter leg 158 and a longer leg 160 , which meet at an apex 162 .
As seen in FIG. 8, the longer leg 160 includes a pair of oval shaped holes 164 and 166 for attachment to the vertical members of one of the mounting brackets. As seen in FIG. 9, the shorter leg 158 includes three smaller mounting holes 168 , 170 and 172 for attachment to the box 11 .
Referring now to FIG. 15, another possible mounting arrangement for the box 11 is shown.
FIG. 15 illustrates a single box 11 mounted on a hinged front door 174 of a battery box 176 which is in turn mounted on a vertical surface, such as the wall 50 .
It will be understood for example, that the communications device 11 shown in FIG. 15 might be mounted with the battery box 176 in order to provide battery backup in the event of a power failure on the local utility grid. The system shown in FIG. 15 includes the box 11 , which might also be referred to as a chassis 11 mounted on the hinged front door 174 of the battery box 176 . The chassis has a face, such as front face 56 previously described, which is oriented transversely to the door 174 . Face 56 includes openings such as 72 , 74 and the like defined therein for receiving a plurality of data communication devices, such as 12 , 14 and the like therein as shown in FIG. 3 .
The box 11 will be mounted on the door 174 in the same manner as described with reference to FIG. 14, utilizing the brackets 34 and 36 which cannot be seen in the view of FIG. 15 .
Additionally, an external power supply and charger 142 is mounted on one side of the chassis 11 as seen in FIG. 15 .
It will be understood that the system illustrated in FIG. 15 might be mounted on the wall 50 of a utility closet at the user's facility, and quite often there will be a great deal of other electrical equipment also mounted on the wall 50 in close proximity to the battery box 176 .
With the system illustrated in FIG. 15, the front door 174 can be pivoted along vertical hinge 178 to move the battery box 11 away from the wall 50 to provide access to the devices 12 and 14 received therein. If the box 11 could not be so pivoted, it could be very difficult to remove and replace the devices 12 and 14 if another electrical apparatus were mounted on the wall 50 in close proximity to the open front 56 of box 11 .
As previously noted, the front side 56 of box 11 has openings such as 72 and 74 defined therein for receiving a plurality of data communication devices, such as 12 , 14 , 16 and the like within the box 11 . Those devices are not illustrated in FIG. 15, but are shown in FIG. 3 .
Another new feature of the enclosure box 11 is the provision of means for retaining the data communication devices, such as 12 , 14 and 16 within the box 11 . This feature is provided by a retaining bracket 144 best seen in FIG. 16 .
The retaining bracket 144 includes two hooks 146 and 148 defined on its side, and a tab 156 on its right hand end. The box 11 includes two holes 150 and 152 defined therein, and includes an ear 130 with a slot 128 therein. The holes 150 and 152 and hooks 146 and 148 are complementary shaped. Also the tab 156 fits in slot 128 . After the communication devices 12 , 14 , 16 and the like are placed within the open front 56 of the box 11 , the retaining bracket 144 can be placed across the front of the communication devices, and the hooks 146 and 148 engaged with the slots or openings 150 and 152 in the box 11 , and the tab 156 received in slot 128 . The retaining bracket 144 is then detachably connected to the box 11 by fastener 154 which may be a threaded lock screw.
The slots 150 and 152 defined in box 11 may be described as engagement surfaces 150 and 152 , and the hooks 146 and 148 defined on retaining bracket 144 may be described as second engagement surfaces which are complementary to the slots 150 and 152 , so that the hooks and slots can interlock. The threaded fastener 154 in turn can retain the bracket 148 in place, with the hooks and slots in their interlocked positions.
Preferably, the threaded fastener 154 is constructed to be actuated or engaged with a tool, such as a screwdriver or an allen wrench, and can be described as a tool actuated fastener 154 .
Thus, it is seen that the apparatus of the present invention readily achieves the ends and advantages mentioned as well as those inherent therein. While certain preferred embodiments of the invention have been illustrated and described for purposes of the present disclosure, numerous changes in the arrangement and construction of parts may be made by those skilled in the art, which changes are encompassed within the scope and spirit of the present invention as defined by the appended claims.
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A mounting system is provided whereby a data communications system can be mounted in a plurality of different ways in one or more standard size rack openings and on planar surfaces. A first bracket selection and arrangement provides side by side dual mounting of two closures within a first rack having a first rack width. A second bracket selection and arrangement provides side by side dual mounting of two enclosures within a second rack having a second rack width greater than the first rack width. A third bracket selection and arrangement provides a single mounting of one enclosure in the first rack. A fourth bracket selection and arrangement provides a single mounting of one enclosure in the second rack. A fifth bracket selection and arrangement provides a single mounting of one enclosure on a planar surface.
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FIELD OF THE INVENTION
This invention relates generally to mounting of optical and electro-optical components, either active or passive devices such as diode lasers, light emitting diodes, fiber optic connectors, fiber optic couplers, multiplexers or other components to achieve proper positioning, stability, cooling and electrical connection, and more particularly concerns a simple method and apparatus for providing proper mounting of such devices.
BACKGROUND OF THE INVENTION
Micro devices, either active or passive components, such as light emitting diodes (LED's), laser diodes, phototransistors, photodiode detectors, fiber optic connectors, fiber optic multiplexers, fiber optic couplers and other individual elements or arrays of such optical or electro-optical components have been available and have certain precision physical requirements for enabling their use in a convenient way. Prior devices have addressed themselves primarily to the solution of the problems of electrical connection or of thermal conductivity to prevent excessive temperature rise in the component, or to other particular purposes. Many devices have been put forth which offer solutions to some or all of these problems, often in a relatively expensive or complex manner.
The basic requirements for use of many such micro electro-optical or optical devices are that the device be positioned accurately on a substrate, that it be mechanically secured to the substrate, it may require electrical connections for forward biasing and, if required, for modulation, and that it be in thermal contact with an appropriate heat sink to prevent undesired and excessive temperature rise in the component during use.
SUMMARY OF THE INVENTION
Broadly speaking, this invention satisfies all of the requirements for practical use of micro-chip size optical and electro-optical devices in a very simple and convenient structure.
More specifically, a substrate with a relief pattern of grooves and lands thereon very simply and precisely aligns and holds micro devices Additionally it electrically connects and thermally sinks the active devices. The electrodes on the sides of the electro-optical device make contact in a press fit configuration with confronting electrodes at the sides of the grooves on the substrate. Alternatively, the electrodes may be soldered to the relief pattern electrodes. For passive devices the mounting method will align and hold the device even if no electrical connections are needed.
Alternative embodiments are disclosed which indicate that the method of this invention may be used to create two- or three- dimensional arrays of optical and electro-optical devices on a substrate. Different means are provided for electrically connecting devices to the substrate. Additionally, mounting means for active electro-optical devices and beam deflectors are also disclosed. Further, means for actively removing the heat from the substrate on which are mounted active devices are included.
BRIEF DESCRIPTION OF THE DRAWING
The objects, advantages and features of this invention will be more readily perceived from the following detailed description, when read in conjunction with the accompanying drawing, in which:
FIG. 1 is a partial cross-section of a substrate with optical or electro-optical components, such as laser diodes, mounted therein;
FIG. 2 shows an alternative arrangement for electrical interconnection;
FIG. 3 is a top view of the arrangement of FIG. 2;
FIG. 4 shows an alternative embodiment similar to FIG. 2 for a diode laser component mounted in a groove in the substrate;
FIG. 5 is an end view showing a three-dimensional stair step arrangement for mounting optical or electro-optical components;
FIG. 6 is a partial front view of the structure of FIG. 5;
FIG. 7 is a top, somewhat schematic, view of optical or electro-optical components with beam deflectors, shown in different orientations;
FIG. 8 is a sectional view through cutting plane 8--8 of FIG. 7; and
FIG. 9 is a partial sectional view through a substrate with an active cooling structure.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The term "optical or electro-optical component" will be used herein to refer to any of the optical or electro-optical devices which may be connected to the substrate in accordance with this invention. Alternatively, the terms "device" or "component" may be used. Such devices may be light emitting diodes (LED's), phototransistors and photodiode detectors, among others.
Although many of the illustrations of the manner in which this technology may be used for micro device mounting are given with reference to optoelectronic components such as diode lasers or photodetectors, this mounting technology is not limited to these components. Active devices such as optical transmitters, receivers and modulators, passive devices such as optical multiplexers or demultiplexers, or both, may be used. In addition, this technology is not restricted to individual elements on a substrate. Also contemplated is a groove-within-a-groove to give precise control of one micro element above another, for example, a lens above a diode laser or a lens above a photodetector.
With reference now to the drawing and more particularly to FIG. 1 thereof, there is shown substrate 11 having top surface 12 and a relief pattern formed of lands 13, 14 and 15 defining grooves 16 and 17 therein. On the lands defining the top edges of the grooves are formed electrodes 21 and 22 flanking groove 16 and electrodes 23 and 24 flanking groove 17. These electrodes are formed in a conventional manner such as by vapor deposition or by any other suitable means. Although one embodiment contemplates the lands and grooves to be unitarily formed from a monolithic substrate, it is possible that a different material may be used for the lands which thereby form the grooves.
A device such as a diode laser or photodetector 26, having electrodes 31 and 32 on opposite sides thereof, is mounted in groove 16. Typically the device would be press fit into the groove whereby relatively rigid electrodes 31 and 32 would be in an interference fit with relatively deformable electrodes 21 and 22, thereby not only providing positive, secure mounting but also electrical connection as well. One of electrodes 21 and 22 is common or ground while the other one provides a bias or an appropriate signal, such as for modulation purposes. Similarly, electrodes 33 and 34 of device 27 make electrical and physical contact in groove 17 with respective electrodes 23 and 24 at the shoulders of the groove. It should be noted that the grooves may be formed by suitable means such as sawing, etching or milling the substrate in a precise manner to provide accurate control of the width and depth of the spacing between lands. Of course, that spacing comprises the grooves.
An alternative embodiment for the physical and electrical connection for vertical mounting of a micro device is shown in FIG. 2. In the same manner as shown in FIG. 1, electrodes 41 and 42 are formed not only on top of lands 43 and 44 respectively of substrate 40, but also down along the sides 45 and 46 of groove 47. Thus device 35, having side electrodes 36 and 37, makes firm physical and positive electrical contact with the electrodes formed in juxtaposition with the grooves.
With the orientation of a micro device such as a diode laser as shown in FIGS. 1 and 2 the laser emission would be directed generally outwardly from the substrate and top diode surfaces as shown by arrows 51. FIG. 3 is a top view of the structure of FIG. 2, showing active region 53 for laser emission from diode laser 35.
It should be noted that the relief pattern on the substrate may be fashioned to accommodate either vertical or horizontal mounting of the devices.
Another vertical mounting embodiment with reference to a diode laser component is shown in FIG. 4. A somewhat more complex relief pattern is provided where additional sub-groove 54 is formed in the bottom of main groove 55 to accommodate mirror 56 on the bottom of diode laser component 57. Mirror 61 is typically located on the opposite end. The physical and electrical interconnection mounting of FIG. 4 is the same as the FIG. 2 embodiment. In this arrangement, the bottom mirror, non-reflective coating or natural facet reflectivity of the semiconductor, which is important for operation of a diode laser, is protected from hitting the bottom of the substrate by the inclusion of additional shallow groove 54. It should be noted that the mirror need not actually protrude from the lower end of the diode laser, but in any event the bottom additional groove can be provided for protection of that surface.
A three dimensional stair-step arrangement is shown in FIGS. 5 and 6 where a horizontal mounting of the optical or electro-optical component is disclosed. Substrate 62 is formed with, in this case, three different flat surfaces 63, 64 and 65 which are arranged in a stair-step pattern. Etched into each of these flat surfaces are grooves 66, 67 and 68, two of each of which are shown. It should be understood that any number of such steps and grooves can be provided. Optical or electro-optical components 71, 72 and 73 are mounted in these grooves in the manner shown in FIG. 2. For example, if the devices are diode lasers, then the active regions for laser emission, 81, 82 and 83 respectively, are shown in the horizontal orientation in FIG. 6. Device electrodes 84, 85 and 86 are shown in FIGS. 5 and 6 on respective components 71, 72 and 73.
Another arrangement for horizontal mounting is shown in FIGS. 7 and 8 where each optical or electro-optical device is mounted in a groove with a mating beam deflector to direct the light originating in the device in a direction normal to the surface of the substrate. More specifically, substrate 91 having upper surface 92 is formed with a plurality of grooves 93, 94, 95 and 96. In grooves 94, 95 and 96 are optical or electro-optical devices 101 having their optical axes perpendicular to the longitudinal axes of the grooves and parallel to the bottom groove surface. Beam deflectors 102 may be mounted in the groove with the device as a separate element or they may be formed in a unitary manner when the grooves are formed in substrate 91. It is only necessary that the beam deflectors have reflective surface 103. The sloping side of the groove which forms the beam deflector can be formed in the same manner as the straight side of the groove. Then it is possible by polishing, or by surface coating, to create the desired reflective surface. Alternatively, diffusion, ion implantation or ion exchange of a suitable doping material into the sloping surface of the substrate could be employed to provide the reflective surface if desired. It is contemplated that the bottom surface of grooves 93, 94, 95 and 96 would be coated with a metallic conductive path to which one of the device electrodes would be connected if electrodes are needed for the device.
An alternative arrangement is shown in groove 93 of substrate 91 where the optical or electro-optical component 105 and beam deflector 106 elements are shown in pairs at a 90° angle with respect to those shown in the other grooves. The optical axis of the component remains parallel to the groove surface and is aligned with the longitudinal direction or axis of the groove. This is a matter of choice for any particular purpose and does not require any further description. However, with this orientation, it would be normally be expected that the beam deflectors would be separate elements.
Lines 107 arranged in the top surface of the substrate are V-grooves provided for alignment of the optical or electro-optical components and the corresponding beam deflectors. These are optional but can be useful in assembling the substrate with the components. Another alternative is that if the beam deflectors are formed in the sides of the groove, they would be continuous and the components would be aligned with the V-grooves.
In the embodiment of FIGS. 7 and 8, if electrodes are required, the second electrode of selected components could be electrically interconnected by wire bonding 111 to top surface 112 where the second electrode would be exposed. It is contemplated that signal bus 113 could be selectively provided as an electrically conductive path along the lands between the grooves and wires 114 bonded between that path and each component electrode. Alternatively, separate signal wires could be provided to each component if necessary.
With respect to FIG. 9, it is seen how the technology of forming the relief pattern can also be used for forming convective cooling channels in the substrate. Substrate 121 is formed with grooves 122 in the top in which laser diodes 123 are mounted. Grooves 124 may be formed in the opposite side of substrate 121 which can accommodate a cooling fluid of any type. A plate 125 is positioned either in contact with lands 126 forming the bottom surface of substrate 121 or spaced therefrom as shown in the drawing. The space, or reservoir, between top surface 127 and lands 126 is formed by an 0-ring 131 which seals the periphery of the reservoir. Cooling fluid may be pumped through this reservoir and groove combination to provide cooling for the active components mounted to the other side of the thermally conductive substrate.
For reference purposes, it may be stated that the material from which the substrate is formed may preferably be silicon or it could be sapphire or other suitable material. For active components, the basic characteristics of the substrate are that it be electrically non-conductive but be a good thermal conductor. These materials provide such characteristics. It is also noted that while discrete components are shown mounted in grooves in the substrate, monolithic arrays of components may be also advantageously mounted in such a relief pattern on a substrate. For example, a two-dimensional array could be formed by an array of linear diode laser arrays or linear photodiode arrays. Additionally, while both component electrodes are shown connected to opposite sides of the groove in FIGS. 1-6, it is possible that it would be desired to make such a connection in the groove to only one of the component electrodes. Other means may be provided for the electrical connection, such as the wire bonding mentioned with respect to FIGS. 7 and 8. Also, while it is shown in FIG. 4 that a component has two mirrors, it is possible that there is a mirror on one side and the other side is formed as a non-reflective coating or has a natural facet reflectivity of the material.
In view of the above description, it is apparent that the invention has significant advantages. Individual components or monolithic arrays may be mounted on a substrate to give large-scale arrays. The mounting procedure described above is quick, inexpensive and allows for flexible spacing of the components in the array. Such flexible spacing allows for small size and yet controlled temperature increase by varying the spacing between components or by varying the spacing between the grooves in the substrate surface It has already been noted that the fabrication technology employed to create the relief pattern on the substrate can also be used to create the convective cooling pattern. This type of cooling includes the use of channels or micro-channels in the substrate to remove heat from the substrate. Additionally, heat pipes could be used, along with liquid metal coolants, or cryogenic cooling of the substrate.
Arrays of diode lasers in the structure of the invention may also be used with external cavities or other devices to phase couple the individual diode lasers into a coherent array. The use of this precision mounting technique will allow the positioning of passive optics relative to the individual components. For applications such as phase locking of diode laser arrays in an external cavity, the precision mounting scheme here greatly facilitates the precise relative placement of the individual diode laser components and the diode laser optics. The relative position of this placement is a critical factor in achieving a uniform phase distribution across the array of diode lasers.
In view of the above description, it is likely that modifications and improvements will occur to those skilled in the art which are within the scope of the appended claims.
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Apparatus for mounting optical and electro-optical components and the like to a substrate to obtain physical mounting and electrical connections, along with heat dissipation. A relief pattern of precisely dimensioned grooves is formed on a substrate surface and the components are mounted in those grooves. The grooves may be partially lined with electrode material to facilitate electrical interconnection between the components and the substrate. The invention also relates to the method of mounting and interconnection.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This patent application relates to and claims priority to U.S. Provisional Patent Application Serial No. 60/286,914 entitled “Apparatus for Providing AC Power to Airborne In-Seat Power Systems,” by Hambley et al., that was filed on Apr. 27, 2001.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable.
BACKGROUND OF THE INVENTION
[0003] (1) Field of the Invention
[0004] This invention relates to an apparatus for converting an input AC signal to an alternatively configured output signal and providing the output signal to one or more devices. More specifically, the present invention relates to a method of producing a modulated AC signal for use by electrical devices as well as an outlet unit through which the AC signal may be channeled.
[0005] (2) Description of the Related Art
[0006] There exist outlet units for mating with the prongs of a plug through which power is to be supplied to a device which employ mechanical switches to detect the insertion of a plug. An example of an existing outlet unit is described in U.S. Pat. No. 6,016,016 of Starke et al. the disclosure of which is incorporated herein in its entirety by reference. Some existing outlet units make use of a plug case sensor to determine when it is safe to supply power to a plug. A plug case sensor senses the physical contact of a plug against a surface of the outlet unit. Power is enabled to a device only when the plug of the device exerts sufficient pressure against the plug case sensor to indicate that the plug is sufficiently connected to the outlet unit. Unfortunately, when used on a vehicle, the vibration which often attends the motion of the vehicle is sufficient to dislodge a plug from the plug sensor case. In such circumstances, provision of power to the plug from the outlet unit is rendered intermittent.
[0007] Many existing outlet units are attached to In Seat Power Systems (ISPS). An example of an ISPS is described in U.S. Pat. No. 5,754,445 of Jouper et al. the disclosure of which is incorporated herein in its entirety by reference.
[0008] There is therefore needed an outlet unit which can detect a plug insertion without the need for mechanical switches extraneous to the plug itself. In addition, it is preferable to utilize an outlet unit which does not rely upon a plug case sensor to determine when there is sufficient contact between the plug and the outlet unit to continue to provide power. Lastly, there is needed an ISPS configured to filter out the Electro-Magnetic Interference (EMI) produced by an offending device so that the device may continue in use without the need to restrict the provision of power to the offending device.
SUMMARY OF THE INVENTION
[0009] Accordingly, one aspect of the present invention is drawn to an outlet unit for providing a supply voltage to the prongs of a plug comprising a housing having a plurality of electrically conductive plug channels for receiving the prongs of the plug, a shutter rotatably mounted to the housing and operative in one of a first and a second position, the shutter having openings for receiving the prongs of the plug wherein only when in the second position the openings of the shutter and the plug channels are aligned permitting axial displacement of the prongs into the housing, and a strike plate located between the housing and the shutter for preventing the rotation of the shutter to the second position absent axial displacement of the prongs sufficient to engage the strike plate.
[0010] Another aspect of the present invention is drawn to An apparatus for converting a DC input signal to one or more AC output signals comprising a timer/control for emitting modulated timing and logic control signals, and a power converter for receiving the modulated timing and control signals comprising a plurality of master chopper oscillators responsive to the modulated timing and control signals so as to alter the voltage of the DC input signal for output as a single phase of one of the AC output signals, a plurality of current limiting chopper oscillators responsive to the modulated timing and control signals so as to alter the voltage of the DC input signal for output as a single phase of one of the AC output signals, a current integrator in electrical contact with one of the AC output signals the current integrator capable of measuring current drawn from the AC output signal and modifying the control signals of the current limiting chopper oscillators so as to shorten the duration of time of each positive or negative voltage phase of the AC output signal.
[0011] The above-stated objects, features and advantages will become more apparent from the specification and drawings that follow.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] [0012]FIG. 1 is a block diagram of an ISPS in accordance with the present invention.
[0013] [0013]FIG. 2 is a diagram of a pseudo sine wave output signal of the present invention.
[0014] [0014]FIG. 3 is an exploded view of an outlet unit in accordance with the present invention.
[0015] [0015]FIG. 4 is a schematic diagram of a power contact for use with the outlet unit of the present invention.
[0016] [0016]FIG. 5 is a schematic diagram of a sensor contact of the present invention.
[0017] [0017]FIG. 6 is a perspective rendering of an outlet unit of the present invention.
[0018] [0018]FIG. 7 is a schematic diagram of an output converter and timer/control of the present invention
DETAILED DESCRIPTION
[0019] With reference to FIG. 1, there is illustrated in block diagram form the progression from a 400 Hz/115 VAC input signal 10 into an EMI Filter 11 to a PFC (Power Factor Correction) 13 to a 155 VDC Converter 15 . The 155 VDC output 16 as illustrated is converted to a 155 VAC output for use in an ISPS. With regard to the present invention, there follows a description of the elements which combine in operation to form the power converter and outlet unit.
[0020] The EMI Filter 11 serves to filter out conducted Electro-Magnetic Interference (EMI) out of the ISPS. The EMI filter 11 filters out EMI that might travel from load drawing devices back into the aircraft's power supply and find its way into flight critical electrical devices. Connected to the EMI filter 11 is the PFC 13 that serves to eliminate current harmonics present in the ISPS. Connected in series with the PFC 13 is the 155 VDC converter 15 . The 155 VDC converter 15 serves to convert the 400 Hz/115 VAC input signal into a 155 VDC signal. EMI filter 11 , PFC 13 , and 155 VDC converter 15 may be assembled from any number of commercially and readily available components known in the art.
[0021] Output converter 17 receives 155 VDC output 16 and converts it into a 115 VAC output signal 111 . While illustrated herein as consisting of a single 155 VDC output 16 being converted into a single output signal 111 , there may in practice be a plurality of 155 VDC outputs connected to a plurality of output converters 17 which in turn output a plurality of output signals 111 . Such an alteration to the configuration of the present invention described herein would be readily ascertainable to one skilled in the art. With reference to FIGS. 1 and 7, output converter 17 is comprised, in part, of current integrator 12 , master chopper oscillators 71 , current limiting chopper oscillator 73 , and EMI filter 11 ′.
[0022] It is the purpose of the output converter 17 to output a pseudo sine wave on output line 111 for use by electrical devices. The operation of the components of the present invention which interact to produce the required pseudo sine wave 211 is described herein with reference to FIGS. 1, 2, and 7 . As is illustrated, the output converter receives a 155 VDC signal and outputs output signals 111 . While illustrated as receiving a 155 VDC input signal and outputting a 60 Hz 155 VAC signal, an output converter 17 of the present invention is not so limited. Rather an output converter 17 of the present invention could be readily modified to convert a range of input DC voltages to an output AC signal of the same or different voltage wherein the frequency of the output signal may likewise be chosen from a wide range of desired frequencies such as 220 VAC, 50 Hz as commonly available in Europe and 240 VAC, 50 Hz as commonly available in Australia
[0023] Referring to FIG. 1, while illustrated as a box, plug-in detect 19 is comprised of circuitry and hardware disclosed more fully in the text which follows. Plug-in detect 19 determines whether or not a valid plug attempt has been successfully completed. If a plug has been correctly inserted into an outlet unit of the present invention, the plug-in detect will direct timer/control 23 via a high logic signal to turn on the output converter 17 . As used herein, a “high logic” condition is one in which the voltage of a signal is sufficiently high to be interpreted as a boolean 1 for purposes of performing boolean logic. The ground fault interrupt senses the current differential through the power cord of a plugged in device back to ground. Similarly, if the ground fault interrupt 7 does not sense a substantial current differential through the power cord of a plugged in device back to ground, a high logic signal is directed to timer/control 23 . Auxiliary power source 21 provides the power to timer/control 23 required to power the logic circuits contained therein and which are described more fully in the following. System available logic 25 directs a high logic signal to timer/control 23 when there is power available for distribution to a power requesting load device. Timer/control 23 effectively performs an AND function on the input signals received from system available logic 25 , plug-in detect 19 , and ground fault interrupt 7 . In the event that all such input signals correspond to a high logic signal, timer/control 23 proceeds to emit a 240 Hz timing signal for input into the output convertor 17 .
[0024] Under normal operating conditions, output converter 17 makes use of several chopper oscillators 71 , 73 to segment the incoming 155 VDC signal, alter the voltage of the segments into a pseudo sine wave for output, and output the newly constructed 155 VAC signal as output signal lll. With reference to FIG. 7 and FIG. 2 there is now described the operation of power converter 17 to produce output signal 111 .
[0025] Timer/control 23 is comprised in part of a 240 Hz signal generator. As can be seen in FIG. 2 a and 2 b , the pseudo sine wave of output signal 111 is comprised of four phases. Each of the four phase requires a different logic input to direct the master chopper oscillators 71 and the current limit chopper oscillators 73 to pull the output signal 111 to a voltage defined by one of the four phases. Because each full cycle of the output signal 111 requires four phases, and each phase change occurs at a single clock cycle or control signal of the 240 Hz signal generator, the resulting output signal is a 60 Hz signal (240 Hz divided by 4).
[0026] As is illustrated, timer/control 23 outputs four logic switch control signals SC 1 , SC 2 , SC 3 , and SC 4 . SCI and SC 2 control the operation of master chopper oscillators 71 . Similarly, SC 3 and SC 4 control the operation of current limiting chopper oscillators 73 . When the timer/control 23 sends a logic high signal to any of the switch controls, the corresponding switches are closed thereby altering the output voltage of output signal 111 . In phase 1 , SC 1 and SC 2 are activated. In phase 2 , SC 2 and SC 4 are activated. In phase 3 , SC 1 and SC 4 are activated. In phase 4 , SC 1 and SC 3 are activated. Under normal operating conditions, signals sent from the timer/control 23 to the chopper oscillators 71 , 73 of output converter 17 result in the 60 Hz 155 VAC pseudo sine wave signal detailed in FIGS. 2 a and 2 b . At 60 Hz, the duration of each phase of the four phase output signal cycle is approximately 4.17 ms in duration. As a result, pseudo sine wave 211 yields a 110V rms signal as well as the same (155V) peak voltage as would a true 110Vrms sine wave.
[0027] The power system of the invention is particularly useful to provide power to personal devices carried by a passenger onto a vehicle, such as an aircraft, ship or bus. In particular, the vehicle is a commercial aircraft. An exemplary load device for drawing power from the present invention is an AC-adapter laptop computing device. Such laptops utilize rectified peak detectors which are also typically transformer isolated. Because the peak voltage of a true sine wave is equivalent to the peak voltage of the pseudo sine wave 211 , the inductive currents in the transformers of such laptop loads will be approximately the same. A true 110 VAC sine wave has an average voltage of 99V (computed as 110V*sqrt2*2/pi). Because pseudo sine wave 211 is at ±155V for two phases of each cycle and at OV for the remainder, use of the pseudo sine wave 211 creates 22% less average voltage (77.5V) in the adapter transformers than would a true 110 VAC sine wave. Therefore, the output pseudo sine wave of the present invention provides at least 75W of power to devices attached so as to receive the output signal while remaining below the FAA mandated maximum power limit of 100W for use in aircraft. In the present invention as will be described more fully below, the power provided through the pseudo sine wave 211 is limited to a maximum of 80W through the interaction of the current integrator 12 , the timer/control 23 , and the current limiting chopper oscillators 73 .
[0028] Current input signal 711 senses the current flowing through L 1 to output signal 111 . Current input signal 711 is received by current integrator 12 which integrates over a single phase the amount of current flowing through output signal 111 to a load device receiving power. Should the amount of current outputted to a device over a single phase, for example phase 1 as illustrated in FIG. 2 a , exceed the amount of current which may be provided such that the total power draw of the device remains under the allowed 80W, the current integrator 12 can function to reduce the power consumption of the device. Specifically, in the event that the maximum allowable current for a cycle has been outputted to a device, the current integrator toggles the control signals sent by timer/control 23 to SC 3 and SC 4 . Such a toggle could be achieved by XORing a logic high signal with SC 3 and SC 4 . When such a toggle is performed before the usual 4.17 ms duration of a single phase, pseudo sine wave 211 returns from either ±155V to 0V earlier than usual. This phenomena is illustrated in FIG. 2 a by the dotted lines representing a leftward shift, or prematurely occurring onset, in the voltage change from +155V to 0V and from −155V to 0V. As noted, while in phase 1 , SC 2 and SC 3 are on. If SC 3 is toggled off and SC 4 is toggled on, the resulting SC 2 and SC 4 being on is the condition that brings about phase 2 in which the voltage drops from 155V to 0V. Similarly, while in phase 3 , SC 1 and SC 4 are on. If SC 4 is toggled off and SC 3 is toggled on, the resulting SC 1 and SC 3 being on is the condition that brings about phase 4 in which the voltage rises from −155V to 0V. In this manner, the power supplied to a load device is maintained below a designated maximum value, for example 80W. Once either SC 3 or SC 4 is toggled and the voltage is brought to 0V, the next 240 Hz signal from the timer/control 23 does not alter the switch control settings but rather maintains them as they were.
[0029] In addition to safe guarding against a load device drawing an excessive amount of power, the present invention similarly prevents any load from drawing a peak amount of current in excess of a predetermined amount. Typically, such a predefined peak amount of current is approximately 3 amps. If the peak current drawn by a load device reaches such a predefined peak current amount, SC 3 and SC 4 are provided with a control circuit signal between approximately 100 and 200 KHz which is then used to pulse width modulate the output signal 111 .
[0030] Referring once again to FIG. 1, output converter 17 is includes EMI filter 11 ′. As noted above, each output converter may support multiple output signals 111 for use by a plurality of load devices. For example, a single output converter 17 may provide power via two output signal lines 111 to two laptop computers connected as load devices. Each laptop may produce EMI which could potentially be transmitted to the other laptop via the output converter 17 . To prevent such an occurrence, each output converter 17 includes an EMI filter 11 ′ connected so as to filter any EMI which might pass from one load to another via a single output converter 17 . When combined with the EMI filter l 1 noted above, each device is shielded from EMI coming from the main power source, is prohibited from injecting EMI back into the aircraft's other systems, and is shielded from EMI originating at the site of other devices plugged into the same ISPS unit.
[0031] The outlet unit of the present invention is illustrated with reference to FIG. 3. Outlet unit 41 is comprised generally of bezel 31 , torque springs 32 , shutter 33 , strike plate 35 , pressure springs 36 , fastening pins 43 , housing 37 , sensor contacts 38 , power contacts 39 , printed circuit board 34 , and cap 40 . When assembled and in static mode, bezel 31 is fastened to housing 37 through the use of fastening pins 43 inserted through holes located at peripheral points near opposing corners and extending through bezel 31 and mating with receiving cavities 45 formed integral to housing 37 .
[0032] Once assembled, shutter 33 rests generally flush with bezel 3 1 . Torque springs 32 are attached to shutter 33 in such a fashion as to exert a radial torque upon shutter 33 sufficient to rotationally displace shutter 33 around axis 47 . In its static configuration, the resting position of shutter 33 is such that torque springs 32 are least extended and shutter 33 is rotated around axis 47 such there is no correspondence between the openings in shutter 33 and the openings of strike plate 35 . As a result, there is no continuous opening through which the prongs of a plug could be inserted through shutter 33 , through strike plate 35 and into housing 37 .
[0033] Continuing with the discussion of the static arrangement of the outlet unit 41 , the outward facing face of strike plate 35 is pressed away from housing 37 and into contact with shutter 33 by a plurality of pressure springs 36 . Pressure springs 36 are disposed between the housing 37 and strike plate 35 . When pressed by pressure springs 36 into maximal contact with shutter 33 , tabs located on the underside of shutter 33 and extending a short ways axially towards housing 37 engage slots 49 cut into the periphery of strike plate 35 . Strike plate 35 is attached to housing 37 in such a way as to not permit axial rotation about axis 47 . Therefore while strike plate 35 can extend back and forth a short distance along axis 47 , it cannot rotate about axis 47 . When strike plate 35 is maximally extended by pressure springs 36 against shutter 33 , the slots 49 engage the tabs of shutter 33 so as to prevent the axial rotation of shutter 33 . Only when strike plate 35 is sufficiently displaced along axis 47 towards housing 37 such that slots 49 no longer engage the tabs of shutter 33 can shutter 33 be radially displaced such that the openings through shutter 33 correspond to those of strike plate 35 .
[0034] With reference to FIG. 4 there is illustrated a power contact 39 of the present invention. Power contact 39 is comprised in part of opposing sides 46 and back plate 48 . When positioned behind housing 37 as shown in FIG. 3, the prongs of an inserted plug will contact the gently outwardly sloping ends of opposing sides 46 forcing a slight outward deformation of opposing sides 46 . This slight outward deformation causes the opposing sides 46 of the power contact 39 to apply pressure against the plug prong and thus maintain physical and electrical contact with the prong. Depending on the configuration of the prong, the prong may also form a contact with back plate 48 . As opposing sides 46 and back plate 48 are fashioned from the same piece of electrically conductive material, contact with either opposing sides 46 or back plate 48 is sufficient to enable electrical contact between the power contact 39 and the prong.
[0035] With reference to FIG. 5, there is illustrated a sensor contact 38 of the present invention. Contact sensor 3 8 is constructed of a single piece of electrically conductive material. Contact sensor 38 is comprised in part of contact hook 51 . When positioned behind housing 37 as shown in FIG. 3, the prongs of an inserted plug will contact contact hook 51 forming a slight outward deformation of contact hook 51 . The resulting deformation will cause contact hook 51 to exert pressure against the prong of the plug so as to assure both physical and electrical connectivity between the sensor contact 38 and the plug prong.
[0036] With continued reference to FIG. 3, both power contacts 39 and sensor contacts 38 are positioned to receive and maintain contact with the prongs of a plug. In addition, both power contacts 39 and sensor contacts 38 are provided electrical connectivity to printed circuit board 34 . Printed circuit board 34 contains circuit traces capable of carrying electrical impulses to the plug-in detect 19 of FIG. 1. To avoid exposure and subsequent connectivity to any external element, power contacts 39 , sensor contacts and 38 , and printed circuit board 34 are enclosed between housing 37 and cap 40 . Cap 40 is attached to housing 37 by means of a bolt, screw, adhesive, or other apparatus capable of providing sufficient attachment force sufficient to avoid the separation of cap 40 from printed circuit housing 37 .
[0037] With reference to FIG. 6, there is illustrated a perspective view of outlet unit 41 in its static state in accordance with the present invention. As used herein, static state refers to the configuration of an outlet unit 41 absent the insertion of the prongs of a plug. As described above, shutter 33 through which the prongs of the plug are to be inserted is rotated approximately 45 degrees about its center. When the prongs of a plug are inserted with through the holes in the face of shutter 33 , they come into physical contact with strike plate 35 . As described, strike plate 35 is pressed outwards against the back side of shutter 33 by pressure springs 36 . When the prongs of a plug are inserted through shutter 33 and into contact with strike plate 35 with sufficient force, the force exerted upon strike plate 35 by pressure springs 36 is counter balanced and the strike plate 35 is moved axially back towards the housing 37 . When the strike plate 35 has been so moved sufficiently, the engage slots 49 of the strike plate 35 extend so as to no longer engage the tabs attached to shutter 33 and shutter 33 is able to rotate such that the openings through shutter 33 are in correspondence with those of strike plate 35
[0038] As used herein, a “plug channel” is the empty space through which the prongs of a plug may be inserted. The plug channels of the present invention are formed from the openings in the shutter 33 , the strike plate 35 , through the housing 37 , and on till the power and sensor contacts 3 8 , 39 . As the inserted prongs of a plug proceed further into the plug channel, each prong contacts a power contact 39 and then a sensor contact 38 . The power contact 39 is not initially activated to provide power. The power contact 39 remains off until the control circuitry of the plug-in detect 19 attached to the sensor contact determines that power is to be provided. The control circuitry senses electrical continuity between the power contact 39 and the sensor contact 38 provided by the prongs of the plug and ensures that such continuity is provided along both prongs within a predetermined time, nominally 200 milliseconds of each other. Preferably, this predetermined time is between 0 and 300 milliseconds and more preferably, between 150 milliseconds and 250 milliseconds. Only if such continuity is established within this time frame is current enabled to flow through the power contacts. When removing a plug, the sensor contacts 38 can sense that that the plugs are no longer in contact with them as the plug is pulled out. As a result, the flow of current can be stopped prior to the plug passing past the power contacts 39 . In this manner, the presence of arcing is avoided when a plug is removed.
[0039] Prior art outlet units typically rely on mechanical micro-switches to sense the insertion of a plug before providing power. In an aspect of the present invention, the plug itself is used to test for continuity with no need for additional mechanical switches. In other implementations, prior art outlets make use of a plug case sensor. The plug case sensor requires constant pressure upon it provided by the case of the inserted plug to cause power to be provided. Such a system is unreliable as aircraft vibration may partially evacuate an otherwise engaged plug through which current may and should still flow. The plug of the present invention is capable of operation without a plug case sensor and therefore does not suffer from the noted deficiency of plug case sensors.
[0040] In addition, after turning a plug through the required 45 degree angle of the present invention and then inserting the plug until electrical contact is made between the prongs of the plug and the sensors 38 , 39 of the outlet, there remains a substantial residual torque arising from the predilection of the outlet unit to return to its 45 degree offset. This torque provides for a secure fitting of the plug of a device into an outlet unit 41 and resists the tendency to become loose as a result of prolonged exposure to aircraft vibration.
[0041] With reference to FIG. 3, there is illustrated the pattern of openings extending through shutter 33 through which the prongs of a plug may be extended. These openings need not match the precise openings required by only a single class of plugs to facilitate the insertion and extension of the prongs of the plug through shutter 33 and into contact with sensor contacts 38 and power contacts 39 . Rather, as is illustrated, the openings in the shutter 33 preferably form a superposition of the openings required for a plurality of plug classes. Such classes include, for example, the generally rectangular cross-section of a United States prong and the generally circular cross-section of a European prong. In this manner, an outlet unit 41 of the present invention may serve as a universal outlet constructed to receive the prongs of a variety of plug classes and provide power thereto.
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An outlet unit for providing a supply voltage to the prongs of a plug comprising a housing having a plurality of electrically conductive plug channels for receiving the prongs of the plug, a shutter rotatably mounted to the housing and operative in one of a first and a second position, the shutter having openings for receiving the prongs of the plug wherein only when in the second position the openings of the shutter and the plug channels are aligned permitting axial displacement of the prongs into the housing, and a strike plate located between the housing and the shutter for preventing the rotation of the shutter to the second position absent axial displacement of the prongs sufficient to engage the strike plate.
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FIELD OF THE INVENTION
The present invention relates to telecommunication devices for the deaf in general, and, in particular, to improve telecommunication devices for the deaf which offer increased conversation-like ability while maintaining compatibility with existing devices already in use.
BACKGROUND OF THE INVENTION
Persons who are deaf or hearing impaired who cannot hear well enough to use the telephone commonly make use of communication terminals specifically constructed in design to enable such persons to converse over telephone lines. Such devices are referred to as telecommunication devices for the deaf, or TDD's, and include both a keyboard and a display connected to the telephone through a modem (modulator/demodulator). The modem is typically built into a TDD connected either by hard wiring directly to a telephone line or through an acoustic coupler which couples the modem to a normal telephone handset. TDD's are normally capable of transmitting information over a telephone line by means of coded tones to another compatible TDD connected at the opposite end of the telephone line through another modem.
There are several protocols that are used for transmitting digital information through analog lines such as telephone lines. The most commonly used information protocol in the electronics industry is referred to as ASCII (American Standard Code for Information Interchange). The ASCII code was designed for and is most commonly used for information interchange between computers. However, largely due to historic reasons, TDD's have operated on a different protocol, originally developed specifically for TDD communication. This TDD protocol is referred to here as the Baudot/Weitbrecht, or standard Baudot, and includes both a specific 5-bit Baudot code and a frequency shift keying (FSK) protocol of electronic communication. The standard Baudot communication is simplex, that is to say it is capable of only transmitting in one direction at one time. Therefore, during normal TDD communication, one station must be silent while the other is transmitting. It has become a convention that one TDD user informs the other TDD user when it is the other user's turn to utilize the communication link.
The inability of the traditional Baudot/TDD communication network to permit bi-directional or duplex communication of the network created by this form of communications has been an inadequacy since its inception. Under current TDD/Baudot communication protocols, if both users attempt to transmit at the same time, each station will only display to the user the characters it is transmitting. This is because standard Baudot TDD's are designed to give priority to transmission. Since prior TDD's cannot receive data while transmitting, when transmitting standard TDD's make no attempt to receive incoming characters. This creates obvious difficulties in the use of TDD systems for communication between individuals and makes such communication not similar to normal human communication. As in even a brief monitoring of oral communication between hearing individuals will indicate, human speech is characterized by constant interruptions and interchange. The current TDD/Baudot communication network is incapable of handling such interruptions and interjections, and hence is less similar to audible human conversations than would be desired in an ideal system.
In addition, it is often desired that during a TDD communication that one user be able to signal or interrupt the other user. Often, for example, one user may be launched onto a long description, or explanation, which the other user is already aware of or has heard before. In normal human audible conversation, a listener can indicate to the speaker that he has already heard that part of the explanation. In TDD communication, due to the simplex nature of the communication link, the receiver is unable to communicate with the transmitter until the transmission is complete. Since communications can sometimes be quite long, this is a source of frustration and time delay, and hampers normal human tendencies during conversation. Heretofore the standard Baudot/Weitbrecht network has been incapable of handling such tendencies.
There was one instance known of an attempt to permit interruption in a communication device operating under Baudot protocol. One of the early originators of TDD communications in the United States, Mr. Weltbrecht instituted a "news service" for the deaf community in the United States accessible by telephone. Mr. Weitbrecht constructed what was, in essence a recording device, which played out a periodic news compilation in Baudot communication to any TDD that would dial the phone number associated with the news service. In that time period, it was common for TDD's to listen for space tones (1800 Hertz) only, and to not even sense mark tones (1400 Hertz). A receiving TDD would simply assume absence of space tones during a character meant mark. Utilizing this characteristic, Weitbrecht constructed the news service device so that if it was to transmit a bit sequence of three marks (or 1's) at any point during the transmission, the device would simply stop transmitting the mark tone and listen for tones from the communicating station. If tones were sensed during the interval, the news service device would cease transmission. This feature was transparent to users at that time since most TDD's of the era did not detect mark tones. This characteristic is no longer true of modern electronic TDD's.
SUMMARY OF THE INVENTION
In accordance with the present invention, a telecommunication device for the deaf is constructed which operates so as to observe two rules which constrain its activity so as to permit interrupts and pseudo-duplex activity. The two rules are that the terminal is not permitted to transmit when it is receiving transmissions from a device with which it is communicating. The second rule is that the terminal creates a pause in the communication line at periodic intervals of transmitted characters and, during that pause, senses for transmissions by the remote terminal. The combination of these two rules in the operation of a telecommunication device permits the device both to be interrupted, and permits pseudo-duplex communication between two telecommunication devices for the deaf.
It is an object of the present invention to provide a telecommunication device for the deaf which is capable of providing an interrupt signal from one user to another, which is still compatible with and capable of communicating with existing TDD devices previously installed within the deaf community.
It is yet another object of the present invention to provide a telecommunication device for the deaf which is capable of providing two-way communication, or pseudo-duplex communication, while still being fully compatible with existing telecommunication devices for the deaf already installed in the deaf community.
It is another object of the present invention to provide a telecommunication device of the deaf which is capable of providing interrupt and pseudo-duplex capabilities, while also being capable of communicating with an enhanced TDD protocol permitting faster speeds of communication.
It is an advantage of the present invention in that it can be implemented totally in microcode, or firmware, where changes to existing TDD designs so as to permit cost-effective and convenient retrofitting of existing TDD's in the field so that the benefits of these enhanced methods of TDD communication can be utilized by the existing community of TDD users.
The pseudo-duplex and interrupt capabilities will also result in a net savings of on-line time and telephone costs as users can interrupt previously transmitted communications. This results also in more natural conversation-like communications. Also the interrupt capability allows for handling emergency communications more effectively.
Other objects, advantages, and features of the present invention will become apparent from the following specification when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram of prior art TDD hardware suitable for use with the present invention.
FIG. 2 illustrates schematic details of the prior art analog circuit of FIG. 1.
FIG. 3 is a flow chart illustrating the method of operation of a terminal operating in accordance with the present invention.
DESCRIPTION OF THE INVENTION
In accordance with the present invention, a telecommunication device for the deaf has built into its functioning an enhanced set of protocols which enable it to communicate with conventional Baudot terminals and also to be capable of handling an interrupt situation and also handling bi-directional, or pseudo-duplex, communication. The ability to do both the interrupt and the bi-directional communication arises from the terminal following two relatively simple rules in its method of operation. The first rule is that the terminal is constrained not to present carrier or characters on the communication line when the other terminal with which it is communicating is presenting such characters. The second rule is that the terminal is constrained to present a pause, or null, on the communication line at predetermined intervals, i.e. after the transmission of a specific number of characters. The implementation of these two rules in a telecommunications device enables such devices to interrupt each other, and to communicate in a pseudo-duplex fashion to each other. The implementation of these rules does not prevent communication between such an improved TDD and a conventional TDD.
Shown in FIG. 1 is a schematic block diagram of the function of a typical TDD. In the TDD of FIG. 1, the user types on a keyboard indicated at 12 to input characters into a microprocessor indicated at 14. Characters which are received or transmitted by the microprocessor are also displayed to the user on a visual electronic display, indicated at 16. Characters may also optionally be displayed by means of a hard copy printer, indicated at 18, which some TDD's include. Thus the keyboard serves as the source of input data characters and either or both of the display 16 and the printer 18 serve as ultimate destinations for the data characters. The microprocessor 14 is largely responsible for the implementation of the various timing and decoding functions of the TDD. The microprocessor has data and address buses, Jointly indicated at 20, which connect to a read-only memory (ROM) 22 and a random access memory (RAM) 24. Appropriate control lines 26 and 28 connect to the ROM 22 and RAM 24 so as to control the operation thereof. The ROM is intended to contain the program which dictates the functional operation of the microprocessor 14. The RAM is utilized as a holding place or stack for data coming into or out of the TDD. In some TDD's, the microprocessor, the RAM and the ROM are all combined in a single integrated circuit, while in others they are separate circuits.
As an additional output, the microprocessor connects through analog circuitry 30 to one of three separate outputs. The analog circuitry 30 is, most preferably, a modem. One output of the analog circuitry 30 could be a telephone direct connect circuitry 32 which connects the modem directly by hardwiring into the telephone network. A second possible output from the analog circuitry is through an acoustic output circuit 34 intended to audibly connect through a speaker 38 to the microphone of a telephone handset. At 36 is indicated acoustic input circuitry connected to a microphone 40, which is intended to audibly couple to the speaker in a telephone handset. The acoustic output speaker and the acoustic input microphone may be connected through a so-called "acoustic coupler" to a conventional telephone handset. In any TDD, either the hardwired connection or the acoustic connection is provided, and sometimes both. It is also envisioned that the telephone line need not be a physical link. A TDD could be made to operate as a cordless phone or through a cellular telephone system rather than through a conventional telephone two-wire connection.
Shown in FIG. 2 is a simplified schematic of how the input and outputs of the analog circuitry would work. For data coming into the terminal, the audible input from a microphone or telephone line is translated into electronic components and then presented to an amplifier 42. The output of the amplifier is presented to two phase-locked-loops 44. One of the phase locked-loops 44 is tuned to a frequency of 1800 Hertz, while the other phase-locked-loop 44 is tuned to a frequency of 1400 Hertz. 1800 Hertz and 1400 Hertz are the designated carrier frequencies for standard Baudot communication. On the output side of the circuitry, output signals are presented to a LPF (low pass filter) transmit wave shaping circuit 46. The output of that circuit, consisting of alternate 1400 and 1800 Hertz signals, is presented to an amplifier 48 which is hardwired to the speaker or telephone line.
In normal Baudot communications with existing TDD's, each TDD communicates at 45.5 baud in a simplex mode. In some countries, the protocol is the same but the speed is 50 baud. That is to say each TDD transmits a character on the line whenever a key is pressed at the TDD. As a result, in order to approximate the give-and-take of normal conversation, TDD users generally have to indicate to the other user when the user that has the floor is ending that particular communication. For example, it is quite common convention in the United States to type the letters "GA" as an abbreviation for "go ahead" at the end of a text string to indicate to the other user that it is his or her turn to type. This procedure is awkward and not like normal conversation. Also, occasionally users wish to interrupt and, regardless of the constraints of their machine, do attempt to type keys into their machine while receiving data. Such attempts to interrupt are typically not successful since the station transmitting data does not monitor the line for incoming data.
The TDD of the present invention is constrained not to even attempt truly simultaneous communication. The improved TDD described here is simply programmed not to transmit data when data is being received. This concept is directly opposite to the conventional operation of TDD's, but is effective if utilized as described here. It is a relatively simple matter that, when the microprocessor senses that a key has been pressed during data reception and which is intended to ultimately transmit a character to the remote station, for the microprocessor first to test whether analog data is being received. If data is being received, the microprocessor is constrained by the software not to immediately output the character onto the transmit line but, instead, to store the appropriate characters which have been entered by the user into the RAM. Typed characters are also stored in a queue or stack during all times of data reception. The user may continue to type, and the characters are entered by the keyboard, and are placed into the RAM, until such time as communication from the remote station has ceased.
When it is time for the station in accordance with the present invention to transmit, the improved TDD transmits characters either directly from its keyboard, or from the buffer composed of the RAM, out through the transmission line. The pseudo-duplex capable TDD of this invention will, however, cause periodically during the transmit data stream. The device is programmed to pause after the transmission of a pre-determined number of characters. The purpose of the pause is for the terminal to test during the pause whether input data is being received. In other words, the pause serves as an interrupt window for the other communicating machine. Since the device is constrained not to transmit when receiving, if, during a pause, the other remote machine begins transmitting the local terminal will cease transmission. In this way, most of the situations in which the two terminals would simultaneously transmit data are avoided. It is still possible occasionally for simultaneous data transmissions to occur, when both stations simultaneously transmit data onto the line, but these situations will be quite rare.
The number of characters which are transmitted by the TDD in accordance with the present invention before a pause is subject to some variation between two extremes. At one extreme, it is possible to present a pause on the transmission line after the transmission of every single character. While this choice minimizes the number of potential data collisions on the telephone line, it also slows down the transmission when conducted at ordinary Baudot transmission rates. Since Baudot operates relatively slow in any event, i.e. at 45.5 Baud, which approximates 6 characters per second, adding an extra bit time or two to every character might perceptively slow down the transmission by the terminal. At its upper limit, it is clearly possible to impose such a pause every 72 characters, since the normal constraints of conventional Baudot communication protocols require that a carriage return and line feed be implemented every 72 characters followed by a pause, originally imposed to allow for a mechanical TDD systems which must mechanically return the printing head. Thus there is an automatic pause time traditionally included in Baudot/Weitbrecht protocol at least every 72 characters within the data stream, by convention. In its preferred embodiment, it is anticipated that the number of characters which will be transmitted in between pauses would be between 1 and 72, and most preferably between 1 and 10. Actual empirical testing of terminals on a number of communication lines is necessary to determine which is the exact and optimum number of characters to be transmitted between pauses.
The length of the pause after the packet of characters should be sufficient so as to permit settling of the communication line, a time period sufficient for the other terminal to commence data transmission, and a time period sufficient for the pausing station to sense that data is being transmitted to it over the telephone line. These times can be varied over a wide range depending on the quality of the telephone network and the timing constraints of the hardware in the TDD. The normal bit time of conventional Baudot communication is approximately 22 milliseconds. After transmitting Baudot tones, it can typically take some telephone lines some time period for echoes, transients, and other chatter introduced on the line by previous communication signals to fade. In most modern telephone systems, a time period of five to fifty milliseconds is needed to permit such settling. A TDD in the accordance with the present invention pauses for a time period divided into two portions. The first portion is a pause for a sufficient time period, such as 10 milliseconds, to permit the telephone line to settle. The second pause is for a sufficient time period, such as, 10 to 44 milliseconds, which is sufficient time for the transmitting terminal to initiate transmission and for the transmission to be sensed by the pausing station. An interrupt-competent and pseudo-duplex TDD constructed in accordance with the present invention will therefore often have to buffer data being typed in by the user. During time periods in which the user is typing at the keyboard, but the terminal is constrained from transmitting characters due to the receipt of characters from the remote terminal, the data characters being entered by the user would be stored in the random access memory in a stack or queue. Then, during the station's next interval for transmission, it would transmit characters on a first-come first-serve basis out of the queue onto the transmission line.
This system is capable of operating either in conventional Baudot/Weitbrecht or in a newly designed enhanced Baudot communication protocol. Nevertheless, it is an advantage of the operation of this machine that it is capable of operating also with conventional TDD's, without any alteration to the conventional machines. If the TDD of the present invention is communicating with an otherwise conventional remote TDD, the remote terminal could occasionally lose characters if keys are pressed while it is receiving. The pseudo-duplex TDD will tend to drop fewer characters since it cannot transmit when the remote terminal is transmitting. In addition, any such losses at the remote terminal are minimized, since the TDD in accordance with the present invention creates a pause at predetermined intervals, and when the first of those intervals occurs, the pseudo-duplex TDD will stop transmitting. Thereafter, the pseudo-duplex TDD will be able to receive whatever information is being transmitted by the station with which it is communicating. Clearly the fewer the number of characters transmitted between pauses, the fewer the number of characters which might be lost.
As an option, it may also be appropriate to include an interrupt signal in the TDD of the present invention. If such an interrupt sign is implemented, the microprocessor would as usual, monitor the input line during times it is not transmitting data to test for signals. The TDD would thus detect any data signal received during the periodic pause, even if the terminal still had characters to transmit. The microprocessor would then visually signal to the user that an interrupt is being initiated by the remote station. The visual interrupt signal could consist of the word "interrupt" on the display, could consist of the display of a specially designated character not in the normal Baudot character set, such as an asterisk or could consist of any characteristic character, word or pattern designated for this purpose. Another alternative is to split the display into two sets (input and received characters) and the user can be informed of the interrupt by noticing the split display. Then the user may cease typing on the keyboard, to permit the transmission from the remote station to be received by the terminal and displayed appropriately.
In the event that two interrupt-competent TDD's in accordance with the present invention are communicating, missing transmitted data becomes an extremely unlikely event. In normal communication, when either one of the two terminals is transmitting, the other terminal is constrained not to transmit. Then, since each station when transmitting is constrained to stop after a certain number of characters and present a pause, during that pause the other station will gain control of the communication line. Then that station will transmit until its turn to pause. For example, if the persons at stations A and B are both typing at the same time, one of the two TDD's at each station will initially gain control of the communication line, and transmit the predetermined number of characters. Assume, for purposes of this example, that the number of transmitted characters is seven. Station A would transmit seven characters to Station B, and Station B would be constrained not to transmit during that interval. At the end of the transmission of the seventh character, Station A would pause and Station B would seize control of the communication line and then communicate seven characters to Station A. After that time period, Station B would pause, and Station A would resume control of the communication lines. In other words, each station would separately transmit to the other a burst of characters during alternate time periods. In this way, it would appear to the users as if a full duplex communication were occurring. This form of communication is referred to here as pseudo-duplex, since the actual technical communications over the telephone line is in simplex, i.e. with only one station able to communicate at an instant, while the appearance to the users is of duplex, or two-way, communication.
Obviously, if a station is alternately both transmitting and receiving data in groups of small numbers of characters, some provision must be made to make the display appropriate and readable to a user. At least two options are possible. One option is simply to have the user only see the information received from the foreign station. The other, a more preferable option, is to split the screen of the display on the terminal. This split can be either vertical for one-line displays or horizontal if there is a two line or larger display. One portion of the split screen would be reserved for the characters being transmitted by the terminal and other portion of the split screen would display the characters being received from the remote terminal. Such split-screen operation is entirely within the capability of the microprocessor to effectuate, the screen display being under software control in any event.
Shown in FIG. 3 is a flow-chart representation of the workings of the terminal of FIGS. 1 and 2 operating in accordance with the present invention. At step 50, the microprocessor monitors the keyboard and the incoming telephone line for data. This step is performed in the normal fashion by which TDD's perform these functions. When a user presses a key the key selected by the user represents data which is accepted from the keyboard at method step 52. Most conventional prior TDD's would immediately transmit the character to the telephone line. Instead the pseudo-duplex TDD first checks to ensure that no data is being received on the telephone line. If data is being received the program branches and continues to receive the input data and buffer the output data until the incoming character stream ceases. This step is indicated at 55. Once the received data is stopped, the program may proceed back through the step of detecting whether data is being received at step 54. Once the situation arises where no data is being received, the program then proceeds to step 56 where it transmits N characters of data from the keyboard. In this instance the letter N represents the numbers of letters in the character packet which is transmitted by the pseudo-duplex TDD. As stated, the number N can be between 1 and 72 and is preferably between 3 and 10. After the characters packet has been transmitted, the program then determines whether or not there are characters left to transmit. If all the characters have been transmitted the program can return to its monitoring state at step 50. If there are more characters left to transmit, the TDD does not immediately begin to transmit the new characters, but instead imposes a pause at 58. During the pause at step 58, the remote TDD may start transmitting data. Thus, at step 60 the TDD senses whether data is being received. At step 60, the machine has paused during a data transmission. Accordingly, if data is being received, that represents an interrupt by the remote station. Accordingly, the program proceeds at step 62 to provide an interrupt signal to the user. Nevertheless the device still receives the data from the remote device and stores the potential output characters, again at step 55, rather than transmitting characters onto the transmission line. At step 60 if no data was being received the program can branch back to step 56 and transmit characters again. The result of all of these steps is the implementation of the two rules discussed above. Steps of FIG. 3 result from following the two rules of simply not transmitting when data is being received and also pausing after the transmission of every N character to permit the remote station to transmit.
Thus, the pseudo-duplex TDD terminal constructed in accordance with the present invention is fully capable of pseudo-duplex communication with a compatible TDD. At the same time, the terminal is capable of communication with conventional TDD's, which would simply ignore the brief pause during the character transmission time. In addition, the pseudo-duplex TDD is competent to handle interruptions, so if the pseudo-duplex TDD is communicating with a conventional TDD, and the conventional TDD begins to transmit, there may be a brief loss of a few characters, but then during the appropriate transmission pause, the pseudo-duplex TDD will recognize that a transmission is being received, and inhibit further character transmissions until the next pause. Thus the device is compatible with existing TDD's in the communication network, and does not require any modifications or changes in operation to existing TDD's in order to be compatible with this new device. Users do not have to alter their habits to use the improved TDD yet will appreciate the advantages it offers.
It is a further advantage of the present invention in that it can be implemented and upgraded to existing TDD's by software upgrade. As may be seen in FIG. 1, the hardware portions of the circuit have to do with the analog input and output. The detail transmission behavior of the device, including the timing of transmitted data bits, and the translation of characters into Baudot code, are all handled under software control by the program for the microprocessor contained in the ROM. Thus, to retrofit old TDD's with the pseudo-duplex capability, all that needs to be replaced is the ROM in the older TDD. With a replacement of a single integrated circuit, the older conventional TDD can be given the capability of handling an interrupt and acquire the pseudo-duplex capability described in the present invention.
It is understood that the present invention is not limited to the particular embodiments illustrated herein, but embraces such modified forms thereof as come within the scope of the following claims.
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A telecommunication device for the deaf operates under conventional Baudot communication protocol, but has enhanced features enabling it to handle interrupts either from a conventional or a similar TDD. The improved TDD is also capable of pseudo-duplex communication with a similar TDD in which each device transmits packets of characters alternatively to the other thus making it appear to the users that simultaneous transmission is occurring. The implementation of these features is done in such a way that the TDD is fully capable of communication with existing TDD devices and the device obeys normals rules and conventions for Baudot communication.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a Continuation-In-Part of pending U.S. patent application Ser. No. 11/356,515, entitled “LUGGAGE COVER,” filed on Feb. 17, 2006, which is hereby incorporated by reference for all purposes.
TECHNICAL FIELD
The invention relates generally to covers for articles of luggage and, more particularly, to a cover for an article of luggage with wheels that preserves the aesthetic appearance of the luggage at a low cost.
BACKGROUND
Today, luggage has become an element of fashion. As a result, a number of designer articles of luggage can be purchased. The cost of these articles of luggage can range from less than one hundred dollars to thousands of dollars. Additionally, as anyone who has ever traveled on an airliner has experienced, the processing of baggage is a course process where damage to articles of luggage is not uncommon. In fact, one manufacturer even marketed their articles of luggage as durable, showing a gorilla (a baggage handler) that was attempting to destroy their articles of luggage in a television commercial.
Thus, a dilemma has developed between fashion and protection with respect to articles of luggage. Many have attempted to solve this dilemma by placing a cover over fashionable as well as other articles of luggage. Some examples of this are U.S. Pat. Nos. 2,487,596, 2,647,595, 2,711,234, 2,724,467, 3,901,360, 4,307,765, 5,083,644, 5,107,971, 5,172,795, 5,255,765, 5,293,975, 5,547,051, 6,637,562, U.S. Patent Application No. 2004/0206431, U.S. Design Pat. No. D338,559, and U.S. Design Pat. No. D345,652. However, none of these patents sufficiently address the problems of ease of use and expense, as well as a host of other problems.
Therefore, there is a need for an improved luggage cover that can accommodate the various physical aspects of modern articles of luggage (wheels, extendable handles, etc.) while not interfering with aesthetics.
SUMMARY
The present invention, accordingly, provides a luggage cover having a first side panel, an opposite second side panel, and a main panel. The second side panel is substantially parallel to the first side panel. Each of the panels is generally laminar. The main panel is generally disposed between the first side panel and the second side panel having a first, a second, a third, and a fourth edge. Specifically, the main panel is dimensioned to cover a plurality of sides of an article of luggage where the first and second edges are generally parallel to one another. The third edge of the main panel also includes an integral securing member and fastener for securing the third edge to the fourth edge. Moreover, the first edge is secured to the majority of the perimeter of the first side panel, and the second edge is secured to the majority of the perimeter of the second side panel. Additionally, a first ligature is provided to secure the first and second side panels together.
In an embodiment of the present invention, the first side panel, the second side panel, and the main panel are each made of a water-repellant, transparent, and non-rigid material.
In an embodiment of the present invention, the first side panel and the second side panel are sewn to the main panel.
In an embodiment of the present invention, the luggage cover further comprises at least one substantially open end when the third edge is secured to the fourth edge.
In an embodiment of the present invention, at least one aperture is located on at least the first side panel, the second panel, and the main panel, wherein the aperture is generally coextensive with luggage handles.
In an embodiment of the present invention, the securing member is comprised of a strap.
In an embodiment of the present invention, the fastener is a hook and loop fastener.
In an embodiment of the present invention, printed material is embedded in at least one of the main panel, the first side panel, and the second side panel.
Additionally, the present invention can also include a luggage cover with a main panel formed of a laminar transparent material and having two side edges. The main panel is generally oblong and dimensioned to cover three sides of an article of luggage. Also, a pair of side panels is provided, where each side panel has a pair of opposed edges. Additionally, the opposed edges of each side panels is secured to at least one edge of the main panel, and the assembly covers at least five sides of the article of luggage. Furthermore, a plurality of closure panels associated with the main panel and the side panels is provided. The closure panels include fasteners, wherein the closure panel extends around a side of the article of luggage not covered by the main panel and side panels and the fastener secures the main and side panels to the article of luggage.
The foregoing has outlined rather broadly the features and technical advantages of the present invention in order that the detailed description of the invention that follows may be better understood. Additional features and advantages of the invention will be described hereinafter which form the subject of the claims of the invention. It should be appreciated by those skilled in the art that the conception and the specific embodiment disclosed may be readily utilized as a basis for modifying or designing other structures for carrying out the same purposes of the present invention. It should also be realized by those skilled in the art that such equivalent constructions do not depart from the spirit and scope of the invention as set forth in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the present invention, and the advantages thereof, reference is now made to the following descriptions taken in conjunction with the accompanying drawings, in which:
FIG. 1 is an isometric view of a luggage cover in accordance with a preferred embodiment of the present invention, which is covering a wheeled article of luggage;
FIG. 2A is a plan view of the main panel;
FIGS. 2B and 2C are plan views of the side panels;
FIG. 3 is an isometric view of the luggage cover of FIG. 1 ;
FIG. 4 is a front view of the luggage cover of FIG. 1 ;
FIG. 5 is a side view of the luggage cover of FIG. 1 ;
FIG. 6 is another side view of the luggage cover of FIG. 1 ;
FIG. 7 is a top view of the luggage cover of FIG. 1 ; and
FIG. 8 is a bottom view of the luggage cover of FIG. 1 .
DETAILED DESCRIPTION
Refer now to the drawings wherein depicted elements are, for the sake of clarity, not necessarily shown to scale and wherein like or similar elements are designated by the same reference numeral through the several views.
Referring to FIGS. 1-8 of the drawings, the reference numeral 100 generally designates a luggage cover. As seen in FIG. 1 , luggage cover 100 is dimensioned to cover an article of luggage or conventional wheeled luggage 200 , allowing access to wheels and handles while covering and protecting. The cover 100 can come in a variety of shapes and sizes to cover articles of luggage of different dimensions. For example, cover 100 can be dimensioned to cover an article of luggage 22.00 inches in height by 14.00 inches in width by 7.75 inches in depth. Preferably, the luggage cover 100 comprises a main panel 102 , a first side panel 104 , and a second side panel 106 .
Each of the panels 102 , 104 , and 106 are comprised of a substantially laminar or flat material, such as an extruded plastic like polyethylene. The material that comprises the panels 102 , 104 , and 106 should be generally transparent so as to allow persons to view the fashionable articles of luggage through the cover 100 . Additionally, the material that comprises the panels 102 , 104 , and 106 can be a waterproof or water-resistant material so that the cover 100 can provide a barrier between the article of luggage and the elements.
Preferably, cover 100 is designed to cover substantially rectangular or parallelepiped shaped articles of luggage, such as conventional wheeled luggage. Moreover, cover 100 can be easily slid over the article of luggage and secured into place by a securing member 108 or closure panel, such as a strap. As seen in FIGS. 1-8 , the securing member 108 is a strap having lateral supports, increased width, or curved reliefs 109 on its fixed end to prevent tearing.
To provide this, the main panel 102 can be dimensioned to cover three panels (i.e. front, top, and rear) of the conventional rectangular article of luggage. Along either side of the cover 100 are the first side panel 104 and the second side panel 106 . When fully extended, the first side 104 and the second side 106 are generally parallel to one other. Each of the first side panel 104 and the second side panel 106 are secured to edges of the main panel 102 to form a seam 118 . Preferably, seam 118 encompasses the majority of the perimeter of each of the first side panel 104 and the second side panel 106 . Typically, the seam 118 can be formed by sewing or welding the respective panels 102 , 104 , and 106 together. Additionally, side panels 104 and 106 typically have the same general dimensions, making the manufacture of the cover 100 easier because a single jig or template can be used to make both side panels 104 and 106 .
Once the main panel 102 and the side panels 104 and 106 are secured together, the bottom of the cover 100 forms an opening 120 . Opening 120 enables a user to be able to slide the cover 100 over articles of luggage so that the majority of the surface area is covered by the cover 100 . To prevent the cover 100 from sliding off of the articles of luggage, a securing member or closure panel 108 covers at least a portion of opening 120 . Preferably, the securing member or closure panel 108 is integral to the main panel 102 , but the securing member 108 may, alternatively, be secured to the main panel 102 by sewing or welding. Additionally, the securing member 108 can be comprised of a transparent laminar material that is waterproof or water resistant, such as polyethylene.
In addition to securing member 108 , first ligature 130 and second ligature 134 are provided, which are typically made of NYLON®. First ligature 130 is secured at one end to first side panel 104 while second ligature 134 is secured at one end to the second side panel 106 . The free ends of the first ligature 130 and second ligature 134 are then adapted to be secured to one another so as to provide a “supporting strap” that is generally perpendicular to the securing member 108 .
The securing of the free end of the securing member 108 to the main panel 102 is preferably accomplished by use of a fastener 110 . As shown in FIGS. 1-8 , the fastener 110 is a hook and loop system comprising a hook member 112 and a loop member 114 . Additionally (as with the securing member 108 and main panel 102 ), the ligatures 130 and 134 are secured together at their respective free ends with hook member 132 and loop member 136 . As has been established over the past 25 years or so, hook and loop securing systems can provide a reliable and easily removable fastener. Additionally, snap-on, as well as other removable fasteners, can employed.
In addition to protecting the article of luggage, such as the article 200 , the cover 100 should also be functional. Specifically, a user should be able to use handles or other carrying members provided by the articles of luggage. If a cover does not allow access to these handles, then one of the purposes of the articles of luggage is lost. To account for usage of the handles, holes 116 are strategically located on the cover 100 to allow access to handles or other carrying members. Specifically, a variety of hole patterns can be used so that the holes 116 correspond to handles or carrying members of different brands of luggage and be generally coextensive with those carrying members or handles. As shown in FIGS. 1-8 , the main panel 102 includes two holes 116 for handles or carrying members, while each of the side panels includes a single hole 116 for a handle or carrying member.
Because there are also areas within the cover 100 , where there is not a seam 118 , the possibility of tearing exists. To prevent tearing of the cover 100 , the welds (typically melting) or sewn seams can be formed. Typically, these areas are located around the holes 116 and along the perimeter of opening 120 . Thus, the forming of welds or sewn seams prevents a substantial amount of tearing.
One other aspect of the invention is the use of silk-screening or other imprinting techniques with the cover 100 . Cover 100 generally is inexpensive to manufacture and could be given out by travel agents, hotels, and so forth as complimentary items. These covers 100 would serve their purpose of providing protection for patrons' or customers' articles of luggage as well as providing advertising. Specifically, silk-screening, molding, or any other way of imprinting or embedding printed matter into or onto the cover while also not interfering with the general transparency of cover 100 . Specifically, the printed matter can include text, graphics, logos, and so forth.
Having thus described the present invention by reference to certain of its preferred embodiments, it is noted that the embodiments disclosed are illustrative rather than limiting in nature and that a wide range of variations, modifications, changes, and substitutions are contemplated in the foregoing disclosure and, in some instances, some features of the present invention may be employed without a corresponding use of the other features. Many such variations and modifications may be considered obvious and desirable by those skilled in the art based upon a review of the foregoing description of preferred embodiments. Accordingly, it is appropriate that the appended claims be construed broadly and in a manner consistent with the scope of the invention.
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Today, luggage has become an element of fashion. As a result, a number of designer articles of luggage can be purchased. The cost of these articles of luggage can range from less than one hundred dollars to thousands of dollars. However, adequate protection for these articles of luggage, which preserves the aesthetic features of the articles of luggage, has not been previously available. Now, a simple, cheap, easily manufacturable, and easily used cover is available for articles of luggage that both protects and preserves the aesthetic features. This cover also allows easy access to handles and works well with conventional wheeled luggage.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application is a divisional of U.S. patent application Ser. No. 10/184,833, filed on Jun. 28, 2002, now U.S. Pat. No. 6,964,301.
TECHNICAL FIELD
The invention relates to apparatus and methods for collecting fluid samples from subsurface formations.
BACKGROUND OF THE INVENTION
The collection and sampling of underground fluids contained in subsurface formations is well known. In the petroleum exploration and recovery industries, for example, samples of formation fluids are collected and analyzed for various purposes, such as to determine the existence, composition and producibility of subsurface hydrocarbon fluid reservoirs. This aspect of the exploration and recovery process can be crucial in developing drilling strategies and impacts significant financial expenditures and savings.
To conduct valid fluid analysis, the fluid obtained from the subsurface formation should possess sufficient purity, or be virgin fluid, to adequately represent the fluid contained in the formation. As used herein, and in the other sections of this patent, the terms “virgin fluid”, “acceptable virgin fluid” and variations thereof mean subsurface fluid that is pure, pristine, connate, uncontaminated or otherwise considered in the fluid sampling and analysis field to be sufficiently or acceptably representative of a given formation for valid hydrocarbon sampling and/or evaluation.
Various challenges may arise in the process of obtaining virgin fluid from subsurface formations. Again with reference to the petroleum-related industries, for example, the earth around the borehole from which fluid samples are sought typically contains contaminates, such as filtrate from the mud utilized in drilling the borehole. This material often contaminates the virgin fluid as it passes through the borehole, resulting in fluid that is generally unacceptable for hydrocarbon fluid sampling and/or evaluation. Such fluid is referred to herein as “contaminated fluid.” Because fluid is sampled through the borehole, mudcake, cement and/or other layers, it is difficult to avoid contamination of the fluid sample as it flows from the formation and into a downhole tool during sampling. A challenge thus lies in minimizing the contamination of the virgin fluid during fluid extraction from the formation.
FIG. 1 depicts a subsurface formation 16 penetrated by a wellbore 14 . A layer of mud cake 15 lines a sidewall 17 of the wellbore 14 . Due to invasion of mud filtrate into the formation during drilling, the wellbore is surrounded by a cylindrical layer known as the invaded zone 19 containing contaminated fluid 20 that may or may not be mixed with virgin fluid. Beyond the sidewall of the wellbore and surrounding contaminated fluid, virgin fluid 22 is located in the formation 16 . As shown in FIG. 1 , contaminates tend to be located near the wellbore wall in the invaded zone 19 .
FIG. 2 shows the typical flow patterns of the formation fluid as it passes from subsurface formation 16 into a downhole tool 1 . The downhole tool 1 is positioned adjacent the formation and a probe 2 is extended from the downhole tool through the mudcake 15 to the sidewall 17 of the wellbore 14 . The probe 2 is placed in fluid communication with the formation 16 so that formation fluid may be passed into the downhole tool 1 . Initially, as shown in FIG. 1 , the invaded zone 19 surrounds the sidewall 17 and contains contamination. As fluid initially passes into the probe 2 , the contaminated fluid 20 from the invaded zone 19 is drawn into the probe with the fluid thereby generating fluid unsuitable for sampling. However, as shown in FIG. 2 , after a certain amount of fluid passes through the probe 2 , the virgin fluid 22 breaks through and begins entering the probe. In other words, a more central portion of the fluid flowing into the probe gives way to the virgin fluid, while the remaining portion of the fluid is contaminated fluid from the invasion zone. The challenge remains in adapting to the flow of the fluid so that the virgin fluid is collected in the downhole tool during sampling.
Various methods and devices have been proposed for obtaining subsurface fluids for sampling and evaluation. For example, U.S. Pat. No. 6,230,557 to Ciglenec et al., U.S. Pat. No. 6,223,822 to Jones, U.S. Pat. No. 4,416,152 to Wilson, U.S. Pat. No. 3,611,799 to Davis and International Pat. App. Pub. No. WO 96/30628 have developed certain probes and related techniques to improve sampling. Other techniques have been developed to separate virgin fluids during sampling. For example, U.S. Pat. No. 6,301,959 to Hrametz et al. and discloses a sampling probe with two hydraulic lines to recover formation fluids from two zones in the borehole. Borehole fluids are drawn into a guard zone separate from fluids drawn into a probe zone. Despite such advances in sampling, there remains a need to develop techniques for fluid sampling to optimize the quality of the sample and efficiency of the sampling process.
In considering existing technology for the collection of subsurface fluids for sampling and evaluation, there remains a need for apparatus and methods having one or more, among others, of the following attributes: the ability to selectively collect virgin fluid apart from contaminated fluid; the ability to separate virgin fluid from contaminated fluid; the ability to optimize the quantity and/or quality of virgin fluid extracted from the formation for sampling; the ability to adjust the flow of fluid according to the sampling needs; the ability to control the sampling operation manually and/or automatically and/or on a real-time basis. To this end, the present invention seeks to optimize the sampling process.
BRIEF SUMMARY OF THE INVENTION
In one aspect, the present invention relates to a probe deployable from a downhole tool positionable in a wellbore surrounded by a layer of contaminated fluid. The wellbore penetrates a subsurface formation having virgin fluid therein beyond the layer of contaminated fluid. The sampling probe comprises a housing and a sampling intake. The housing is engageable with a sidewall of the wellbore. The housing is also in fluid communication with the subsurface formation whereby the fluids flows from the subterranean formation through the housing and into the downhole tool. The sampling intake is positioned within said housing and in non-engagement with the sidewall of the wellbore. The sampling intake is adapted to receive at least a portion of the virgin fluid flowing through the housing.
In another aspect, the invention relates to a downhole tool useful for extracting fluid from a subsurface formation penetrated by a wellbore surrounded by a layer of contaminated fluid, the subsurface formation having virgin fluid therein beyond the layer of contaminated fluid. The downhole tool comprises a probe carried by the downhole tool. The probe is positionable in fluid communication with the formation whereby the fluids flow from the subterranean formation through the housing and into the downhole tool. The probe has a wall therein defining a first channel and a second channel. The wall is adjustably positionable within the probe whereby the flow of the virgin fluid through the first channel and into the downhole tool is optimized.
In another aspect of the invention, a downhole tool useful for extracting virgin fluid from a subsurface formation penetrated by a wellbore surrounded by contaminated fluid is provided. The downhole tool comprises a probe, first and second flow lines and at least one pump. The probe is positionable in fluid communication with the formation and has a wall therein defining a first channel and a second channel. The wall is adjustably positionable within the probe whereby the flow of virgin fluid into the first channel is optimized. The first flow line is in fluid communication with the first channel. The second flow line is in fluid communication with the second channel. The pump(s) draw the fluids from the formation into the flow lines.
In another aspect, the invention relates to a method of sampling virgin fluid from a subterranean formation penetrated by a wellbore surrounded by contaminated fluid, the subterranean formation having virgin fluid therein. The method comprises positioning a downhole tool in the wellbore adjacent the subterranean formation, the downhole tool having a probe adapted to draw fluid therein, positioning the probe in fluid communication with the formation, the probe having a wall therein defining a first channel and a second channel, drawing at least a portion of the virgin fluid through the first channel and into the downhole tool, and selectively adjusting the wall within the probe whereby the flow of virgin fluid into the downhole tool is optimized.
In yet another aspect, the invention relates to a method of sampling virgin fluid from a subterranean formation penetrated by a wellbore surrounded by contaminated fluid, the subterranean formation having virgin fluid therein. The method comprises positioning a downhole tool in the wellbore adjacent the subterranean formation, the downhole tool having a probe adapted to draw fluid therein, positioning the probe in fluid communication with the formation, the probe having a wall therein defining a first channel and a second channel, drawing at least a portion of the virgin fluid into the first channel in the probe and selectively adjusting the flow of fluid into the channels whereby the flow of virgin fluid into the probe is optimized.
Another aspect of the invention relates to a downhole tool useful for extracting virgin fluid from a subsurface formation penetrated by a wellbore surrounded by contaminated fluid. The apparatus comprises a probe, a contamination monitor and a controller. The probe is positionable in fluid communication with the formation and adapted to flow the fluids from the formation into the downhole tool. The probe has a wall therein defining a first channel and a second channel. The contamination monitor is adapted to measure fluid parameters in at least one of the channels. The controller is adapted to receive data from the contamination monitor and send command signals in response thereto whereby the wall is selectively adjusted within the probe to optimize the flow of the virgin fluid through the first channel and into the downhole tool.
Another aspect of the invention relates to a downhole tool useful for extracting virgin fluid from a subsurface formation penetrated by a wellbore surrounded by contaminated fluid. The downhole tool comprises a probe, first and second flow lines, at least one pump, a monitor and a controller. The probe is positionable in fluid communication with the formation and adapted to flow the fluids from the formation into the downhole tool. The probe has a wall therein defining a first channel and a second channel. The first flow line is in fluid communication with the first channel. The second flow line is in fluid communication with the second channel. The pump(s) draw the fluids from the formation. The contamination monitor is adapted to measure fluid parameters in at least one of the channels. The controller is adapted to receive data from the contamination monitor and send command signals in response thereto whereby the pump is selectively activated to draw fluid into the flow lines to optimize the flow of the virgin fluid through the first channel and into the downhole tool.
In another aspect, the invention relates to a method of sampling virgin fluid from a subterranean formation penetrated by a wellbore surrounded by contaminated fluid, the subterranean formation having virgin fluid therein. The method comprises positioning a probe in fluid communication with the formation, the probe carried by a downhole tool and having a wall therein defining a first channel and a second channel, flowing the fluids through the probe and into the downhole tool, monitoring fluid parameters of the fluid passing through the probe, and selectively adjusting the flow of fluids into the probe in response to the fluid parameters whereby the flow of virgin fluid through the first channel and into the downhole tool is optimized.
The invention also relates to a downhole apparatus for separating virgin fluid and contaminated fluid extracted from a subsurface formation. The downhole apparatus comprises a fluid sampling probe and means for separating virgin fluid. The fluid sampling probe has first and second pathways in fluid communication with each other and the subsurface formation. The means is capable of separating virgin fluid extracted from the subsurface formation and contaminated fluid extracted from the subsurface formation, whereby separation of the virgin and contaminated fluids occurs within said fluid sampling probe, and whereby contaminated fluid is extracted through said first pathway and virgin fluid is extracted through said second pathway.
Other aspects and advantages of the invention will be apparent from the following description and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
For a detailed description of preferred embodiments of the invention, reference will now be made to the accompanying drawings wherein:
FIG. 1 is a schematic view of a subsurface formation penetrated by a wellbore lined with mudcake, depicting the virgin fluid in the subsurface formation.
FIG. 2 is a schematic view of a down hole tool positioned in the wellbore with a probe extending to the formation, depicting the flow of contaminated and virgin fluid into a downhole sampling tool.
FIG. 3 is a schematic view of down hole wireline tool having a fluid sampling device.
FIG. 4 is a schematic view of a downhole drilling tool with an alternate embodiment of the fluid sampling device of FIG. 3 .
FIG. 5 is a detailed view of the fluid sampling device of FIG. 3 depicting an intake section and a fluid flow section.
FIG. 6A is a detailed view of the intake section of FIG. 5 depicting the flow of fluid into a probe having a wall defining an interior channel, the wall recessed within the probe.
FIG. 6B is an alternate embodiment of the probe of FIG. 6A having a wall defining an interior channel, the wall flush with the probe.
FIG. 6C is an alternate embodiment of the probe of FIG. 6A having a sizer capable of reducing the size of the interior channel.
FIG. 6D is a cross-sectional view of the probe of FIG. 6C .
FIG. 6E is an alternate embodiment of the probe of FIG. 6A having a sizer capable of increasing the size of the interior channel.
FIG. 6F is a cross-sectional view of the probe of FIG. 6E .
FIG. 6G is an alternate embodiment of the probe of FIG. 6A having a pivoter that adjusts the position of the interior channel within the probe.
FIG. 6H is a cross-sectional view of the probe of FIG. 6G .
FIG. 6I is an alternate embodiment of the probe of FIG. 6A having a shaper that adjusts the shape of the probe and/or interior channel.
FIG. 6J is a cross-sectional view of the probe of FIG. 6I .
FIG. 7A is a schematic view of the probe of FIG. 6A with the flow of fluid from the formation into the probe with the pressure and/or flow rate balanced between the interior and exterior flow channels for substantially linear flow into the probe.
FIG. 7B is a schematic view of the probe of FIG. 7A with the flow rate of the interior channel greater than the flow rate of the exterior channel.
FIG. 8A is a schematic view of an alternate embodiment of the downhole tool and fluid flowing system having dual packers and walls.
FIG. 8B is a schematic view of the downhole tool of FIG. 8A with the walls moved together in response to changes in the fluid flow.
FIG. 8C is a schematic view of the flow section of the downhole tool of FIG. 8A .
FIG. 9 is a schematic view of the fluid sampling device of FIG. 5 having flow lines with individual pumps.
FIG. 10 is a graphical depiction of the optical density signatures of fluid entering the probe at a given volume.
FIG. 11A is a graphical depiction of optical density signatures of FIG. 10 deviated during sampling at a given volume.
FIG. 11B is a graphical depiction of the ratio of flow rates corresponding to the given volume for the optical densities of FIG. 11A .
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Presently preferred embodiments of the invention are shown in the above-identified figures and described in detail below. In describing the preferred embodiments, like or identical reference numerals are used to identify common or similar elements. The figures are not necessarily to scale and certain features and certain views of the figures may be shown exaggerated in scale or in schematic in the interest of clarity and conciseness.
Referring to FIG. 3 , an example environment within which the present invention may be used is shown. In the illustrated example, the present invention is carried by a down hole tool 10 . An example commercially available tool 10 is the Modular Formation Dynamics Tester (MDT) by Schlumberger Corporation, the assignee of the present application and further depicted, for example, in U.S. Pat. Nos. 4,936,139 and 4,860,581 hereby incorporated by reference herein in their entireties.
The downhole tool 10 is deployable into bore hole 14 and suspended therein with a conventional wire line 18 , or conductor or conventional tubing or coiled tubing, below a rig 5 as will be appreciated by one of skill in the art. The illustrated tool 10 is provided with various modules and/or components 12 , including, but not limited to, a fluid sampling device 26 used to obtain fluid samples from the subsurface formation 16 . The fluid sampling device 26 is provided with a probe 28 extendable through the mudcake 15 and to sidewall 17 of the borehole 14 for collecting samples. The samples are drawn into the downhole tool 10 through the probe 28 .
While FIG. 3 depicts a modular wireline sampling tool for collecting samples according to the present invention, it will be appreciated by one of skill in the art that such system may be used in any downhole tool. For example, FIG. 4 shows an alternate downhole tool 10 a having a fluid sampling system 26 a therein. In this example, the downhole tool 10 a is a drilling tool including a drill string 29 and a drill bit 30 . The downhole drilling tool 10 a may be of a variety of drilling tools, such as a Measurement-While-Drilling (MWD), Logging-While Drilling (LWD) or other drilling system. The tools 10 and 10 a of FIGS. 3 and 4 , respectively, may have alternate configurations, such as modular, unitary, wireline, coiled tubing, autonomous, drilling and other variations of downhole tools.
Referring now to FIG. 5 , the fluid sampling system 26 of FIG. 3 is shown in greater detail. The sampling system 26 includes an intake section 25 and a flow section 27 for selectively drawing fluid into the desired portion of the downhole tool.
The intake section 25 includes a probe 28 mounted on an extendable base 30 having a seal 31 , such as a packer, for sealingly engaging the borehole wall 17 around the probe 28 . The intake section 25 is selectively extendable from the downhole tool 10 via extension pistons 33 . The probe 28 is provided with an interior channel 32 and an exterior channel 34 separated by wall 36 . The wall 36 is preferably concentric with the probe 28 . However, the geometry of the probe and the corresponding wall may be of any geometry. Additionally, one or more walls 36 may be used in various configurations within the probe.
The flow section 27 includes flow lines 38 and 40 driven by one or more pumps 35 . A first flow line 38 is in fluid communication with the interior channel 32 , and a second flow line 40 is in fluid communication with the exterior channel 34 . The illustrated flow section may include one or more flow control devices, such as the pump 35 and valves 44 , 45 , 47 and 49 depicted in FIG. 5 , for selectively drawing fluid into various portions of the flow section 27 . Fluid is drawn from the formation through the interior and exterior channels and into their corresponding flow lines.
Preferably, contaminated fluid may be passed from the formation through exterior channel 34 , into flow line 40 and discharged into the wellbore 14 . Preferably, fluid passes from the formation into the interior channel 32 , through flow line 38 and either diverted into one or more sample chambers 42 , or discharged into the wellbore. Once it is determined that the fluid passing into flow line 38 is virgin fluid, a valve 44 and/or 49 may be activated using known control techniques by manual and/or automatic operation to divert fluid into the sample chamber.
The fluid sampling system 26 is also preferably provided with one or more fluid monitoring systems 53 for analyzing the fluid as it enters the probe 28 . The fluid monitoring system 53 may be provided with various monitoring devices, such as optical fluid analyzers, as will be discussed more fully herein.
The details of the various arrangements and components of the fluid sampling system 26 described above as well as alternate arrangements and components for the system 26 would be known to persons skilled in the art and found in various other patents and printed publications, such as, those discussed herein. Moreover, the particular arrangement and components of the downhole fluid sampling system 26 may vary depending upon factors in each particular design, or use, situation. Thus, neither the system 26 nor the present invention are limited to the above described arrangements and components and may include any suitable components and arrangement. For example, various flow lines, pump placement and valving may be adjusted to provide for a variety of configurations. Similarly, the arrangement and components of the downhole tool 10 may vary depending upon factors in each particular design, or use, situation. The above description of exemplary components and environments of the tool 10 with which the fluid sampling device 26 of the present invention may be used is provided for illustrative purposes only and is not limiting upon the present invention.
With continuing reference to FIG. 5 , the flow pattern of fluid passing into the downhole tool 10 is illustrated. Initially, as shown in FIG. 1 , an invaded zone 19 surrounds the borehole wall 17 . Virgin fluid 22 is located in the formation 16 behind the invaded zone 19 . At some time during the process, as fluid is extracted from the formation 16 into the probe 28 , virgin fluid breaks through and enters the probe 28 as shown in FIG. 5 . As the fluid flows into the probe, the contaminated fluid 22 in the invaded zone 19 near the interior channel 32 is eventually removed and gives way to the virgin fluid 22 . Thus, only virgin fluid 22 is drawn into the interior channel 32 , while the contaminated fluid 20 flows into the exterior channel 34 of the probe 28 . To enable such result, the flow patterns, pressures and dimensions of the probe may be altered to achieve the desired flow path as will be described more fully herein.
Referring now to FIGS. 6A–6J , various embodiments of the probe 28 are shown in greater detail. In FIG. 6A , the base 30 is shown supporting the seal 31 in sealing engagement with the borehole wall 17 . The probe 28 preferably extends beyond the seal 31 and penetrates the mudcake 15 . The probe 28 is placed in fluid communication with the formation 16 .
The wall 36 is preferably recessed a distance within the probe 28 . In this configuration, pressure along the formation wall is automatically equalized in the interior and exterior channels. The probe 28 and the wall 36 are preferably concentric circles, but may be of alternate geometries depending on the application or needs of the operation. Additional walls, channels and/or flow lines may be incorporated in various configurations to further optimize sampling.
The wall 36 is preferably adjustable to optimize the flow of virgin fluid into the probe. Because of varying flow conditions, it is desirable to adjust the position of the wall 36 so that the maximum amount of virgin fluid may be collected with the greatest efficiency. For example, the wall 36 may be moved or adjusted to various depths relative to the probe 28 . As shown in FIG. 6B , the wall 36 may be positioned flush with the probe. In this configuration, the pressure in the interior channel along the formation may be different from the pressure in the exterior channel along the formation.
Referring now to FIGS. 6C–6H , the wall 36 is preferably capable of varying the size and/or orientation of the interior channel 32 . As shown in FIG. 6C through 6F , the diameter of a portion or all of the wall 36 is preferably adjustable to align with the flow of contaminated fluid 20 from the invaded zone 19 and/or the virgin fluid 22 from the formation 16 into the probe 28 . The wall 36 may be provided with a mouthpiece 41 and a guide 40 adapted to allow selective modification of the size and/or dimension of the interior channel. The mouthpiece 41 is selectively movable between an expanded and a collapsed position by moving the guide 40 along the wall 36 . In FIGS. 6C and 6D , the guide 40 is surrounds the mouthpiece 41 and maintains it in the collapsed position to reduce the size of the interior flow channel in response to a narrower flow of virgin fluid 22 . In FIGS. 6E and 6F , the guide 41 is retracted so that the mouthpiece 41 is expanded to increase the size of the interior flow channel in response to a wider flow of virgin fluid 22 .
The mouthpiece depicted in FIGS. 6C–6F may be a folded metal spring, a cylindrical bellows, a metal energized elastomer, a seal, or any other device capable of functioning to selectively expand or extend the wall as desired. Other devices capable of expanding the cross-sectional area of the wall 36 may be envisioned. For example, an expandable spring cylinder pinned at one end may also be used.
As shown in FIGS. 6G and 6H , the probe 28 may also be provided with a wall 36 a having a first portion 42 , a second portion 43 and a seal bearing 45 therebetween to allow selective adjustment of the orientation of the wall 36 a within the probe. The second portion 43 is desirably movable within the probe 28 to locate an optimal alignment with the flow of virgin fluid 20 .
Additionally, as shown in FIGS. 6I and 6J , one or more shapers 44 may also be provided to conform the probe 28 and/or wall 36 into a desired shape. The shapers 44 have two more fingers 50 adapted to apply force to various positions about the probe and/or wall 36 causing the shape to deform. When the probe 40 and or wall 36 are extended as depicted in FIG. 6E , the shaper 44 may be extended about at least a portion of the mouthpiece 41 to selectively deform the mouthpiece to the desired shape. If desired, the shapers apply pressure to various positions around the probe and/or wall to generate the desired shape.
The sizer, pivoter and/or shaper may be any electronic mechanism capable of selectively moving the wall 36 as provided herein. One or more devices may be used to perform one or more of the adjustments. Such devices may include a selectively controllable slidable collar, a pleated tube, or cylindrical bellows or spring, an elastomeric ring with embedded spring-biased metal fingers, a flared elastomeric tube, a spring cylinder, and/or any suitable components with any suitable capabilities and operation may be used to provide any desired variability.
These and other adjustment devices may be used to alter the channels for fluid flow. Thus, a variety of configurations may be generated by combining one or more of the adjustable features.
Now referring to FIGS. 7A and 7B , the flow characteristics are shown in greater detail. Various flow characteristics of the probe 28 may be adjusted. For example, as shown in FIG. 7A , the probe 28 may be designed to allow controlled flow separation of virgin fluid 22 into the interior channel 32 and contaminated fluid 20 into the exterior channel 34 . This may be desirable, for example, to assist in minimizing the sampling time required before acceptable virgin fluid is flowing into the interior channel 32 and/or to optimize or increase the quantity of virgin fluid flowing into the interior channel 32 , or other reasons.
The ratio of fluid flow rates within the interior channel 32 and the exterior channel 34 may be varied to optimize, or increase, the volume of virgin fluid drawn into the interior channel 32 as the amount of contaminated fluid 20 and/or virgin fluid 22 changes over time. The diameter d of the area of virgin fluid flowing into the probe may increase or decrease depending on wellbore and/or formation conditions. Where the diameter d expands, it is desirable to increase the amount of flow into the interior channel. This may be done by altering the wall 36 as previously described. Alternatively or simultaneously, the flow rates to the respective channels may be altered to further increase the flow of virgin fluid into the interior channel.
The comparative flow rate into the channels 32 and 34 of the probe 28 may be represented by a ratio of flow rates Q 1 /Q 2 . The flow rate into the interior channel 32 is represented by Q 1 and the flow rate in the exterior channel 34 is represented by Q 2 . The flow rate Q 1 in the interior channel 32 may be selectively increased and/or the flow rate Q 2 in the exterior channel 34 may be decreased to allow more fluid to be drawn into the interior channel 32 . Alternatively, the flow rate Q 1 in the interior channel 32 may be selectively decreased and/or the flow rate (Q 2 ) in the exterior channel 34 may be increased to allow less fluid to be drawn into the interior channel 32 .
As shown in FIG. 7A , Q 1 and Q 2 represent the flow of fluid through the probe 28 . The flow of fluid into the interior channel 32 may be altered by increasing or decreasing the flow rate to the interior channel 32 and/or the exterior channel 34 . For example, as shown in FIG. 7B , the flow of fluid into the interior channel 32 may be increased by increasing the flow rate Q 1 through the interior channel 32 , and/or by decreasing the flow rate Q 2 through the exterior channel 34 . As indicated by the arrows, the change in the ratio Q 1 /Q 2 steers a greater amount of the fluid into the interior channel 32 and increases the amount of virgin fluid drawn into the downhole tool ( FIG. 5 ).
The flow rates within the channels 32 and 34 may be selectively controllable in any desirable manner and with any suitable component(s). For example, one or more flow control device 35 is in fluid communication with each flowline 38 , 40 may be activated to adjust the flow of fluid into the respective channels ( FIG. 5 ). The flow control 35 and valves 45 , 47 and 49 of this example can, if desired, be actuated on a real-time basis to modify the flow rates in the channels 32 and 34 during production and sampling.
The flow rate may be altered to affect the flow of fluid and optimize the intake of virgin fluid into the downhole tool. Various devices may be used to measure and adjust the rates to optimize the fluid flow into the tool. Initially, it may be desirable to have increased flow into the exterior channel when the amount of contaminated fluid is high, and then adjust the flow rate to increase the flow into the interior channel once the amount of virgin fluid entering the probe increases. In this manner, the fluid sampling may be manipulated to increase the efficiency of the sampling process and the quality of the sample.
Referring now to FIGS. 8A and 8B , another embodiment of the present invention employing a fluid sampling system 26 b is depicted. A downhole tool 10 b is deployed into wellbore 14 on coiled tubing 58 . Dual packers 60 extend from the downhole tool 10 b and sealingly engage the sidewall 17 of the wellbore 14 . The wellbore 14 is lined with mud cake 15 and surrounded by an invaded zone 19 . A pair of cylindrical walls or rings 36 b are preferably positioned between the packers 60 for isolation from the remainder of the wellbore 14 . The packers 60 may be any device capable of sealing the probe from exposure to the wellbore, such as packers or any other suitable device.
The walls 36 b are capable of separating fluid extracted from the formation 16 into at least two flow channels 32 b and 34 b. The tool 10 b includes a body 64 having at least one fluid inlet 68 in fluid communication with fluid in the wellbore between the packers 60 . The walls 36 b are positioned about the body 64 . As indicated by the arrows, the walls 36 b are axially movable along the tool. Inlets positioned between the walls 36 preferably capture virgin fluid 22 , while inlets outside the walls 36 preferably draw in contaminated fluid 20 .
The walls 36 b are desirably adjustable to optimize the sampling process. The shape and orientation of the walls 36 b may be selectively varied to alter the sampling region. The distance between the walls 36 b and the borehole wall 17 , may be varied, such as by selectively extending and retracting the walls 36 b from the body 64 . The position of the walls 36 b may be along the body 64 . The position of the walls along the body 64 may to moved apart to increase the number of intakes 68 receiving virgin fluid, or moved together to reduce the number of intakes receiving virgin fluid depending on the flow characteristics of the formation. The walls 36 b may also be centered about a given position along the tool 10 b and/or a portion of the borehole 14 to align certain intakes 68 with the flow of virgin fluid 22 into the wellbore 14 between the packers 60 .
The position of the movement of the walls along the body may or may not cause the walls to pass over intakes. In some embodiments, the intakes may be positioned in specific regions about the body. In this case, movement of the walls along the body may redirect flow within a given area between the packers without having to pass over intakes. The size of the sampling region between the walls 36 b may be selectively adjusted between any number of desirable positions, or within any desirable range, with the use of any suitable component(s) and technique(s).
An example of a flow system 27 b for selectively drawing fluid into the downhole tool is depicted in FIG. 8C . A fluid flow line 70 extends from each intake 68 into the downhole tool 10 b and has a corresponding valve 72 for selectively diverting fluid to either a sample chamber 75 or into the wellbore outside of the packers 60 . One or more pumps 35 may be used in coordination with the valves 72 to selectively draw fluid in at various rates to control the flow of fluid into the downhole tool. Contaminated fluid is preferably dispersed back to the wellbore. However, where it is determined that virgin fluid is entering a given intake, a valve 72 corresponding to the intake may be activated to deliver the virgin fluid to a sample chamber 75 . Various measurement devices, such as an OFA 59 may be used to evaluate the fluid drawn into the tool. Where multiple intakes are used, specific intakes may be activated to increase the flow nearest the central flow of virgin fluid, while intakes closer to the contaminated region may be decreased to effectively steer the highest concentration of virgin fluid into the downhole tool for sampling.
One or more probes 28 as depicted in any of FIGS. 3–6J may also be used in combination with the probe 28 b of FIGS. 8A or 8 B.
Referring to FIG. 9 , another view of the fluid sampling system 26 c of FIG. 5 is shown. In FIG. 9 , the flow lines 38 and 40 each have a pump 35 for selectively drawing fluid into the channels 32 and 34 of the probe 28 .
The fluid monitoring system 53 of FIG. 5 is shown in greater detail in FIG. 9 . The flow lines 38 and 40 each pass through the fluid monitoring system 53 for analysis therein. The fluid monitoring system 53 is provided with an optical fluid analyzer 73 for measuring optical density in flow line 40 and an optical fluid analyzer 74 for measuring optical density in flow line 38 . The optical fluid analyzer may be a device such as the analyzer described in U.S. Pat. Nos. 6,178,815 to Felling et at and/or U.S. Pat. No. 4,994,671 to Safinya et al., both of which are hereby incorporated by reference.
While the fluid monitoring system 53 of FIG. 9 is depicted as having an optical fluid analyzer for monitoring the fluid, it will be appreciated that other fluid monitoring devices, such as gauges, meters, sensors and/or other measurement or equipment incorporating for evaluation, may be used for determining various properties of the fluid, such as temperature, pressure, composition, contamination and/or other parameters known by those of skill in the art.
A controller 76 is preferably provided to take information from the optical fluid analyzer(s) and send signals in response thereto to alter the flow of fluid into the interior channel 32 and/or exterior channel 34 of the probe 28 . As depicted in FIG. 9 , the controller is part of the fluid monitoring system 53 ; however, it will be appreciated by one of skill in the art that the controller may be located in other parts of the downhole tool and/or surface system for operating various components within the wellbore system.
The controller is capable of performing various operations throughout the wellbore system. For example, the controller is capable of activating various devices within the downhole tool, such as selectively activating the sizer, pivoter, shaper and/or other probe device for altering the flow of fluid into the interior and/or exterior channels 32 , 34 of the probe. The controller may be used for selectively activating the pumps 35 and/or valves 44 , 45 , 47 , 49 for controlling the flow rate into the channels 32 , 34 , selectively activating the pumps 35 and/or valves 44 , 45 , 47 , 49 to draw fluid into the sample chamber(s) and/or discharge fluid into the wellbore, to collect and/or transmit data for analysis uphole and other functions to assist operation of the sampling process. The controller may also be used for controlling fluid extracted from the formation, providing accurate contamination parameter values useful in a contamination monitoring model, adding certainty in determining when extracted fluid is virgin fluid sufficient for sampling, enabling the collection of improved quality fluid for sampling, reducing the time required to achieve any of the above, or any combination thereof. However, the contamination monitoring calibration capability can be used for any other suitable purpose(s). Moreover, the use(s) of, or reasons for using, a contamination monitoring calibration capability are not limiting upon the present invention.
An example of optical density (OD) signatures generated by the optical fluid analyzers 73 and 74 of FIG. 9 is shown in FIG. 10 . FIG. 10 shows the relationship between OD and the total volume V of fluid as it passes into the interior and exterior channels of the probe. The OD of the fluid flowing through the interior channel 32 is depicted by line 80 . The OD of the fluid flowing through the exterior channel 34 is depicted as line 82 . The resulting signatures represented by lines 80 and 82 may be used to calibrate future measurements.
Initially, the OD of fluid flowing into the channels is at OD mf . OD mf represents the OD of the contaminated fluid adjacent the wellbore as depicted in FIG. 1 . Once the volume of fluid entering the interior channel reaches V 1 , virgin fluid breaks through. The OD of the fluid entering into the channels increases as the amount of virgin fluid entering into the channels increases. As virgin fluid enters the interior channel 32 , the OD of the fluid entering into the interior channel increases until it reaches a second plateau at V 2 represented by OD vf . While virgin fluid also enters the exterior channel 34 , most of the contaminated fluid also continues to enter the exterior channel. The OD of fluid in the exterior channel as represented by line 82 , therefore, increases, but typically does not reach the OD vf due to the presence of contaminates. The breakthrough of virgin fluid and flow of fluid into the interior and exterior channels is previously described in relation to FIG. 2 .
The distinctive signature of the OD in the internal channel may be used to calibrate the monitoring system or its device. For example, the parameter OD vf , which characterizes the optical density of virgin fluid can be determined. This parameter can be used as a reference for contamination monitoring. The data generated from the fluid monitoring system may then be used for analytical purposes and as a basis for decision making during the sampling process.
By monitoring the coloration generated at various optical channels of the fluid monitoring system 53 relative to the curve 80 , one can determine which optical channel(s) provide the optimum contrast readout for the optical densities OD mf and OD vf . These optical channels may then be selected for contamination monitoring purposes.
FIGS. 11A and 11B depict the relationship between the OD and flow rate of fluid into the probe. FIG. 11A shows the OD signatures of FIG. 10 that has been adjusted during sampling. As in FIG. 10 , line 82 shows the signature of the OD of the fluid entering the interior channel 32 , and 82 shows the signature of the OD of the fluid entering the exterior channel 34 . However, FIG. 11A further depicts evolution of the OD at volumes V 3 , V 4 and V 5 during the sampling process.
FIG. 11B shows the relationship between the ratio of flow rates Q 1 /Q 2 to the volume of fluid that enters the probe. As depicted in FIG. 7A , Q 1 relates to the flow rate into the interior channel 32 , and Q 2 relates to the flow rate into the exterior channel 34 of the probe 28 . Initially, as mathematically depicted by line 84 of FIG. 11B , the ratio of flow Q 1 /Q 2 is at a given level (Q 1 /Q 2 ) i corresponding to the flow ratio of FIG. 7A . However, the ratio Q 1 /Q 2 can then be gradually increased, as described with respect to FIG. 7B , so that the ratio of Q 1 /Q 2 increases. This gradual increase in flow ratio is mathematically depicted as the line 84 increases to the level (Q 1 /Q 2 ) n at a given volume, such as V 4 . As depicted in FIG. 11B , the ratio can be further increased up to V 5 .
As the ratio of flow rate increases, the corresponding OD of the interior channel 32 represented by lines 80 shifts to deviation 81 , and the OD of the exterior channel 34 represented by line 82 shifts to deviations 83 and 85 . The shifts in the ratio of flow depicted in FIG. 11B correspond to shifts in the OD depicted in FIG. 11A for volumes V 1 through V 5 . An increase in the flow rate ratio at V 3 ( FIG. 11B ) shifts the OD of the fluid flowing into the exterior channel from its expected path 82 to a deviation 83 ( FIG. 11B ). A further increase in ratio as depicted by line 84 at V 4 ( FIG. 11A ), causes a shift in the OD of line 80 from its reference level OD vf to a deviation 81 ( FIG. 11B ). The deviation of the OD of line 81 at V 4 , causes the OD of line 80 to return to its reference level OD vf at V 5 , while the OD of deviation 83 drops further along deviation 85 . Further adjustments to OD and/or ratio may be made to alter the flow characteristics of the sampling process.
It should also be understood that the discussion and various examples of methods and techniques described above need not include all of the details or features described above. Further, neither the methods described above, nor any methods which may fall within the scope of any of the appended claims, need be performed in any particular order. Yet further, the methods of the present invention do not require use of the particular embodiments shown and described in the present specification, such as, for example, the exemplary probe 28 of FIG. 5 , but are equally applicable with any other suitable structure, form and configuration of components.
Preferred embodiments of the present invention are thus well adapted to carry out one or more of the objects of the invention. Further, the apparatus and methods of the present invention offer advantages over the prior art and additional capabilities, functions, methods, uses and applications that have not been specifically addressed herein but are, or will become, apparent from the description herein, the appended drawings and claims.
While preferred embodiments of this invention have been shown and described, many variations, modifications and/or changes of the apparatus and methods of the present invention, such as in the components, details of construction and operation, arrangement of parts and/or methods of use, are possible, contemplated by the applicant, within the scope of the appended claims, and may be made and used by one of ordinary skill in the art without departing from the spirit or teachings of the invention and scope of appended claims. Because many possible embodiments may be made of the present invention without departing from the scope thereof, it is to be understood that all matter herein set forth or shown in the accompanying drawings is to be interpreted as illustrative and not limiting. Accordingly, the scope of the invention and the appended claims is not limited to the embodiments described and shown herein.
It should be understood that before any action is taken with respect to any apparatus, system or method in accordance with this patent specification, all appropriate regulatory, safety, technical, industry and other requirements, guidelines and safety procedures should be consulted and complied with, and the assistance of a qualified, competent personnel experienced in the appropriate fields obtained. Caution must be taken in manufacturing, handling, assembling, using, and disassembling any apparatus or system made or used in accordance with this patent specification.
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The apparatuses and methods herein relate to techniques for extracting fluid from a subsurface formation. A downhole sampling tool is provided with a probe having an internal wall capable of selectively diverting virgin fluids into virgin flow channels for sampling, while diverting contaminated fluids into contaminated flow channels to be discarded. The characteristics of the fluid passing through the channels of the probe may be measured. The data generated during sampling may be sent to a controller capable of generating data, communicating and/or sending command signals. The flow of fluid into the downhole tool may be selectively adjusted to optimize the flow of fluid into the channels by adjusting the internal wall within the probe and/or by adjusting the flow rates through the channels. The configuration of the internal wall and/or the flow rates may be automatically adjusted by the controller and/or manually manipulated to further optimize the fluid flow.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention concerns a hold-down device for a battery, particularly for automotive vehicles.
2. Description of the Related Art
In all types of automotive vehicles, the battery is a standard component whose dimensions are governed by precise standards. There are various types of known hold-down devices for placing and immobilizing the battery on the chassis of the vehicle. A first type of known hold-down device utilizes the upper surface of the battery and a second type of known hold-down device utilizes the lugs of the battery.
A first example of a hold-down device utilizing the upper surface of the battery consists in resting the battery on a support tray, placing two vertical rods one on each side of the battery and positioning a bracketing element that connects the two vertical rods above the battery. The hold-down device then exerts a vertical clamping action on the battery by bearing on its upper surface. The rods generally have threaded ends that pass through the bracketing element and cooperate with nuts to bring about the clamping action. However, this type of device calls for the use of tools, especially for tightening the nuts, and the manipulation of the various parts is exacting.
Other examples of hold-down devices utilizing the upper surface of the battery consist in employing a support tray having raised side walls replacing the vertical rods and cooperating with a bracketing element that connects the two walls of the tray and is fixed by one or two anchoring points. Another example of a hold-down device uses a simple fabric strap surrounding the battery with its ends fastened on one and the other side of the battery.
However, all these examples of hold-down devices utilizing the upper surface of the battery have proven overly complex, since they are made up of several easy-to-lose parts and necessitate the use of tools for installing and removing the battery. Furthermore, the retention of the battery in its support tray is not safeguarded.
A first example of a hold-down device utilizing the lugs of the battery is a metal clamp integral to the support tray and made to bear against a lug of the battery. The clamp is fixed to the support tray, for example by a screw fastening system, and produces a high clamping pressure on the lug of the battery. However, tools still have to be used to install and remove the battery, and the hold-down device is made up of several parts that are hard to manipulate. In addition, the production cost of such a device is still high.
Another example of a hold-down device utilizing the lug of the battery is a pivoting cam system. One side of the battery is gripped in a fixed lug on the support tray and the other side of the battery cooperates with a cam system mounted to rotate parallel to the support tray. The cam is set in motion manually by an eccentric, which comes to bear against the lug of the battery in the locking position, while at the same time applying a clamping force to the lug. However, this type of device also requires the use of a screwdriver-type tool, especially during the removal of the battery. In addition, dust can come to foul the internal friction zones of the hold-down device. This then creates difficulties in removing the battery.
Another example is given by the document FR 2 796 494, which describes a battery hold-down device that is an integral part of the support tray. As illustrated schematically in FIG. 1 , the hold-down device 10 for a battery 11 comprises a support tray 12 with a first flange 13 a , serving as a stop for a first lug 14 a of the battery 11 . The support tray 12 comprises a second flange 13 b provided with a deformable tab 15 , articulated in rotation according to arrow F 1 and designed to quickly immobilize and release the battery 11 . The immobilizing is done by pressing the second lug 14 b of the battery 11 against the tab 15 , which deforms, thereby making it possible to position the battery 11 on the floor of the support tray 12 . The battery 11 is loosened by exerting a pressure according to arrow F 2 on the free end of the tab 15 , which then releases the second lug 14 b of the battery 11 and allows the battery 11 to be disengaged.
Although this type of device avoids the use of tools, it does not ensure safeguarded retention of the battery 11 in the support tray 12 and does not make it possible to determine whether the lug of the battery is actually in place. In addition, such a hold-down device does not permit positive locking of the battery in the support tray.
SUMMARY OF THE INVENTION
The present invention provides a simple and inexpensive battery hold-down device of reduced weight and space consumption, permitting quick and reliable locking and unlocking of a standard battery on its support tray without the need to use tools.
The subject of the invention is characterized in that the support tray comprises at least one movable lug, connected to the second longitudinal flange and cooperating with a corresponding actuating lever and defining a first immobilizing surface for the second lug of the battery; and a locking means comprising a locking ramp that inserts itself between each movable lug and each corresponding actuating lever, said ramp comprising at least one locking wedge having a first, lower inclined surface associated with a second immobilizing surface of the corresponding movable lug, and a second, upper inclined surface associated with the corresponding actuating lever and designed to ensure positive locking of the actuating lever between a first, locking position that locks the position of the battery in the support tray and a second, unlocking position.
Such a hold-down device, employing a locking ramp cooperating both with movable lugs of the support tray and with actuating levers, makes it possible to effectively immobilize the position of the battery in its support tray and to ensure effective, reliable locking of that position.
In one embodiment, each movable lug is connected to the corresponding longitudinal flange of the support tray by means of two flexible connecting ridges that form elastic hinges and make it possible to shift the movable lug between a first, idle position, awaiting the battery, and a second position immobilizing the battery.
Such flexible hinges facilitate the drawing back of the movable lugs and their automatic return to their initial position.
In another embodiment of the invention, the upper surface of each locking wedge is provided with a plurality of notches.
The notches of the locking wedges ensure positive locking of the actuating levers to the locking ramp, preventing any inadvertent disengagement of the actuating levers.
In another embodiment, the locking ramp comprises a plurality of locking wedges, interconnected by rigid, high-mechanical-strength connection zones, and the support tray comprises a plurality of movable lugs, each associated with a corresponding actuating lever, which in turn is associated with a corresponding locking wedge. The actuating levers are connected in their respective upper portions by connecting bars that serve as gripping means for the levers.
Such a hold-down device is therefore easy to manipulate and ensures safeguarded locking of the position of the battery, since all the levers are simultaneously made to move toward the locking position.
BRIEF DESCRIPTION OF THE DRAWINGS
The above mentioned and other features and objects of this invention, and the manner of attaining them, will become more apparent and the invention itself will be better understood by reference to the following description of embodiments of the invention taken in conjunction with the accompanying drawings, wherein:
FIG. 1 schematically illustrates a partial view of a battery hold-down device according to the prior art;
FIGS. 2 and 3 respectively illustrate a perspective view and a partial cutaway front view of a hold-down device according to the invention, on which a battery is positioned;
FIGS. 4 and 5 respectively illustrate a front sectional view along axis A-A and a top view of a support tray of the hold-down device according to FIGS. 2 and 3 .
FIGS. 6 and 7 show two perspective views of the support tray according to FIGS. 4 and 5 ;
FIGS. 8 and 9 show two perspective views of a locking ramp of the hold-down device according to FIGS. 2 and 3 ;
FIG. 10 is a side sectional view along axis B-B of the locking ramp according to FIGS. 8 and 9 ;
FIGS. 11 to 17 show various successive steps in the installation of a battery on the hold-down device according to FIGS. 2 to 10 ; and
FIGS. 18 and 19 show two successive steps in the removal of the battery from the hold-down device according to FIGS. 2 to 17 .
Corresponding reference characters indicate corresponding parts throughout the several views. Although the exemplifications set out herein illustrate embodiments of the invention, in several forms, the embodiments disclosed below are not intended to be exhaustive or to be construed as limiting the scope of the invention to the precise forms disclosed.
DETAILED DESCRIPTION
Referring to FIGS. 2 and 3 , the hold-down device 10 is designed particularly to fix a battery 11 on the chassis of an automotive vehicle. Regardless of the standardized dimensions of the battery 11 , the hold-down device 10 comprises a standard support tray 12 of substantially rectangular overall shape, capable of receiving all types of batteries, and a locking ramp 26 serving to lock the position of the battery 11 in its support tray 12 .
The hold-down device 10 according to the invention therefore makes it possible, on the one hand, to immobilize the battery 11 in its support tray 12 , and, on the other hand, to lock the position of the battery 11 . The hold-down device 10 shifts from a first, locking position ( FIGS. 2 and 3 ), in which the battery 11 is solidly fixed, to a second, unlocking position ( FIGS. 11 to 14 and 18 - 19 ), in which the battery 11 can be removed.
In FIGS. 4 to 7 , the support tray 12 of the battery 11 comprises a substantially planar resting surface 16 on which the battery 11 rests after being installed, two longitudinal flanges 17 a , 17 b and two transverse flanges 18 a , 18 b . The support tray 12 is preferably designed with a material that will make it possible to withstand various types of chemical attack, particularly by agents found in the body of the battery 12 .
In FIG. 5 , three fastener holes 19 have been pierced through the resting surface 16 of the support tray 12 in order to fasten the hold-down device 10 to the chassis of the vehicle or any other specific support.
The first longitudinal flange 17 a preferably comprises three fixed lugs 20 projecting from said longitudinal flange 17 a toward the inside of the support tray 12 and designed to cooperate with the first lug 14 a of the battery 11 ( FIG. 3 ). The fixed lugs 20 are of one piece with the support tray 12 and are configured to the longitudinal flange 17 a , such that they cooperate with the corresponding shape of lug 14 a of the battery 11 . The fixed lugs 20 are preferably positioned in a median section of longitudinal flange 17 a , particularly so that they can be used regardless of the size of the battery 11 ( FIGS. 5 to 7 ).
The support tray 12 preferably comprises three movable lugs 21 capable of shifting between a first, idle position, in which the support tray 12 and the movable lugs 21 await the positioning of the battery 11 ( FIGS. 4 to 7 and 11 ), and a second, immobilizing position, in which the second lug 14 b of the battery 11 is completely immobilized by the movable lugs 21 ( FIGS. 2 , 3 and 15 to 17 ).
Each movable lug 21 is configured to cooperate with the corresponding shape of the second lug 14 b of the battery 11 ( FIG. 3 ). Each movable lug 21 comprises two reinforcing ribs 22 ( FIG. 6 ), defining a first immobilizing surface for lug 14 b of the battery 11 ( FIG. 3 ). The two ribs 22 reinforce the mechanical strength of the movable lugs 21 ( FIGS. 5 and 6 ) and constitute an inclined ramp facilitating the sliding of lug 14 b during the installation and removal of the battery 11 .
The respective positions of the movable lugs 21 on longitudinal flange 17 b are advantageously offset from the respective positions of the fixed lugs 20 on longitudinal flange 17 a ( FIG. 5 ). This configuration enables the support tray 12 to adapt to all sizes of battery 11 and makes it possible to optimize the immobilization of the battery 11 .
In FIGS. 5 and 6 , each movable lug 21 is connected to longitudinal flange 17 b by two flexible ridges 23 forming elastic hinges that are capable of deforming during the installation of the battery 11 in and its removal from the support tray 12 . The flexible ridges 23 have substantially S-shaped sections and deform elastically to act as springs. The flexible ridges 23 absorb the longitudinal stresses generated by the installation of the battery 11 , so that the movable lugs 21 can travel parallel to the resting surface 16 of the support tray 12 , in the direction of longitudinal flange 17 b.
In addition, as depicted in FIG. 4 , each movable lug 21 is connected solely to the corresponding longitudinal flange 17 b and not to the resting surface 16 of the support tray 12 , to allow the movable lugs 21 to draw back longitudinally in the direction of longitudinal flange 17 b . Each movable lug 21 thus delimits an empty space 24 extending between the resting surface 16 of the support tray 12 and the respective bottom ends of the reinforcing ribs 22 defining the first immobilizing surface of the movable lug 21 . This empty space 24 particularly constitutes a compensating play that is necessary for the movements of the lug 14 b and the battery 11 , to make up for the size differences between standard batteries 11 .
In FIGS. 4 , 6 and 7 , longitudinal flange 17 b of the support tray 12 is preferably prolonged by three actuating levers 25 extending substantially perpendicularly to the resting surface 16 of the support tray 12 and at the level of the movable lugs 21 . The levers 25 form a single piece with the support tray 12 and act as locking/unlocking levers designed to cooperate with the movable lugs 21 and the locking ramp 26 ( FIGS. 2 and 3 ) to lock the position of the battery 11 in the support tray 12 .
For this purpose, each actuating lever 25 is elastically deformable and is rotationally mounted on longitudinal flange 17 b , at the level of each movable lug 21 , by means of hinge elements 27 formed, for example, by a narrowing of material in the thickness of the levers 25 ( FIGS. 4 and 7 ). The hinge elements 27 enable the actuating levers 25 to move rotationally with respect to their lower portion connecting them to longitudinal flange 17 b , between a locking position of the hold-down of the battery 11 in the support tray 12 ( FIGS. 2 and 3 ) and an unlocking position of the hold-down of the battery 11 ( FIGS. 4 to 7 ). By way of example, the hinge elements 27 are elements of rectangular section designed to withstand a high tensile load.
The actuating levers 25 are advantageously connected in their respective upper portions by a bar 31 serving as a grasping member that facilitates the simultaneous manipulation of the actuating levers 25 ( FIGS. 6 and 7 ). Locking is thereby facilitated and made more reliable.
In FIGS. 8 to 10 , the locking ramp 26 of the hold-down device 10 according to the invention is preferably provided with three locking wedges 29 designed to cooperate with the movable lugs 21 and the corresponding actuating levers 25 to immobilize and lock the position of the battery 11 in its support tray 12 .
Each actuating lever 25 comprises an opening 28 delimited by the hinge elements 27 and designed to cooperate with a locking wedge 29 of the ramp 26 . Each opening 28 is provided with a beveled edge 30 projecting toward the inside of the opening 28 and designed to cooperate with the locking wedge 29 , as described below.
In FIGS. 5 and 6 , the support tray 2 also comprises guide grooves 32 formed so as to project from longitudinal flange 17 b in the direction of the corresponding movable lug 21 and in prolongation of the opening 28 in each actuating lever 25 . The grooves 32 cooperate with each locking wedge 29 of the ramp 26 ( FIGS. 2 and 3 ) to center the locking wedges 29 in their descending movement.
In FIGS. 8 to 10 , the locking ramp 26 comprises three locking wedges 29 , each cooperating with the opening 28 in a respective actuating lever 25 and a corresponding movable lug 21 of longitudinal flange 17 b . Each locking wedge 29 interposes itself between a second immobilizing surface 33 of the associated movable lug 21 ( FIGS. 3 and 5 ) and longitudinal flange 17 b of the support tray 12 .
Each locking wedge 29 comprises two centering ribs 34 defining a first, lower inclined surface ( FIG. 10 ). The centering ribs 34 of each locking wedge 29 position themselves and slide on one and the other side of the second immobilizing surface 33 of the corresponding movable lug 21 during the placement of the locking ramp 26 . The ribs 34 thus serve to optimize and improve the placement of the locking ramp 26 .
As illustrated in FIG. 3 , the first, lower face 34 of each locking wedge 29 bears against the second immobilizing surface 33 of each associated movable lug 21 , and the first immobilizing surface 22 of each movable lug 21 thus exerts a very strong pressure on lug 14 b of the battery 11 .
Each locking wedge 29 also has a second, upper inclined surface 35 , cooperating with the opening 28 in the corresponding actuating lever 25 ( FIGS. 2 and 3 ).
The upper inclined surface 35 of each locking wedge 29 is provided with a series of notches 36 designed to cooperate with the beveled edge 30 of the opening 28 in the corresponding actuating lever 25 . The notches 36 have a slight inclination ( FIG. 10 ), to ensure positive locking of the actuating lever 25 to the associated locking wedge 29 and to prevent inadvertent disengagement of the lever 25 . The notches 36 also make it possible to compensate for dimensional differences in the batteries 11 by offering different positioning options for the actuating levers 25 .
The locking wedges 29 pass through the openings 28 in the actuating levers 25 during the locking of the hold-down of the battery 11 in the support tray 12 . The beveled edges 30 of the openings 28 accordingly place themselves in one of the notches 36 in the upper surfaces 35 of the locking wedges 29 , depending on the size of the battery 11 .
In addition, the locking wedges 29 of the ramp 26 are advantageously connected by connection zones 37 of substantially rectangular section, which are sufficiently rigid to be manipulated by hand. Connection zones 37 have a high mechanical strength, since the loads applied by the user are exerted primarily on said connection zones 37 .
Each locking wedge 29 also comprises positioning ribs 38 cooperating with the guide grooves 32 formed against longitudinal flange 17 b . The positioning ribs 38 of the locking wedges 29 and the guide grooves 32 of second longitudinal flange 17 b serve in particular to optimize the positioning of the locking ramp 26 . This results in optimum centering of the locking wedges 29 between movable lugs 21 and longitudinal flange 17 b.
The installation of the battery 11 in the support tray 12 of the hold-down device 10 according to the invention, the locking of its position and the removal of the battery 11 will be described in more detail with regard to FIGS. 11 to 19 .
In FIG. 11 , the battery 11 is put in place in the support tray 12 by first lodging the first lug 14 a in abutment under the fixed lugs 20 of the support tray 12 . The battery 11 thus is inclined in abutment against the fixed lugs 20 and in bearing relation on the movable lugs 21 of the support tray 12 .
In FIGS. 12 and 13 , a pressure exerted by the battery 11 according to arrow F 3 causes the first lug 14 a of the battery 11 to slide over the resting surface 16 of the support tray 12 , according to arrow F 4 , toward the respective roots of the fixed lugs 20 . The second lug 14 b of the battery 11 slides along the respective first surfaces 22 of the movable lugs 21 , causing said movable lugs 21 to draw back according to arrow F 5 ( FIG. 13 ). The movable lugs 21 shift backward in parallel with the resting surface 16 of the support tray 12 .
In FIG. 14 , the battery 11 is positioned on the resting surface 16 of the support tray 12 . The movable lugs 21 have returned to their idle position, according to arrow F 6 , by virtue of the elastic return effect generated by the flexible ridges 23 of the movable lugs 21 . The lugs 14 a and 14 b of the battery 11 are then immobilized, respectively by the fixed lugs 20 and the first immobilizing surfaces 22 of the movable lugs 21 . A small empty space 39 is still present between the second lug 14 b of the battery 11 and the resting surface 16 of the support tray 12 , since the clamping action generated by the movable lugs 21 is not maximal.
In the position illustrated in FIG. 14 , the first phase of installing the battery 11 in the support tray 12 has been completed. It is now necessary to lock this position by means of the locking ramp 26 , to prevent any inadvertent disassembly of the battery from the support tray 12 .
In FIG. 15 , the locking ramp 26 is put in place between the movable lugs 21 and the actuating levers 25 , according to arrow F 7 , by sliding the centering ribs 34 of each locking wedge 29 along the second immobilizing surface 33 of the movable lugs 21 and sliding the positioning ribs 38 along the guide grooves 32 of the second longitudinal flange 17 b . The actuating levers 25 thus pivot slightly according to arrow F 8 during the insertion of the locking ramp 26 . The positioning of the locking wedges 29 also causes the battery 11 to be applied flatly to the resting surface 16 of the support tray 12 and eliminates the residual empty space 39 described above. This results in complete and maximal immobilization of the battery 11 in the support tray 12 .
In FIG. 16 , the phase of locking the position of the battery 11 in the support tray 12 is carried out by simultaneously applying pressure to the locking ramp 26 according to arrow F 9 and by rotating the actuating levers 25 , according to arrow F 10 , toward the inside of the support tray 12 above the locking ramp 26 . The locking wedges 29 of the ramp 26 then pass through the openings 28 in the actuating levers 25 , which position themselves at the level of the respective upper surfaces 35 of the locking wedges 29 . This step represents a coarse adjustment of the locking of the position of the battery 11 in its support tray 12 . In addition, the clamping action caused by the actuating levers 25 forces the locking ramp 26 to tighten the movable lugs 21 still further by making the locking wedges 29 descend slightly.
In FIG. 17 , the locking phase is completed by applying a substantially horizontal thrust, according to arrow F 11 , to the actuating levers 25 so as to place them in a notch 36 in one of the upper surfaces 35 of the locking wedges 29 that corresponds to the maximum position attainable by the actuating levers 25 . The lock is then positive and prevents inadvertent disengagement of the levers 25 . This phase represents a fine adjustment of the locking of the position of the battery 11 in its support tray 12 .
In FIG. 18 , the unlocking of the battery 11 is performed simply by actuating the levers 25 in the opposite direction to that of arrows F 10 and F 11 in FIGS. 16 and 17 . The slight inclination of the notches 36 in the upper surfaces 35 of the locking wedges 29 makes it possible to disengage the levers 25 . The locking ramp 26 is then released from the lock produced by the actuating levers 25 . All that remains is to remove the locking ramp 26 according to arrow F 12 .
In FIG. 19 , the removal of the battery 11 from its support tray 12 then consists in lifting it according to arrow F 13 while pivoting it around the fixed lugs 20 of the support tray 12 . The movable lugs 21 thereupon draw back according to arrow F 5 , enabling the second lug 14 b of the battery 11 to disengage from the movable lugs 21 . The battery 11 is then removed from the support tray 12 .
Such a hold-down device 10 for a battery 11 , permitting easy installation and removal, as described above, is therefore simple and inexpensive and features reduced weight and space consumption. It serves simultaneously to immobilize and lock the position of the battery 11 in its support tray 12 in an effective and reliable manner.
The hold-down device 10 has only one moving part in addition to the support tray 12 , namely the locking ramp 26 , for holding down and locking the battery 11 . The notched upper surfaces 35 of the locking wedges 29 permit effective positive locking of the actuating levers 25 .
In addition, the actuating levers 25 are connected to one another for better gripping and faster and more reliable manipulation. The locking and unlocking of the battery 11 are simple and quick and are performed without tools.
The invention is not limited to the various embodiments described hereinabove. In FIGS. 2 to 19 , the hold-down device 10 comprises three fixed lugs 20 and three movable lugs 21 , so that it is able to hold down all standard battery sizes. Obviously, the device 10 can have a different number of movable lugs 21 and fixed lugs 20 , as long as the number of movable lugs 21 is equal to the number of locking wedges 29 of the locking ramp 26 , which in turn is equal to the number of actuating levers 25 of the support tray 12 , to ensure optimum immobilization and locking.
While this invention has been described as having a preferred design, the present invention can be further modified within the spirit and scope of this disclosure. This application is therefore intended to cover any variations, uses, or adaptations of the invention using its general principles. Further, this application is intended to cover such departures from the present disclosure as come within known or customary practice in the art to which this invention pertains and which fall within the limits of the appended claims.
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The invention relates to a device ( 10 ) for fixing a battery ( 11 ), consisting of a support tray ( 12 ) comprising an essentially-flat support face ( 16 ) and two longitudinal flanges ( 17 a, 17 b ). According to the invention, the first longitudinal flange ( 17 a ) comprises fixed lugs ( 20 ) which serve as positioning stops for a first lug ( 14 a ) of the battery ( 11 ). The support tray ( 12 ) comprises mobile lugs ( 21 ) which are connected to the second longitudinal flange ( 17 b ) and which each define a first blocking surface ( 22 ) for a second lug ( 14 b ) of the battery ( 11 ). The fixing device ( 10 ) comprises elastically-deformable actuation levers ( 25 ) which are associated with the mobile lugs ( 21 ) and a locking ramp ( 26 ) which co-operates with each mobile lug ( 21 ) and each corresponding actuation lever ( 25 ) such as to lock the battery ( 11 ) in position in the support tray ( 12 ).
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This is a division of copending application Ser. No. 07/793,961, filed on Nov. 18, 1991, now U.S. Pat. No. 5,334,521.
FIELD OF THE INVENTION
This invention relates to a DNA sequence encoding a novel effector enzyme referred to as a cardiac adenylyl cyclase, This invention also relates to the amino acid sequence of the cardiac adenylyl cyclase encoded by that DNA sequence.
BACKGROUND OF THE INVENTION
The signal transduction pathway may be subdivided into three steps. The first is the recognition of the ligand by the receptor. The second is the transmission and amplification of the signal by a "transducer" protein. The final step is the generation of the second messenger by an effector enzyme.
Adenylyl cyclases are effector enzymes that are coupled to various hormone-receptor systems, such as catecholamine and ACTH. The catecholamine receptor and its transducer protein (G-protein) have been well characterized since the cloning of their cDNAs. However, relatively little is known about the adenylyl cyclase.
Once such a hormone binds to the receptor, it activates G protein, a heterotrimeric guanine nucleotide-binding regulatory protein (α, β, γ). The activated G-protein elicits the exchange of GDP for GTP, as well as the dissociation from βγ subunits. The GTP bound form of the α-subunit stimulates adenylyl cyclase, which generates cyclic AMP from ATP. Cyclic AMP, a second messenger, activates various proteins, including protein kinases.
Protein kinases then phosphorylate other proteins, thus initiating a signal transduction cascade. Another type of activation is through the increased intracellular calcium concentration, especially in nervous tissues. After depolarization, the influx of calcium elicits the activation of calmodulin, an intracellular calcium binding protein. The activated calmodulin has been shown to bind and activate an adenylyl cyclase directly (Bibliography 1).
Several papers have suggested the diversity of the adenylyl cyclases. Using forskolin-bound affinity chromatography, a single class of the enzyme protein was purified from bovine brain (2,3). The monoclonal antibody raised against this purified protein also recognized another form of protein in the brain, which was different in size. Biochemical characteristics have shown that these two are different types of adenylyl cyclase; one is calmoduline-sensitive (CaM-sensitive) and the other is CaM-insensitive. This study (2) showed that there are two types of adenylyl cyclase in one tissue, and that these types share the same domain that could be recognized by the same antibody.
Another paper has presented genetic evidence of the diversity of adenylyl cyclase (4). An X-linked recessive mutation in Drosophilla which blocked associative learning lacked the CaM-sensitivity of adenylyl cyclase, but did possess the reactivity to fluoride or GTP. This suggests that the CaM-sensitive cyclase gene is located in the X-chromosome, which is distinct from the CaM-insensitive adenylyl cyclase gene.
Three different cDNAs have been cloned from mammalian tissues so far. These have been designated type I (brain type (5)); II (lung type (6)); and III (olfactory type (7)). The cDNA sequences of Types I and III have been published. The adenylyl cyclases coded for by these cDNAs are large proteins more than 1000 amino acids in length. Topographically, all types are similar. All have two six-transmembrane domains associated with a large cytoplasmic loop. The amino acid sequence of the cytoplasmic loop is conserved among different types of cyclase.
Tissue distribution of these adenylyl cyclase messages is well distinguished, as shown in Northern blotting studies. Type I is expressed only in the brain, type II is distributed in lung and brain, and type III is expressed mostly in the olfactory tissue with little expression in the brain. Thus, the adenylyl cyclases are distributed in a rather tissue specific manner. Despite the fact that heart tissue was one of the tissues in which adenylyl cyclase was originally identified, none of the three known types has been shown to be expressed in heart tissue.
It has been documented that a form of adenylyl cyclase is also present in the heart (8), and that the cyclase from the heart is recognized by a monoclonal antibody originally raised against the cyclase from the brain (9). Given that the three cloned types of adenylyl cyclase have a conserved amino acid sequence in their large cytoplasmic loop, the cyclase from the heart may share sequence homology in this region. Thus, it is possible to attempt to obtain an adenylyl cyclase clone from the heart by using an adenylyl cyclase cDNA from the brain. However, no adenylyl cyclase has been reported to have been cloned from cardiac tissue or expressed.
SUMMARY OF THE INVENTION
The starting point of this invention is the hypothesis that any adenylyl cyclase in the heart should share significant homology with that from the brain, and that it could be screened using a probe from the cyclase of the brain. The adenylyl cyclase in the heart has been shown to be related with the development of heart failure (10). This suggests it is involved with cardiac function.
According to this invention, a novel type of adenylyl cyclase cDNA is cloned from a canine heart library. This novel adenylyl cyclase is referred to as cardiac adenylyl cyclase (B form). This cardiac adenylyl cyclase is composed of 1165 amino acids. Another form (A form) of cardiac adenylyl cyclase, composed of 1019 amino acids, is the subject of co-pending, commonly-assigned application Ser. No. 07/751,460, filed Aug. 29, 1991.
This B form of cardiac adenylyl cyclase is expressed predominantly in the heart, as well as in the brain, but to a lesser degree in other tissues.
The B form of cyclase is translated from the cDNA in a transient expression system using CMT cells. CMT is a monkey kidney cell line stably transformed with a T-antigen gene driven by the metallothionein promoter. This cyclase is stimulated by forskolin, which is known to stimulate adenylyl cyclase activity in the heart (10).
The structure of this B form of cardiac adenylyl cyclase is similar to those of other types of adenylyl cyclase. It contains the motif of 6-transmembrane spanning regions associated with a large cytoplasmic loop. The overall homology of the amino acid sequences of the A and B forms of cardiac adenylyl cyclases is 64%. Their amino acid sequences are more homologous in the cytoplasmic portions than in the transmembrane portions. The B form of cardiac adenylyl cyclase may be involved in the regulation of cardiac function. Unless otherwise stated, the balance of this application is directed to the B form of cyclase; the A form is described in the co-pending application referred to above.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 depicts a partial restriction map and the cDNA clone of the cardiac adenylyl cyclase (B form).
Panel A depicts a partial restriction map of adenylyl cyclase cDNA. The coding portion is boxed and a hatched box shows the polyadenylation site. N stands for NarI restriction site, S for SphI, SS for SspI and P for PstI; ATG, a translation initiation codon, and TAG, a translation termination codon are shown.
Panel B depicts two cDNA clones, numbered 6 and 27, obtained from the canine heart λgt 10 library.
FIG. 2 depicts the DNA and predicted amino acid sequence of the cardiac adenylyl cyclase. The entire coding sequence, as well as portions of the 5' and 3' untranslated sequences, are shown. The whole sequence is done bidirectionally twice by dideoxy sequencing method using either Sequanase or Taq polymerase. An arrow shows the possible translation initiation site (ATG) in an open reading frame. This ATG is accompanied by the most conserved Kozak consensus sequence.
FIG. 3 depicts a hydropathy plot of the cardiac adenylyl cyclase. MacVector 3.5 software is used to analyze the membrane related structure of cardiac adenylyl cyclase. The method of Kyte and Doolittle (11) is used with a window size of 7.
FIG. 4 depicts a DNA dot matrix comparison between the A and B forms of cardiac adenylyl cyclase. MacVector 3.0 software is used for the analysis with a stringency of 65% and a window size of 8.
FIG. 5 depicts Northern blot analysis of various canine tissues by a fragment from cardiac adenylyl cyclase cDNA. The lanes are as follows: H-heart, B-brain, T-testis, S-skeletal muscle, K-kidney, L-lung. Standards in kilobases (kb) are at the left of the blot.
DETAILED DESCRIPTION OF THE INVENTION
The strategy used to identify and isolate the novel cardiac adenylyl cyclase begins with the construction and screening of canine heart cDNA library.
Left ventricular tissue of canine heart is used as a source of mRNA. The library is prepared in a λgt10 phage with an oligo-dT primer as described (12). The primary screening of the λgt10 library is carried out with gentle washing (less stringent conditions). Approximately 2×10 6 plaques are initially screened from the library. Prehybridization is carried out for at least two hours in a solution containing 30% formamide, 5×SSC, 5×Denhardt's, 25 mM NaPO 4 (pH 6.5), 0.25 mg/ml calf thymus DNA, and 0.1% sodium dodecyl sulfate (SDS) at 42° C. Hybridization is then performed in the same solution at 42° C. An 970 base pair (bp) AatI-HincII fragment from type I adenylyl cyclase cDNA is used as a probe. This fragment encodes the first cytoplasmic domain of the adenylyl cyclase, which has significant homology to other previously-known types of adenylyl cyclase (7).
The probe is radiolabelled with 32 P-dCTP by the multi-primer-random labelling method. After hybridization for 18 hours, the blot is washed under increasingly stringent conditions and then radioautographed. One positive clone is obtained. The size of the insert in the clone is 5.4 kb (kilobases).
The next step is to ascertain the full length cDNA sequence from the inserts in the clones. All the positive clones from the canine heart library are subcloned into plasmid pUC18. After restriction maps are made, they are further subcloned and sequenced with universal primers or synthesized oligomers. For some fragments, sequencing is performed after a series of deletions is made by exonuclease III digestion. The sequence is performed bidirectionally at least twice with either Sequenase (13) or by Tag polymerase (14). In some GC-rich areas, the sequence is performed using a gel containing 7% polyacrylamide, 8M urea, and 20% formamide.
A clone designated #27 is found to be of particular interest. After the entire coding portion of clone #27 is sequenced, it is found that it contains an insert of 5.4 kb with a polyadenylation signal at its 3' end (FIG. 1). However, it does not contain an ATG with a conserved Kozak consensus sequence, which provides a favorable context for initiating translation (15).
A 5' EcoRI-SphI fragment from clone #27 is therefore used as a probe to rescreen the library. Several clones are obtained. It is found that a clone designated #6 overlaps for 800 bases with clone #27, and extends the cDNA sequence upstream an additional 441 bp. After sequencing the whole insert, an ATG with conserved Kozak consensus sequence is found at its 5' end (arrow, FIG. 1). This open reading frame of 3495 bases reads through to a TAG, a translation termination codon (FIGS. 1 and 2). Thus, clones #27 and #6 encode a protein of 1165 amino acids, which is 147 amino acids longer than the A form of cardiac adenylyl cyclase. The entire coding portion of the cDNA and its predicted amino acid sequence are shown (FIG. 2) (SEQ ID NO: 1).
A 4.0 kb EcoRI-SspI fragment from clones #6 (EcoRI-SphI) and #27 (SphI-SSpI) is subcloned into pcDNAamp (formed by introducing an ampicillin resistance gene into pcDNAl, obtained from Invitrogen). The resulting expression vector, containing the full length cDNA, is designated pcDNAamp/27-6. Samples of this expression vector, inserted into an appropriate E. coli strain designated DH5alpha, have been deposited with the American Type Culture Collection, 12301 Parklawn Drive, Rockville, Md. 20852, in accordance with the Budapest Treaty on the International Recognition of the Deposit of Microorganisms for the Purposes of Patent Procedure and have been accorded accession number ATCC 68826.
Production of this cardiac adenylyl cyclase is achieved by the cloning and expression of the cardiac adenylyl cyclase cDNA in a suitable expression system using established recombinant DNA methods. Production of the cardiac adenylyl cyclase can be achieved by incorporation of the cardiac adenylyl cyclase cDNA into any suitable expression vector and subsequent transformation of an appropriate host cell with the vector; alternatively, the transformation of the host cell can be achieved directly by naked DNA without the use of a vector. Production of the cardiac adenylyl cyclase by either eukaryotic cells or prokaryotic cells is contemplated by the present invention. Examples of suitable eukaryotic cells include mammalian cells, plant cells, yeast cells and insect cells. Similarly, suitable prokaryotic hosts, in addition to E. coli, include Bacillus subtilis.
Other suitable expression vectors may also be employed and are selected based upon the choice of host cell. For example, numerous vectors suitable for use in transforming bacterial cells are well known. For example, plasmids and bacteriophages, such as λ phage, are the most commonly used vectors for bacterial hosts, and for E. coli in particular. In both mammalian and insect cells, virus vectors are frequently used to obtain expression of exogenous DNA. In particular, mammalian cells are commonly transformed with SV40 or polyoma virus; and insect cells in culture may be transformed with baculovirus expression vectors. Yeast vector systems include yeast centromere plasmids, yeast episomal plasmids and yeast integrating plasmids.
It will also be understood that the practice of the invention is not limited to the use of the exact sequence of the cardiac adenylyl cyclase cDNA as defined in FIG. 2 (SEQ ID NO: 1). Modifications to the sequence, such as deletions, insertions, or subst itutions in the sequence which produce silent changes in the resulting protein molecule are also contemplated. For example, alterations in the cDNA sequence which result in the production of a chemically equivalent amino acid at a given site are contemplated; thus, a codon for the amino acid alanine, a hydrophobic amino acid, can readily be substituted by a codon encodig another hydrophobic residue, such as glycine, or may be substituted with a more hydrophobic residue such as valine, leucine, or isoleucine. Similarly, changes which result in substitution of one negatively charged residue for another, such as aspartic acid for glutamic acid, or one positively charged residue for another, such as lysine for arginine, can also be expected to produce a biologically equivalent product.
Nucleotide changes which result in alteration of the N-terminal and C-terminal portions of the protein molecule frequently do not alter protein activity, as these regions are usually not involved in biological activity. It may also be desirable to eliminate one or more of the cysteines present in the sequence, as the presence of cysteines may result in the undesirable formation of multimere when the protein is produced recombinantly, thereby complicating the purification and crystallization processes.
Each of the proposed modifications is well within the routine skill in the art, as is determination or retention of biological activity of the encoded products. Therefore, where the phrase "cardiac adenylyl cyclase cDNA sequence" or "cardiac adenylyl cyclase gene" is used in either the specification or the claims, it will be understood to encompass all such modifications and variations which result in the production of a biologically equivalent cardiac adenylyl cyclase protein. It is also understood to include the corresponding sequence in other mammalian species. In particular, the invention contemplates those DNA sequences which are sufficiently duplicative of the sequence of FIG. 2 so as to permit hybridization therewith under standard high stringency Southern hybridization conditions, such a those described in Maniatis et al. (16).
In an example of such expression, twenty μg of the purified plasmid pcDNAamp/27-6 are transfected into the monkey kidney CMT cells using a modified method of Goolub et al. (17). Briefly, the cells are grown to 80% confluence in Dulbecco's modification of Eagle's Medium, 10% fetal calf serum, 2 mM glutamine, 4.5 mg/ml glucose, 10 μg/ml streptomycin sulfate and 60 μg/ml penicillin K. After washing with PBS twice, 0.5 ml of trypsin solution is added. The cells are incubated for 10 minutes, and 20 μg of purified plasmid resuspended in 4 ml of DMEM containing 400 μg/ml DEAE dextran and 0.1 mM chloroquine is added. The cell is incubated for four hours followed by 10% DMSO shock for two minutes. After washing with PBS twice, the induction media, which contains 10% fetal calf serum (FCS), 2 mM glutamine, 4.5 g/ml glucose, 2mM penicillin and streptomycin, and 1 μM CdCl 2 , 0.1 μM ZnCl 2 in DMEM, is added. The plate is incubated at 37° C. for 72 hours before harvesting.
This adenylyl cyclase protein, composed of 1165 amino acids, is analyzed for secondary structure by the method of Kyte-Doolittle (11) (FIG. 3). The software, MacVector 3.5 (IBI, New Haven, Conn.), is used to obtain a hydropathy plot and thereby identify the membrane related structure of this cardiac adenylyl cyclase. The method of Kyte and Doolittle is used with a window size of 7.
As shown in FIG. 3, twelve peaks are numbered. These peaks represent transmembrane spanning regions. These results suggest that this cardiac adenylyl cyclase possesses a structure of twelve transmembrane spanning regions, as well as a large cytoplasmic loop located in the middle and at the end. In the transmembrane positions, the fifth extracellular loop is the largest (between the ninth and tenth transmembrane spans).
One hundred and fifty amino acids of the N-terminal tail are located in the cytoplasm, followed by a 6-transmembrane spanning region of 154 amino acids (amino acid position 151-304). Then 363 amino acids of the cytoplasmic domains (305-667) precede the second 6-transmembrane spanning domain of 242 amino acids (668-909), followed by another cytoplasmic domain of 256 amino acids (910-1165). Thus it makes a duplicated form of 6-transmembrane spanning region and large hydrophobic cytoplasmic domain.
As shown in FIG. 4, a DNA dot matrix comparison between the B form and the A form of cardiac adenylyl cyclase, the two large hydrophobic cytoplasmic loops show homology of 72-80% with each other. The homology between the two transmembrane spanning portions is also high (44-45%).
Thus, these two cardiac cyclases are clearly distinct from each other, but share much higher homology than with other types of cyclases, such as type I and type III. It is therefore reasonable to categorize these cardiac adenylyl cyclases as a new subclass of the entire adenylyl cyclase family. The only distinct difference between the two cardiac cyclases is that the A form lacks an N-terminal cytoplasmic domain, while the B form possesses such a domain 150 amino acids in length.
The membrane associated secondary structure of the protein (based on the results of FIG. 3) is well conserved among different types of mammalian adenylyl cyclases (types I, II, III, and cardiac types). All of them possess two large cytoplasmic loops, interrupted by the presence of 6-transmembrane spanning region. The homology among the different types of adenylyl cyclase is only conserved in the cytoplasmic portions, even though the other portions are structurally similar. Furthermore, in the same adenylyl cyclase protein the homology between the two cytoplasmic portions is also maintained. This suggests the cytoplasmic portion is a result of gene duplication.
It has been suggested that the level of activity of the adenylyl cyclases in the heart correlates with the development of heart failure. There is a significant decrease in the cyclase activity in the failured heart compared with that in the non-failured heart (10,18,19,20). These papers suggest that there is a distal regulation in the signal transduction pathway, i.e., the regulation at the level of cyclase. In fact, the decreased activity of adenylyl cyclase in the heart may be the major factor in the development of heart failure. Thus, the novel cardiac adenylyl cyclase of this invention is used to screen for compounds which stimulate the activity of that cyclase.
The biochemical property of this cardiac adenylyl cyclase is examined in a transient expression system using CMT cells (a derivative of COS cells). CMT cells contain T-antigen driven by a methalothionein promoter in the genome. Thus by induction with heavy metal ion in the medium, CMT cells could produce more T-antigen than COS cells. A 4.0 kb fragment of the adenylyl cyclase cDNA containing the whole coding sequence is inserted into the pcDNAamp plasmid described above.
The adenylyl cyclase activity of a membrane transfected with the expression vector pcDNAamp carrying cardiac adenylyl cyclase cDNA is assayed as follows. The transfected CMT cells are washed twice with PBS and scraped in three ml of cold buffer containing 50 mM Tris (pH 8.0), 1 mM EDTA, 10 μM PMSF (pheynlmethylsulfonylfluoride), 100 U leupeptin, and 50 U egg white trypsin inhibitor (ETI) on ice. The membrane is homogenated in Polytron™ (setting 6 for 10 seconds) and is centrifuged at 800×g for 10 minutes at 4° C. The supernatant is further centrifuged at 100×g for 40 minutes at 4° C. The resultant pellet is resuspended in 50 mM Tris (pH 8.0), 1 mM EDTA, 1 μM PMSF, 50 U leupeptin, and 50 U ETI, to a concentration of 5 μg/μl. This crude membrane solution is used for the adenylyl cyclase asssay.
The adenylyl cyclase assay is performed by the method of Salomon (21). Briefly, the crude membranes from CMT cells are resuspended in a solution containing 1 mM creatine phosphate, 8 μg/ml creatine phophokinase, 4 mM HEPES (pH 8.0), 2 mM MgCl 2 , 0.1 mM c-AMP, 0.1 mM ATP, and 32 P-ATP (0.2-5 μCi/assay tube). The reaction mixture is incubated at 37° C. for 30 minutes and the reaction is stopped by the addition of 100 μl 2% sodium dauryl sulfate. To monitor the recovery from the column, 3H-labelled c-AMP is used. Cyclic-AMP is separated from ATP by passing through Dowex and alumina columns, and the radioactivity is counted by scintillation counter. The protein concentrations of the membranes used are measured by Bradford's method (22), with bovine serum albumin as a standard.
The membrane from untransfected CMT cells is used as a control. The results of the adenylyl cyclase activity assay are shown in Table 1:
TABLE 1______________________________________ Basal* NaF* GTPγS* Forskolin*______________________________________Control 4 ± 0.7 17 ± 3 30 ± 5 61 ± 11Transfected 9 ± 1 46 ± 5 114 ± 12 223 ± 27______________________________________ *control < transfected, p < 0.05, control (n = 6), transfected (n = 8)
The adenylyl cyclase expressed by this cDNA is well stimulated by 10 mM sodium fluoride, 100 μM GTPγS and 100 μM forskolin. It shows 2.7, 3.8 and 3.7 fold more stimulation than the control. Values are shown with ± standard error.
An increased basal activity of adenylyl cyclase in the transfected cells is also observed. This suggests that this cyclase possesses high basal activity, allowing high accumulation of cyclic AMP in the heart. This is consistent with the high basal cyclase activity seen in cardiac tissue.
In order to clarify the tissue distribution of the cardiac adenylyl cyclase (B form), Northern blotting is performed using mRNA from various tissues. Messenger RNA is purified using guanidium sodium (20) and oligo-dT columns from various canine tissues (heart, brain, testis, skeletal muscle, kidney and lung). Five μg of mRNA are used for each assay (per lane of blot).
The blot is prehybridized in a solution containing 50% formamide, 5×SSC, 5×Denhardt's, 25 mM NaPO 4 (pH 6.5), 0.25 mg/ml calf thymus DNA, and 0.1% SDS at 42° C. for two hours before the addition of a probe. The entire 5.4 kb CDNA fragment from the adenylyl cyclase cDNA clone #27 is used as a probe. The probe is made by a multiprimer random labelling method with 32 P-dCTP. Hybridization is performed at 42° C. for 18 hours followed by washing under increasingly stringent conditions. The blot is then autoradiographed.
The results of the Northern blot analysis, as depicted in FIG. 5, show that the message is most abundant in the heart, as well as in the brain, but much less expressed in other tissues, such as testis, skeletal muscle, kidney and lung.
The single class of message which hybridizes with a fragment from clone #27 is 6 kb in size, clearly distinct from the messages (5 and 7 kb) with clone #113 which contains the cDNA for the A form of the cyclase.
BIBLIOGRAPHY
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__________________________________________________________________________SEQUENCE LISTING(1) GENERAL INFORMATION:(iii) NUMBER OF SEQUENCES: 2(2) INFORMATION FOR SEQ ID NO:1:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 4046 base pairs(B) TYPE: nucleic acid(C) STRANDEDNESS: single(D) TOPOLOGY: linear(ii) MOLECULE TYPE: DNA (genomic)(ix) FEATURE:(A) NAME/KEY: CDS(B) LOCATION: 131..3625(xi) SEQUENCE DESCRIPTION: SEQ ID NO:1:CGGCCGGGCGGGCTGCGGGCGGCGAGGCTCGCCGGGGCGCGGGCGGCGGGGGGCGCGGGG60CGGCCGGCCGGGCCGGAGCCCGGGGGGCGGCGGGGCGGGGTCCGGGGCGGCGCGGAGCGG120GGCCGGCAGCATGTCGTGGTTTAGTGGCCTCCTGGTCCCCAAAGTGGAT169MetSerTrpPheSerGlyLeuLeuValProLysValAsp1510GAACGGAAGACAGCCTGGGGTGAACGCAATGGGCAGAAGCGTCCACGC217GluArgLysThrAlaTrpGlyGluArgAsnGlyGlnLysArgProArg152025CGCGGGACTCGGACCAGTGGCTTCTGCACGCCCCGCTATATGAGCTGC265ArgGlyThrArgThrSerGlyPheCysThrProArgTyrMetSerCys30354045CTCCGGGATGCGCAGCCCCCCAGTCCCACCCCTGCGGCTCCCCCTCGG313LeuArgAspAlaGlnProProSerProThrProAlaAlaProProArg505560TGCCCCTGGCAGGATGAGGCCTTCATCCGGAGAGGCGGCCCGGGCAAG361CysProTrpGlnAspGluAlaPheIleArgArgGlyGlyProGlyLys657075GGCACGGAGCTGGGGCTGCGGGCGGTGGCCCTGGGCTTCGAGGACACT409GlyThrGluLeuGlyLeuArgAlaValAlaLeuGlyPheGluAspThr808590GAGGCCATGTCAGCGGTTGGGGCAGCTGGAGGTGGCCCTGACGTGACC457GluAlaMetSerAlaValGlyAlaAlaGlyGlyGlyProAspValThr95100105CCCGGGAGTAGGCGATCCTGCTGGCGCCGTCTGGCCCAGGTGTTCCAG505ProGlySerArgArgSerCysTrpArgArgLeuAlaGlnValPheGln110115120125TCGAAGCAGTTCCGCTCGGCCAAGCTGGAGCGCCTGTACCAGCGGTAC553SerLysGlnPheArgSerAlaLysLeuGluArgLeuTyrGlnArgTyr130135140TTCTTTCAGATGAACCAGAGCAGCCTGACGCTGCTGATGGCGGTGCTG601PhePheGlnMetAsnGlnSerSerLeuThrLeuLeuMetAlaValLeu145150155GTGCTGCTGACAGCGGTGCTGCTAGCCTTCCATGCTGCACCTGCCCGC649ValLeuLeuThrAlaValLeuLeuAlaPheHisAlaAlaProAlaArg160165170CCTCAGCCTGCCTACGTGGCCCTGCTGGCCTGTGCCGCCACCCTCTTC697ProGlnProAlaTyrValAlaLeuLeuAlaCysAlaAlaThrLeuPhe175180185GTGGCGCTCATGGTGGTGTGTAACCGGCACAGCTTTCGCCAGGACTCC745ValAlaLeuMetValValCysAsnArgHisSerPheArgGlnAspSer190195200205ATGTGGGTGGTGAGCTACGTGGTGCTGGGCATCCTGGCAGCCGTTCAG793MetTrpValValSerTyrValValLeuGlyIleLeuAlaAlaValGln210215220GTTGGGGGTGCCCTGGCAGCCAACCCCCGCAGCCCCTCTGTGGGCCTC841ValGlyGlyAlaLeuAlaAlaAsnProArgSerProSerValGlyLeu225230235TGGTGCCCTGTGTTTTTTGTCTACATCACCTACACGCTCCTACCCATC889TrpCysProValPhePheValTyrIleThrTyrThrLeuLeuProIle240245250CGCATGCGGGCAGCTGTCTTCAGTGGCCTGGGCCTGTCCACCCTGCAT937ArgMetArgAlaAlaValPheSerGlyLeuGlyLeuSerThrLeuHis255260265TTGATCTTGGCCTGGCAACTCAACCGCGGTGACGCCTTCCTCTGGAAG985LeuIleLeuAlaTrpGlnLeuAsnArgGlyAspAlaPheLeuTrpLys270275280285CAGCTCGGTGCCAACATGCTGCTGTTCCTCTGCACCAACGTCATTGGC1033GlnLeuGlyAlaAsnMetLeuLeuPheLeuCysThrAsnValIleGly290295300ATCTGCACACACTACCCAGCTGAGGTCTCTCAGCGCCAGGCCTTTCAG1081IleCysThrHisTyrProAlaGluValSerGlnArgGlnAlaPheGln305310315GAGACCCGCGGTTACATTCAGGCCCGGCTGCACCTGCCAGATGAGAAC1129GluThrArgGlyTyrIleGlnAlaArgLeuHisLeuProAspGluAsn320325330CGGCAGCAGGAACGGCTGCTGCTGTCCGTGTTGCCCCAGCATGTTGCC1177ArgGlnGlnGluArgLeuLeuLeuSerValLeuProGlnHisValAla335340345ATGGAGATGAAAGAAGATATCAACACAAAGAAAGAAGACATGATGTTC1225MetGluMetLysGluAspIleAsnThrLysLysGluAspMetMetPhe350355360365CACAAGATCTACATCCAGAAGCATGACAATGTCAGCATCCTGTTTGCA1273HisLysIleTyrIleGlnLysHisAspAsnValSerIleLeuPheAla370375380GACATTGAAGGCTTCACCAGCCTGGCGTCCCAGTGCACCGCGCAGGAG1321AspIleGluGlyPheThrSerLeuAlaSerGlnCysThrAlaGlnGlu385390395CTGGTCATGACCCTGAACGAGCTCTTCGCCCGGTTTGACAAGCTGGCT1369LeuValMetThrLeuAsnGluLeuPheAlaArgPheAspLysLeuAla400405410GCGGAAAATCACTGCCTGAGGATCAAGATCTTAGGGGACTGTTACTAC1417AlaGluAsnHisCysLeuArgIleLysIleLeuGlyAspCysTyrTyr415420425TGTGTGTCGGGGCTGCCGGAGGCCCGGGCAGACCATGCCCACTGGTGT1465CysValSerGlyLeuProGluAlaArgAlaAspHisAlaHisTrpCys430435440445GTGGAGATGGGGGTGGACATGATCGAGGCCATCTCGCTGGTGCGTGAG1513ValGluMetGlyValAspMetIleGluAlaIleSerLeuValArgGlu450455460GTGACAGGTGTGAACGTGAACATCCGCGTGGGCATCCACAGCGGGCGT1561ValThrGlyValAsnValAsnIleArgValGlyIleHisSerGlyArg465470475GTGCACTGTGGTGTCCTTGGCCTGCGGAAATGGCAGTTCGACGTGTGG1609ValHisCysGlyValLeuGlyLeuArgLysTrpGlnPheAspValTrp480485490TCCAATGACGTGACTCTGGCCAACCATATGGAGGCGGCCCGGGCCGGC1657SerAsnAspValThrLeuAlaAsnHisMetGluAlaAlaArgAlaGly495500505CGCATCCACATCACCCGGGCCACGCTGCAGTACCTGAACGGGGACTAC1705ArgIleHisIleThrArgAlaThrLeuGlnTyrLeuAsnGlyAspTyr510515520525GAGGTGGAGCCGGGCCGCGGTGGCGAGCGGAACGCGTACCTCAAGGAG1753GluValGluProGlyArgGlyGlyGluArgAsnAlaTyrLeuLysGlu530535540CAGCACATCGAGACCTTCCTCATCCTGGGAGCCAGCCAGAAACGGAAA1801GlnHisIleGluThrPheLeuIleLeuGlyAlaSerGlnLysArgLys545550555GAGGAGAAGGCCATGCTGGCCAAGCTGCAGCGGACGCGGGCCAACTCC1849GluGluLysAlaMetLeuAlaLysLeuGlnArgThrArgAlaAsnSer560565570ATGGAAGGCCTGATGCCACGCTGGGTGGCCGACCGCGCCTTCTTCCGG1897MetGluGlyLeuMetProArgTrpValAlaAspArgAlaPhePheArg575580585ACCAAGGACTCCAAGGCTTTCCGCCAGATGGGCATTGATGATTCCAGC1945ThrLysAspSerLysAlaPheArgGlnMetGlyIleAspAspSerSer590595600605AAAGACAACCGGGGTGCCCAAGATGCCCTGAACCCCGAGGATGAGGTC1993LysAspAsnArgGlyAlaGlnAspAlaLeuAsnProGluAspGluVal610615620GATGAGTTCCTGGGCCGTGGCATCGATGCCCGCAGCATCGATCAGCTA2041AspGluPheLeuGlyArgGlyIleAspAlaArgSerIleAspGlnLeu625630635CGGAAGGACCATGTGCGCCGCTTCCTGCTCACCTTCCAGAGAGAGGAT2089ArgLysAspHisValArgArgPheLeuLeuThrPheGlnArgGluAsp640645650CTTGAAAAGAAGTACTCAAGGAAGGTGGACCCCCGCTTCGGAGCCTAC2137LeuGluLysLysTyrSerArgLysValAspProArgPheGlyAlaTyr655660665GTGGCCTGTGCGCTGTTGGTCTTCTGCTTCATCTGCTTTATCCAGCTC2185ValAlaCysAlaLeuLeuValPheCysPheIleCysPheIleGlnLeu670675680685CTCGTCTTCCCACACTCAACCGTGATGCTTGGGATCTACGCCAGTATC2233LeuValPheProHisSerThrValMetLeuGlyIleTyrAlaSerIle690695700TTTGTGCTGTTGCTGATCACCGTGCTGACCTGTGCCGTGTACTCCTGT2281PheValLeuLeuLeuIleThrValLeuThrCysAlaValTyrSerCys705710715GGCTCTCTCTTCCCCAAGGCCCTGCGACGTCTTTCCCGCAGCATCGTC2329GlySerLeuPheProLysAlaLeuArgArgLeuSerArgSerIleVal720725730CGCTCTCGGGCACACAGCACTGTGGTTGGCATTTTTTCAGTCTTGCTA2377ArgSerArgAlaHisSerThrValValGlyIlePheSerValLeuLeu735740745GTGTTCACCTCTGCCATCGCCAACATGTTCACCTGTAACCACACCCCC2425ValPheThrSerAlaIleAlaAsnMetPheThrCysAsnHisThrPro750755760765ATCCGGACCTGTGCAGCCCGGATGCTGAATGTAACACCCGCTGACATC2473IleArgThrCysAlaAlaArgMetLeuAsnValThrProAlaAspIle770775780ACTGCCTGCCACCTGCAGCAGCTCAATTACTCTCTGGGCCTGGATGCT2521ThrAlaCysHisLeuGlnGlnLeuAsnTyrSerLeuGlyLeuAspAla785790795CCGCTGTGTGAGGGCACCGCACCCACTTGCAGCTTCCCTGAGTACTTC2569ProLeuCysGluGlyThrAlaProThrCysSerPheProGluTyrPhe800805810GTTGGGAACATGCTGCTGAGTCTCTTGGCCAGCTCTGTTTTCCTGCAC2617ValGlyAsnMetLeuLeuSerLeuLeuAlaSerSerValPheLeuHis815820825ATCAGTAGCATCGGGAAGTTGGCCATGATCTTTGTCCTGGGGGTCATT2665IleSerSerIleGlyLysLeuAlaMetIlePheValLeuGlyValIle830835840845TATTTGGTGCTGCTTCTGCTGGGCCCCCCCAGCACCATCTTTGACAAC2713TyrLeuValLeuLeuLeuLeuGlyProProSerThrIlePheAspAsn850855860TATGACCTGCTGCTTGGTGTCCATGGCTTGGCTTCTTCCAATGACACC2761TyrAspLeuLeuLeuGlyValHisGlyLeuAlaSerSerAsnAspThr865870875TTTGATGGGCTGGACTGCCCAGCTGCGGGGAGGGTGGCACTGAAATAC2809PheAspGlyLeuAspCysProAlaAlaGlyArgValAlaLeuLysTyr880885890ATGACCCCTGTGATTCTGCTGGTGTTTGCCCTGGCGCTGTATCTGCAC2857MetThrProValIleLeuLeuValPheAlaLeuAlaLeuTyrLeuHis895900905GCCCAGCAGGTGGAATCAACTGCACGTCTGGACTTCCTCTGGAAACTG2905AlaGlnGlnValGluSerThrAlaArgLeuAspPheLeuTrpLysLeu910915920925CAGGCAACGGGGGAGAAGGAGGAGATGGAGGAGCTCCAGGCCTACAAC2953GlnAlaThrGlyGluLysGluGluMetGluGluLeuGlnAlaTyrAsn930935940CGAAGGCTGCTGCATAACATTCTGCCTAAGGACGTGGCTGCCCACTTC3001ArgArgLeuLeuHisAsnIleLeuProLysAspValAlaAlaHisPhe945950955CTGGCCCGGGAGCGCCGGAACGATGAGCTCTACTACCAGTCGTGTGAG3049LeuAlaArgGluArgArgAsnAspGluLeuTyrTyrGlnSerCysGlu960965970TGTGTGGCCGTCATGTTTGCCTCCATTGCCAACTTTTCTGAGTTCTAT3097CysValAlaValMetPheAlaSerIleAlaAsnPheSerGluPheTyr975980985GTGGAGCTGGAGGCAAACAATGAGGGTGTCGAGTGCCTGCGGCTGCTC3145ValGluLeuGluAlaAsnAsnGluGlyValGluCysLeuArgLeuLeu99099510001005AACGAAATCATCGCCGACTTTGATGAGATCATCAGCGAGGAGCGGTTC3193AsnGluIleIleAlaAspPheAspGluIleIleSerGluGluArgPhe101010151020CGGCAGCTGGAGAAAATCAAGACGATCGGTAGCACGTACATGGCTGCG3241ArgGlnLeuGluLysIleLysThrIleGlySerThrTyrMetAlaAla102510301035TCGGGGCTGAACGCCAGCACCTACGATCAGGCCGGCCGCTCCCACATC3289SerGlyLeuAsnAlaSerThrTyrAspGlnAlaGlyArgSerHisIle104010451050ACTGCCCTGGCCGACTATGCCATGCGGCTCATGGAGCAGATGAAACAC3337ThrAlaLeuAlaAspTyrAlaMetArgLeuMetGluGlnMetLysHis105510601065ATCAACGAGCACTCCTTCAACAACTTCCAGATGAAGATTGGGCTGAAC3385IleAsnGluHisSerPheAsnAsnPheGlnMetLysIleGlyLeuAsn1070107510801085ATGGGCCCAGTTGTGGCAGGCGTCATTGGGGCTCGGAAGCCACAGTAT3433MetGlyProValValAlaGlyValIleGlyAlaArgLysProGlnTyr109010951100GACATCTGGGGGAACACGGTGAATGTCTCTAGCCGTATGGACAGCACG3481AspIleTrpGlyAsnThrValAsnValSerSerArgMetAspSerThr110511101115GGGGTTCCTGACCGAATCCAGGTGACCACGGACTTGTACCAGGTTCTA3529GlyValProAspArgIleGlnValThrThrAspLeuTyrGlnValLeu112011251130GCTGCCAAACGGTACCAGCTGGAGTGTCGAGGGGTGGTCAAGGTGAAG3577AlaAlaLysArgTyrGlnLeuGluCysArgGlyValValLysValLys113511401145GGCAAGGGGGAGATGACCACCTACTTCCTCAATGGGGGCCCCCCCAGT3625GlyLysGlyGluMetThrThrTyrPheLeuAsnGlyGlyProProSer1150115511601165TAGCAGAGCCCAGCTACAAGTTCAGCTGTCAGGACCAAGGTGGGCATTTAAGTGGACTCT3685GTGCTCGCTGGATGGAGCTGTGGCCGGGGGCACCAAGCCTCCAGACCCTGCTGACCACAA3745AAGGGAACACCTCAGCAGGCTGTGCTTGGACCATGCTCGTCTGCCCTCAGGCTGGTGAAC3805AAGGGATACCAAGAGGATTATGCAAGTGACTTTTACTTTTCTAATTGGGGTAGGGCTGGC3865TGTTCCCTCTTTCTTCCTGCTTTTGGGAGCAGGGGAGGCAGCTGCAGCAGAGGCAGCAGG3925AGCCCTCCTGCCTGAGGGTTTAAAATGGCAGCTTGCCATGCCTACCCTTTCCCCTGTCTG3985TCTGGGCAACAGCATCGGGGCTGGGCCCTTCCTTTCCCTCTTTTTCCTGGGAATATTTTG4045T4046(2) INFORMATION FOR SEQ ID NO:2:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 1165 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: protein(xi) SEQUENCE DESCRIPTION: SEQ ID NO:2:MetSerTrpPheSerGlyLeuLeuValProLysValAspGluArgLys151015ThrAlaTrpGlyGluArgAsnGlyGlnLysArgProArgArgGlyThr202530ArgThrSerGlyPheCysThrProArgTyrMetSerCysLeuArgAsp354045AlaGlnProProSerProThrProAlaAlaProProArgCysProTrp505560GlnAspGluAlaPheIleArgArgGlyGlyProGlyLysGlyThrGlu65707580LeuGlyLeuArgAlaValAlaLeuGlyPheGluAspThrGluAlaMet859095SerAlaValGlyAlaAlaGlyGlyGlyProAspValThrProGlySer100105110ArgArgSerCysTrpArgArgLeuAlaGlnValPheGlnSerLysGln115120125PheArgSerAlaLysLeuGluArgLeuTyrGlnArgTyrPhePheGln130135140MetAsnGlnSerSerLeuThrLeuLeuMetAlaValLeuValLeuLeu145150155160ThrAlaValLeuLeuAlaPheHisAlaAlaProAlaArgProGlnPro165170175AlaTyrValAlaLeuLeuAlaCysAlaAlaThrLeuPheValAlaLeu180185190MetValValCysAsnArgHisSerPheArgGlnAspSerMetTrpVal195200205ValSerTyrValValLeuGlyIleLeuAlaAlaValGlnValGlyGly210215220AlaLeuAlaAlaAsnProArgSerProSerValGlyLeuTrpCysPro225230235240ValPhePheValTyrIleThrTyrThrLeuLeuProIleArgMetArg245250255AlaAlaValPheSerGlyLeuGlyLeuSerThrLeuHisLeuIleLeu260265270AlaTrpGlnLeuAsnArgGlyAspAlaPheLeuTrpLysGlnLeuGly275280285AlaAsnMetLeuLeuPheLeuCysThrAsnValIleGlyIleCysThr290295300HisTyrProAlaGluValSerGlnArgGlnAlaPheGlnGluThrArg305310315320GlyTyrIleGlnAlaArgLeuHisLeuProAspGluAsnArgGlnGln325330335GluArgLeuLeuLeuSerValLeuProGlnHisValAlaMetGluMet340345350LysGluAspIleAsnThrLysLysGluAspMetMetPheHisLysIle355360365TyrIleGlnLysHisAspAsnValSerIleLeuPheAlaAspIleGlu370375380GlyPheThrSerLeuAlaSerGlnCysThrAlaGlnGluLeuValMet385390395400ThrLeuAsnGluLeuPheAlaArgPheAspLysLeuAlaAlaGluAsn405410415HisCysLeuArgIleLysIleLeuGlyAspCysTyrTyrCysValSer420425430GlyLeuProGluAlaArgAlaAspHisAlaHisTrpCysValGluMet435440445GlyValAspMetIleGluAlaIleSerLeuValArgGluValThrGly450455460ValAsnValAsnIleArgValGlyIleHisSerGlyArgValHisCys465470475480GlyValLeuGlyLeuArgLysTrpGlnPheAspValTrpSerAsnAsp485490495ValThrLeuAlaAsnHisMetGluAlaAlaArgAlaGlyArgIleHis500505510IleThrArgAlaThrLeuGlnTyrLeuAsnGlyAspTyrGluValGlu515520525ProGlyArgGlyGlyGluArgAsnAlaTyrLeuLysGluGlnHisIle530535540GluThrPheLeuIleLeuGlyAlaSerGlnLysArgLysGluGluLys545550555560AlaMetLeuAlaLysLeuGlnArgThrArgAlaAsnSerMetGluGly565570575LeuMetProArgTrpValAlaAspArgAlaPhePheArgThrLysAsp580585590SerLysAlaPheArgGlnMetGlyIleAspAspSerSerLysAspAsn595600605ArgGlyAlaGlnAspAlaLeuAsnProGluAspGluValAspGluPhe610615620LeuGlyArgGlyIleAspAlaArgSerIleAspGlnLeuArgLysAsp625630635640HisValArgArgPheLeuLeuThrPheGlnArgGluAspLeuGluLys645650655LysTyrSerArgLysValAspProArgPheGlyAlaTyrValAlaCys660665670AlaLeuLeuValPheCysPheIleCysPheIleGlnLeuLeuValPhe675680685ProHisSerThrValMetLeuGlyIleTyrAlaSerIlePheValLeu690695700LeuLeuIleThrValLeuThrCysAlaValTyrSerCysGlySerLeu705710715720PheProLysAlaLeuArgArgLeuSerArgSerIleValArgSerArg725730735AlaHisSerThrValValGlyIlePheSerValLeuLeuValPheThr740745750SerAlaIleAlaAsnMetPheThrCysAsnHisThrProIleArgThr755760765CysAlaAlaArgMetLeuAsnValThrProAlaAspIleThrAlaCys770775780HisLeuGlnGlnLeuAsnTyrSerLeuGlyLeuAspAlaProLeuCys785790795800GluGlyThrAlaProThrCysSerPheProGluTyrPheValGlyAsn805810815MetLeuLeuSerLeuLeuAlaSerSerValPheLeuHisIleSerSer820825830IleGlyLysLeuAlaMetIlePheValLeuGlyValIleTyrLeuVal835840845LeuLeuLeuLeuGlyProProSerThrIlePheAspAsnTyrAspLeu850855860LeuLeuGlyValHisGlyLeuAlaSerSerAsnAspThrPheAspGly865870875880LeuAspCysProAlaAlaGlyArgValAlaLeuLysTyrMetThrPro885890895ValIleLeuLeuValPheAlaLeuAlaLeuTyrLeuHisAlaGlnGln900905910ValGluSerThrAlaArgLeuAspPheLeuTrpLysLeuGlnAlaThr915920925GlyGluLysGluGluMetGluGluLeuGlnAlaTyrAsnArgArgLeu930935940LeuHisAsnIleLeuProLysAspValAlaAlaHisPheLeuAlaArg945950955960GluArgArgAsnAspGluLeuTyrTyrGlnSerCysGluCysValAla965970975ValMetPheAlaSerIleAlaAsnPheSerGluPheTyrValGluLeu980985990GluAlaAsnAsnGluGlyValGluCysLeuArgLeuLeuAsnGluIle99510001005IleAlaAspPheAspGluIleIleSerGluGluArgPheArgGlnLeu101010151020GluLysIleLysThrIleGlySerThrTyrMetAlaAlaSerGlyLeu1025103010351040AsnAlaSerThrTyrAspGlnAlaGlyArgSerHisIleThrAlaLeu104510501055AlaAspTyrAlaMetArgLeuMetGluGlnMetLysHisIleAsnGlu106010651070HisSerPheAsnAsnPheGlnMetLysIleGlyLeuAsnMetGlyPro107510801085ValValAlaGlyValIleGlyAlaArgLysProGlnTyrAspIleTrp109010951100GlyAsnThrValAsnValSerSerArgMetAspSerThrGlyValPro1105111011151120AspArgIleGlnValThrThrAspLeuTyrGlnValLeuAlaAlaLys112511301135ArgTyrGlnLeuGluCysArgGlyValValLysValLysGlyLysGly114011451150GluMetThrThrTyrPheLeuAsnGlyGlyProProSer115511601165__________________________________________________________________________
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A DNA sequence encoding a novel effector enzyme referred to as a cardiac adenylyl cyclase is described. The amino acid sequence of the cardiac adenylyl cyclase encoded by that DNA sequence is also described.
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SUMMARY OF THE INVENTION
The present invention relates to geminal carboxylic acids and esters thereof of formula (I): ##STR2## wherein: R a and R b are independently hydrogen, an alkali or alkaline-earth metal cation, an ammonium or C 1 -C 10 alkylammonium cation, C 1 -C 4 alkyl, C 1 -C 10 alkoxyethyl, allyl, p-methoxybenzyl, amino-C 2 -C 4 alkyl;
Φ is a group of formula --(Y)q--(CH 2 )r in which Y is CH 2 , 0 or S;
B is a 2-propyl group; a tert-butyl group; a phenyl optionally mono-, di- or tri-substituted with a substituent selected from the group of hydroxy, C 1 -C 4 alkoxy, C 1 -C 4 -alkylthio, C 1 -C 7 acyloxy, chlorine, tert-butyl, trifluoromethyl, isobutyl; α-, β-, γ-pyridyl; C 3 -C 7 -cycloalkyl; α- or β-naphthyl; 6-hydroxy- or 6-C 1 -C 4 -alkoxy-β-naphthyl; m-benzoylphenyl; 3,5-dimethylisossazol-4-yl; thien-2-yl; 1,3-dithian-2-yl or 1,3-dithian-5-yl; 1,3-dioxan-5-yl; pyrimidin-2-yl; triazin-2-yl; --(CH 2 ) 2 --(OCH 2 --CH 2 ) t H; --(CH 2 ) 2 --(OCH 2 --CH 2 ) t --OH; a heterocycle of formula (II): ##STR3## in which -Z< is a group H-C< or --(CH Z ) 2 --N<, whereas X is a single bond (between 2 carbon atoms), CH 2 , O, S, or NR c wherein R c is hydrogen, C 1 -C 4 -alkyl, C 1 -C 8 -acyl, tert-butoxycarbonyl (BOC), 9-fluorenylmethoxycarbonyl (FMOC), benzyloxycarbonyl, p-methoxybenzyloxycarbonyl, phenyl, benzyl, benzhydryl;
R is selected from the group consisting of:
β-pyridyl; fur-2-yl; 5-dimethylaminomethyl-fur-2-yl;
phenyl; phenoxy or phenylthio, being phenyl as defined above;
hydroxy, chlorine, bromine, iodine, (preferably bromine), C 1 -C 7 acyloxy, C 1 -C 7 sulfonate or a group of formula --S--C(═NR d )--NHR e in which R d and R e are independently hydrogen, C 1 -C 4 -alkyl, C 3 -C 7 cycloalkyl, benzyl;
4,5-dihydro-imidazol-2-yl-2-thio; 3,4,5,6-tetrahydro-pyrimidin-2-yl-2-thio;
a group of formula (III): ##STR4## wherein: when R 1 is hydrogen and R 2 is hydrogen, C 1 -C 7 -alkyl, C 3 -C 7 cycloalkyl or benzyl, R 3 is hydrogen, C 1 -C 4 -alkyl, tert-butoxycarbonyl (BOC), 9-fluorenylmethoxycarbonyl (FMOC), benzyloxy, p-methoxybenzyloxycarbonyl, one of the groups of formula R d N═C(YR e )-- or S; R d NH--C(═NH), R d NH--C(═N--CN); --C(═CH--NO 2 )-NHCH 3 , wherein R d and R e are as defined above and Y is 0 or S;
when R 1 is hydrogen, R 2 and R 3 , taken together with the nitrogen atom which they are linked to, can form a 5- or 6- membered nitrogen heterocyclic ring of formula (IV): ##STR5## wherein X and R c are as defined above; when R 2 is hydrogen, C 1 -C 4 -alkyl, R 1 and R 3 , taken together with the N and C atoms which they are linked to, can form a 5- to 7- membered saturated nitrogen heterocyclic ring;
m is zero or an integer 1 to 3;
n is zero or an integer 1 to 6;
p is the integer 2 or 3 but preferably the integer 2;
q is zero or the integer 1;
r is zero or an integer 1 to 3;
t is an integer 1 to 3;
the optically active forms, i.e. the enantiomers, diastereomers and the mixtures thereof and the pharmaceutically acceptable salts thereof.
The invention also relates to a process for the preparation of the compounds of formula (I) and the pharmaceutical compositions containing them for human and veterinary uses.
DESCRIPTION OF PREFERRED EMBODIMENTS
Examples of C 1 -C 4 alkyl groups are: methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl, preferably methyl, ethyl, tert-butyl.
Examples of amino-C 2 -C 4 -alkyl are dialkylamino-C 2 -C 4 -alkyls wherein C 2 -C 4 -alkyl is ethyl, propyl, butyl and the dialkylamino residue is dimethyl, diethyl, piperidin-1-yl and preferably dimethylaminoethyl.
Examples of C 1 -C 4 -alkoxyethyl groups are: methoxy-ethyl, ethoxyethyl, propoxyethyl, isopropoxyethyl, butoxyethyl, tert-butoxyethyl; preferably ethoxyethyl.
Examples of C 1 -C 4 -alkoxyphenyl are C 1 -C 4 -alkoxyethers of phenols and polyphenols and preferably p-methoxyphenyl, p-tert-butoxyphenyl, 3,4,5-trimethoxyphenyl, 4-hydroxy-3,5-dimethoxyphenyl, 3-hydroxy-4-methoxyphenyl, 4-hydroxy-3-methoxyphenyl, preferably 3,4,5-trimethoxyphenyl.
Examples of C 1 -C 4 -alkylthiophenyl are p-methylthiophenyl, p-tert-butylthiophenyl and preferably p-methylthiophenyl.
Examples of C 1 -C 7 -acyloxy are formyl, acetyl and benzoyl.
Examples of 6-C 1 -C 4 -alkoxy-β-naphthyl are 6-tert-butoxy and 6-methoxy, preferably 6-methoxy-β-naphthyl.
Examples of C 3 -C 7 -cycloalkyl are cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl and cycloheptyl, preferably cyclohexyl or cyclopentyl.
Examples of C 1 -C 7 -sulfonate are methanesulfonate, benzenesulfonate, preferably p-toluenesulfonate.
Examples of C 1 -C 7 alkyl groups are: methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl, n-heptyl, 3,3-dimethyl-but-2-yl, 2,2-dimethyl-pent-3-yl, preferably 3,3-dimethyl-but-2-yl.
Examples of heterocycles of formula (IV) are: pyrrolidine, piperidine, piperazine, 4-substituted-piperazines, morpholine, thiomorpholine, azepine, oxazepine, thiazepine, preferably pyrrolidine and morpholine.
Examples of preferred cations are those of lithium, sodium, potassium, magnesium, calcium, ammonium, triethylammonium, tromethamine or those of 1-amino acids such as glycine, lysine, valine, leucine, isoleucine, cysteine, methionine and arginine.
In compounds of formula (I), C 1 -C 4 -alkoxyphenyl is preferably methoxyphenyl, C 1 -C 7 -acyloxyphenyl is preferably formyloxyphenyl or acetoxyphenyl, R 1 is preferably hydrogen, the group --NR 2 R 3 is preferably NH 2 , methylamino, ethylamino, isopropylamino, dimethylamino or diethylamino; or R 2 and R 3 form a pyrrolidin-1-yl, piperidin-1-yl, morpholin-4-yl, thiomorpholin-4-yl group, or a piperazin-1-yl-4 group optionally substituted as 4-ureido, 4-methyl, 4-phenyl, 4-benzyl, 4-benzhydryl.
When the carboxylic groups of the compounds of formula (I) are undissociated or esterified, each of any basic groups present, i.e. any single --NR 2 R 3 and amino-C 2 -C 4 alkyl groups present, can be salified with non toxic, pharmaceutically acceptable acids such as acetic, trifluoroacetic, formic, propionic, fumaric, maleic, malonic, benzoic, salicylic, 3,4,5-trimethoxy-benzoic, methanesulfonic, benzenesulfonic, camphosulfonic, lactic, aspartic, glutamic, R- or S- thiazolidine-2-carboxylic acids, cysteine, N-acetyl-cysteine, carboxymethylcysteine; or inorganic acids such as phosphoric, sulfuric, hydrochloric and hydrobromic acids.
Preferred compounds of formula (I) are those wherein:
1) R a and R b are C 1 -C 4 alkyl, particularly ethyl, hydrogen or a cation as defined above;
2) R is a group of formula (III) as defined above, 5-dimethylamino-fur-2-yl or β-pyridyl;
3) n is an integer 2 to 5;
4) Φ is a group of formula --(CH 2 ) 1-3 and B is cycloalkyl C 3 -C 7 , particularly cyclohexyl;
5) Φ is a oxygen atom and B is 4-tetrahydropyranyloxy;
6) Φ is a group of formula --(CH 2 ) 1-2 --O-- and B is C 1 -C 7 acyloxy, particularly 2-ethoxy;
7) Φ is a sulfur atom and B is C 3 -C 7 cycloalkyl, particularly cyclohexyl;
8) the combination of two or more of the substituents of the above points.
Specific examples of the compounds of the invention are:
ethyl 4-(5-dimethylaminomethyl-fur-2-ylmethyltio)-2-cyclohexylmethyl-2-ethoxycarbonyl-butanoate;
ethyl 3-(3-pyridyl)-2-cyclohexylmethyl-2-ethoxycarbonyl-propanoate;
ethyl 5-BOC-amino-2-(4-tetrahydropyranyloxy)-2-ethoxycarbonyl-pentanoate;
ethyl 5-BOC-amino-2- 2-(ethoxy)-ethyloxy!-2-ethoxycarbonyl-pentanoate;
5-BOC-amino-2 (2-ethoxy)ethyloxy!-2-carboxy-pentanoic acid and the lithium salt thereof;
5-BOC-amino-2-(4-tetrahydropyranyloxy)-2-carboxy-pentanoic acid and the lithium, tromethamine and L-lysine salts thereof;
ethyl 5-BOC-amino-2-(3-cyclohexylpropyl)-2-ethoxycarbonyl-pentanoate;
ethyl 4-(pyrrolidin-1-yl)-2-cyclohexylmethyl-2-ethoxycarboxy-butanoate;
ethyl 3-(5-dimethylaminomethyl-fur-2-yl)-2-cyclohexylmethyl-2-ethoxycarbonyl-propanoate;
ethyl 5-amino-2-(4-tetrahydropyranyloxy)-2 -ethoxycarbonyl-pentanoate;
ethyl 5-amino-2- 2-(ethoxy)-ethyloxy!-2-ethoxycarbonyl-pentanoate;
ethyl 5-isopropylamino-2-cyclohexylmethyl-2-ethoxycarbonyl-pentanoate;
N- (4,4-diethoxycarbonyl),4-tetrahydropyranyloxy!-butyl guanidinium sulfate;
N- (4,4-diethoxycarbonyl),4-cyclohexylthio!,N'-ethylcyanoguanidine;
S- (4,4-diethoxycarbonyl),4-(2-(2-ethoxy)ethyl)!-butyl isothiouronium bromide.
The compounds of formula (I) are obtained by means of a process of substitution at the methine C-H of malonic esters of formula (V), wherein: ##STR6## R' a and R' b can be C 1 -C 4 -alkyl, C 1 -C 4 -alkoxyalkyl, allyl, p-methoxybenzyl, Φ is as defined above and B' is hydrogen; 2-propyl; tert-butyl; phenyl optionally mono-, di- and tri-substituted with a substituent selected from the group of C 1 -C 4 alkoxy, C 1 -C 4 -alkylthio, C 1 -C 7 acyloxy, chlorine, tert-butyl, trifluoromethyl, isobutyl; α-, β-, γ-pyridyl; C 3 -C 7 -cycloalkyl; fur-2-yl; α-, β-naphthyl; 6-C 1 -C 7 -acyloxy- and 6-C 1 -C 4 -alkoxy-β-naphthyl; m-benzoylphenyl, 3,5-dimethylisoxazol-5-yl; thien-2-yl; 1,3-dithian-2-yl and 1,3-dithian-5-yl; 1,3-dioxan-5-yl; pyrimidin-2-yl; triazin-2-yl, --(CH 2 ) 2 --(OCH 2 --CH 2 ) t H and --(CH 2 ) 2 --(OCH 2 --CH 2 ) t --O--C 1 --C 7 acyl, a heterocycle of formula (II), wherein, being Z selected from the group of H--C< and --(CH 2 ) 2 --N<, X is a single bond (between 2 carbon atoms), CH 2 , O, S, NR' c wherein R' c can be C 1 -c 4 -alkyl, C 1 -C 8 -acyl, tert-butoxycarbonyl (BOC), 9-fluorenylmethoxycarbonyl (FMOC), benzyloxycarbonyl, p-methoxybenzyloxycarbonyl, phenyl, benzyl, benzhydryl.
The process comprises the alkylation of a compound of formula (V) with a compound of formula (VI):
Ψ--(CH.sub.2).sub.n --W (VI)
wherein n is as defined above, and is selected from:
β-pyridyl;
phenyl, acyloxyphenyl, phenoxy or phenylthio as defined above;
hydroxy, C 1 -C 7 -acyloxy;
a group of formula (VII): ##STR7## wherein m is as defined above, and: when R' 1 is hydrogen and R' 2 is hydrogen, C 1 -C 7 -alkyl, C 3 -C 7 -cycloalkyl or benzyl, R' 3 is hydrogen, C 1 -C 4 -alkyl, tert-butoxycarbonyl (BOC), 9-fluorenylmethoxycarbonyl (FMOC), benzyloxy or p-methoxybenzyloxycarbonyl,
when R' 1 is hydrogen, R' 2 and R' 3 taken together with the nitrogen atom which are linked to, can form a 5- or 6- membered nitrogen heterocyclic ring of formula (IV): ##STR8## wherein X and R' c are as defined above; when R' 2 is hydrogen, C 1 -C 4 -alkyl, R' 1 and R' 3 , taken together with the N and C carbon atoms which are linked to, can form a 5- to 7- membered saturated heterocyclic ring, as defined above;
W is chlorine, bromine, iodine or a sulfonic ester such as mesylate, p-toluenesulfonate, benzenesulfonate, trifluoromethanesulfonate;
to give a compound of formula (Ia): ##STR9## wherein R' a , R' b , Ψ, B' and Φ are as defined above, which can be optionally transformed into a compound of formula (I), for example through ester interchange reactions, cleavage of any protecting groups present, N-alkylation or acylation, O-acylation or O-substitution with thiol groups to give mercaptans and the straight or cyclic thioureids thereof, salification of free amino and/or carboxylic groups. For example, the diesters of the compounds of formula (Ia), can be hydrolyzed or transformed into the geminal dicarboxylic acids thereof to be recovered as salts or free acids or re-esterified with a suitable alcohol R a OH or R b OH or mixtures thereof. When Ψ in the compounds of formula (Ia) is the residue of a primary and/or secondary amino-protecting group, after cleavage of the protecting group itself, the resulting amine can be transformed into the corresponding ureide, thioureide, isothioureide, guanidine, cyanoguanidine and N'-alkylderivatives thereof using methods well known in preparative organic chemistry, and described recently by, for example, C. R. Rasmussen, Synthesis 460, 1988; A. B. Miller et al, ibidem, 777, 1986; C. A. Marianoff and al. J. Org. Chem., 51, 1882, 1986; Org. Synth., 21, 89, 1948; E. Schmidt et al., Ann, 6, 1, 1959; H. A. Staab, ibidem, 657, 104, 1982; Monatsh. fur Chemie, 90, 41, 1959; K. Ley, Ang. Chem., 78, 672, 1968; Helv. Chim. Acta, 1716, 1966; J. Org. Chem., 30, 2465, 1965. Analogously, when Ψ in the compounds of formula (Ia) is the residue of a primary or secondary hydroxy-protecting group or a hydroxy group, this can be converted into the corresponding sulfonic acid ester (mesylate, triflate, benzenesulfonate, p-toluenesulfonate), using well known methods, or in the corresponding alkyl halide, preferably iodide or bromide, which, by reaction with a suitable thiol, will give the compounds of formula (Ia) wherein R is a group --S--C(═NR d )-NHR e , 4,5-dihydroimidazol-2-yl-2-thio; 3,4,5,6-tetrahydro-pyrimidin-2-yl-2-thio, (R d and R e being as defined above).
The hydrolysis of the esters of the gemdicarboxylic acids of the compounds of formula (Ia) is effected preferably with LiOH aqueous solutions of LiOH in a C 1 -C 3 alcohol, in a temperature range from room temperature to -10° C., in a time from a few hours to 48 hours. Preferred solvent is methanol and the reaction is performed in the presence of at least two molar equivalents of the base or of a slight excess thereof. The allyl esters can be removed in the presence of Pd-phosphines and of an alkanoic acid alkali salt. The transformation of a compound of formula (Ia) into a compound of formula (I) wherein R a , R b are hydroxy, can be carried out, by hydrolysis of the ester groups, prior to removing all the protecting groups optionally present.
A compound of formula (I) wherein R a , R b are hydroxy can be converted into another compound of formula (I) wherein R a and R b are the counter-ions thereof with a conventional salification process with a pharmaceutically acceptable inorganic or organic base. Particularly preferred organic bases are basic α-amino acids such as L-lysine, L-arginine and L-N'-methylarginine and aminoalcohols such as tromethamine and D-glucamine.
The malonic acid diesters of formula (V): ##STR10## are commercially available compounds or can be prepared from commercially available products with known methods.
Thus, malonic acid esters of formula (V) wherein Φ is a S atom can be obtained by thiolating the halomalonate diesters R' a O 2 C--(CH--G)--CO 2 R' b wherein G is Cl, Br, I, preferably Br, with a suitably reactive mercaptan, such as (B'--S - Na + ) or by reacting a reactive malonate, such as R' a O 2 C--(CH - Na + )--CO 2 R' b with a sulfenyl halide (B'--S + G a - ) being G a Cl or Br, preferably Br, and B', R' a and R' b as defined above. More precise indications about these preparation methods can be found in the following literature. Use of sulfenyl halides: Brintzinger et al., Chem. Ber., 86, 557, 1953; Mattioda et al., J. Med. Chem., 18, 553, 1975, Labushagne et al., Tetrah. Lett., 3571 (1976); use of halomalonates and thiols: in Kaloustian et al, J. Amer. Chem. Soc., 98, 956, 1976; E. Juaristi et al., J. Org. Chem., 55, 33, 1990; J. Grossert et al., J. Chem. Soc. Comm., 20, 1183, 1982; R. Aveta et al., Gazz. Chim. It., 116, 649, 1986; use of sulfanes in Labuschagne et al., J. Chem. Soc. Perk. Trans. I, 955, 1978; or thioacetimide esters halohydrates in H. Singh et al., Indian J. Chem. Sect. B, 21, 272, 1982 and 24, 131, 1985 esters; or p-toluenethiosulfonic S-esters in Hayashi et al., Chem. Pharm. Bull., 19, 1557, 1971.
Still more particularly, malonic acid diesters of formula (V) wherein Φ is an O atom are prepared by reaction of a B'--OH alcohol with a diazomalonic acid ester of formula (VIII): ##STR11## in the presence of dimer Rh diacetate, (B', R' a and R' b as above described). The O-alkylation technique derives from that described by Paulissen et al., Tetrah. Lett., 2223 (1973) in the case of carboxylic acid α-diazo esters. Alternatively, the reaction can also be performed in the presence of silica gel, according to the process described by Ohno et al., Tetrah. Lett., 4005 (1979) as far as carboxylic acid α-diazo esters are concerned.
Malonic acid diesters of formula (V) and methods suitable for the preparation thereof are described inter alia in WO 94/10127, PCT/EP93/02941 (23.10.1993) in the Applicant's name.
The compounds of the invention can be used in the treatment of osteoporosis and bone dysmetabolism diseases, in the treatment of malignant hypercalcemia and of Paget's disease.
The metabolic abnormalities of bone tissue are often characterized by a loss in the bone mass and they can be related both to a matrix mineralisation incapability and an inadequate matrix formation, which pathologies are also known under the names of osteomalacia and osteoporosis, respectively. Bone tissue is an active, continuously formed tissue, whose equilibrium depends on an appropriate control of the bone neo-formation and degradation processes which are regulated by the functional activity of osteoblasts and osteoclasts, which are cells respectively presiding the osteogenic and osteolytic functionalities.
Osteoclasts are considered to be the main responsible for bone resorption. Pits following to bone resorption processes are observed, for example, when enzymatically recovered primary cultures of rabbit osteoclasts are grown on bovine devitalized bone fragments. As a consequence, medicaments that may maintain the osteoclastic activity while inhibiting any hyperactivity in all the osteoclastic hyper-reactivity pathological conditions, in which bone resorption processes prevail on the neo-formation ones, are of paramount interest.
The compounds of the invention, when tested n vitro, according to the method described by Y. Su et al., Endocrinology, 131, 1497, 1992 in a concentration scalar range from 10 -12 to 10 -6 M, evidence an effective inhibition of the formation of bone pits without cytotoxyc effects on the osteoclasts themselves.
Moreover, the compounds of the invention are effective in vivo, after both subcutaneous and oral administrations, in inhibiting bone resorption which is usually observed in female mice after ovariectomy. The experimental method used, with minor changes, is that described by R. Kitazava et al., (J. Clin. Inv., 94, 2397, 1994). For the final evaluation of the percent changes in the bone mass of shin bone and long bone, compared with non-treated, ovariectomized controls, the experimental method refers, with the appropriate changes, to the method described by E. I. Barengolts et al., (Calcif. Tissue Int., 52, 239, 1993).
Specific examples of the compounds of the invention are:
A) 5-BOC-amino-2- 2-(ethoxy)-ethoxy!-2-carboxy-pentanoic acid lithium salt;
B ethyl 5-BOC-amino-2- 2-(ethoxy)-ethoxyl!-2-carboxypentanoate;
C) ethyl 5-BOC-amino-2-cyclohexylmethyl-2-carboxypentanoate;
D) ethyl 5-BOC-amino-2- 4-tetrahydropyranyl-1-oxy!-2carboxy-pentanoate;
E) ethyl 5-BOC-amino-2- 3-cyclohexyl-prop-1-yl!-2-carboxypentanoate;
In a series of tests, the compounds were evaluated compared with:
ALN:alendronate;
F) ethyl 5-BOC-amino-2- 2-tetrahydropyranyl-1-oxy!-2-carboxy-pentanoate;
G) 5-BOC-amino-2- 2-tetrahydropyranyl-1-oxy!-2-carboxypentanoic acid lithium salt;
taken as positive standards. The synthesis of the compounds F and G has been performed according to the process described in WO 94/10127 PCT/EP93/02941 (23.10.1993).
After subcutaneous administration, compared with -1,83±1,53 and -3,06±1,50% decreases in bone mass in ovariectomized female mice, respectively for shin bone and long bone, in the animals treated with the compounds ALN, A, F, G, the following results were obtained:
______________________________________ % changes mg/kg shin bone long bone______________________________________ALN 20 (mg) 0.78 ± 1.69 0.02 ± 1.86 20 (mg) 1.+9 ± 2.46 0.66 ± 3.23 20 (mg) 3.43 ± 0.95 4.04 ± 1.21F 10 2.20 ± 0.85 -0.60 ± 0.73 30 6.49 ± 0.83 1.56 ± 1.46G 10 -0.40 ± 1.00 1.29 ± 0.26 30 3.57 ± 2.03 6.12 ± 3.04 100 2.28 ± 1.75 2.80 ± 2.55A 10 0.34 ± 1.49 0.84 ± 1.43 30 1.68 ± 1.80 2.15 ± 2.57______________________________________
After oral administration, compared with -0,50±1,74 and -7,92±1,63 decreases in bone mass in ovariectomized female mice, respectively for shin bone and long bone, in the animals treated with the compounds ALN, B, C, D, F, the following results were obtained:
______________________________________ % changesmg/kg shin bone long bone______________________________________ALN 6 4.86 ± 1.30 0.08 ± 1.62F 25 -4.97 ± 3.10 -13.42 ± 3.68B 25 -1.59 ± 1.51 -3.61 ± 1.66C 25 1.98 ± 1.78 -2.90 ± 2.03D 25 4.05 ± 1.44 -1.67 ± 1.44______________________________________
The evaluation of all the test results proves that the compounds of the present invention are particularly suitable for attaining the desired therapeutical purposes. More particularly, the compounds of the present invention turned out to be effective even after oral administration, which is obtained not so effectively as with tartronic acids and the acetal ethers thereof.
The administration of the compounds of the invention causes no adverse effects on bone growth and mineralisation.
For the envisaged therapeutical purposes, the compounds of the invention are suitably formulated in pharmaceutical compositions using conventional techniques, such as those described in "Remington's Pharmaceutical Sciences Handbook" Mack Publishing Co., New York, USA, 17th Ed., 1985.
The pharmaceutical compositions of the invention can be administered intramuscularly, intravenously, as a bolus and preferably orally, in the form of capsules, tablets, syrups and optionally as controlled-release forms. The daily dosage will vary depending on a number of factors, such as the severity of the disease and the conditions of patient (sex, weight, age): the dose will vary from 2 to 1200 mg of compound daily, optionally in repeated administrations. Higher dosages and more protracted administration times could be considered, in view of the low toxicity of the compounds of the invention.
The following examples further illustrate the invention.
EXAMPLE 1
48 g of p-tosylazide (J. Prakt. Chem., 125, 323, 1930) are added in small portions, under stirring and at room temperature, to a solution of diethyl malonate (40 g) in abs. ethanol (EtOH); when the addition is completed, stirring is continued for 5 min., then a solution of triethylamine (34 ml) in 30 ml of abs. ethanol is added dropwise keeping stirring overnight. When the reaction is complete, (TLC, SiO 2 Hexane/AcOEt 8:2), ethanol is evaporated off and the residue is suspended in hexane/AcOEt 7:3 to separate p-tosylamide which is filtered off. After a second precipitation with hexane/AcOEt 7:3, 40 g of good purity ethyl diazomalonate (90% yield) are obtained.
EXAMPLE 2
A catalytic amount of Rh(OAc) 2 ! 2 is added to a solution of ethyl diazomalonate (20 g) in ethylene glycol (40 ml) which acts both as reagent and solvent. Carefully checking the reaction mixture reactivity, and under stirring, the mixture is heated gradually to a temperature of 50° C., keeping stirring at this temperature for 24 h., which is the time necessary for the starting diazoderivative to disappear (TLC, SiO 2 CHCl 3 /MeOH 98:2). The solvent excess is evaporated, under reduced pressure at 40° C.; the residual alcohol is distilled off azeotropically with toluene. After purification on a silica gel column, eluent CHCl 3 /MeOH 98:1, 18.2 g of ethyl 2-(2-ethoxyethyl)oxy-malonate are obtained (69% yield). 1 HNMR (CDCl 3 , ppm): 4.6 (1H, s, O═C--(CHO--)--C═O); 4.2 (4H, q, O═C--O--CH 2 --CH 3 ); 3.75 (2H, t, O═C--(CHO--CH 2 --)--C═O, J 5 Hz); 3.6 (2H, t, O═C--(CHO--CH 2 --CH 2 --)--C═O, J 5 Hz); 3.45 (2H, q, --O--CH 2 --CH 3 , J 4 Hz); 1.25 (6H, t, O═C--O--CH 2 --CH 3 , J 7 Hz); 1.1 (3H, t, --O--CH 2 --CH 3 , J 7 Hz).
EXAMPLE 3
A solution of 4-hydroxy-tetrahydropyrane (11.5 g) and ethyl diazomalonate (18.7 g) in 30 ml of dichloromethane, added with a catalytic amount of Rh(OAc) 2 ! 2 , is refluxed under stirring for 24 h until the starting diazoderivative completely disappears. The mixture is concentrated to small volume and the residue is eluted through silica gel, eluent CHCl 3 /MeOH 98:1, to obtain 16.4 g of ethyl 4-tetrahydropyranyloxy-malonate. 1 HNMR (CDCl 3 , ppm): 4.6 (1H, s, O═C--(CHO--)--C═O); 4.3 (4H, q, O═C--O--CH 2 --CH 3 ); 4.0-3.9 3.45-3.4 (4H, m system, --CH 2 --O--CH 2 --); 3.71 (1H, m, >C(--H)--O--); 2.0-1.85 1.8-1.65 (4H, m system, --CH 2 --C(--O--)--CH 2 --); 1.2 (6H, t, O═C--O--CH 2 --CH 3 , J 7 Hz).
Using in the procedure of example 2 a different alcohol (as reagent and solvent) or when, as described above, said alcohols and phenols cannot be used as solvents due to their poor volatility and high cost by reacting ethyl diazomalonate with 1.1 molar equivalents of said reagents in the presence of Rh(OAc) 2 ! 2 in an inert solvent such as dichloromethane, ethyl acetate, dioxane, benzene, tetrahydrofuran and mixtures thereof in a reagents/solvents weight ratio of at least 2:1, the following compounds are obtained: ethyl phenoxymalonate;
ethyl p-chlorophenoxymalonate, chemically identical to a sample prepared according to C. A. 113: 211579 k;
ethyl 1-(3-ethoxy-propyl)-oxy-malonate;
ethyl 1-(4,7-dioxa-nonyl)-oxy-malonate;
ethyl 1-(3,6-dioxa-octyl)-oxy-malonate;
ethyl 1-(5-hydroxy-3-oxa-pentyl)-oxy-malonate;
ethyl cyclohexyloxymalonate;
ethyl cyclohexylmethoxymalonate;
ethyl 2-cyclohexyl-ethoxymalonate;
ethyl 3-cyclohexyl-propoxymalonate;
ethyl 2-cyclopentyl-ethoxymalonate;
ethyl 3-cyclopentyl-propoxymalonate;
ethyl 4-tetrahydropyranylmethoxy-malonate;
ethyl 4-tetrahydrothiapyranylmethoxy-malonate;
ethyl 2-(tetrahydropyran-4-yl)-ethoxy-malonate;
ethyl 3-(tetrahydropyran-4-yl)-propoxy-malonate;
ethyl 1,3-dioxan-5-yloxy-malonate;
ethyl 1-BOC-piperidin-4-yloxy-malonate;
ethyl 1-BOC-piperidin-4-yl-methoxy-malonate;
ethyl 1-isopropyl-piperidin-4-yl-methoxy-malonate;
ethyl 2-(1-isopropyl-piperazin-4-yl)ethoxy-malonate;
ethyl 2-(pyrrolidin-1-yl)ethoxy-malonate;
ethyl 2-(piperidin-1-yl)ethoxy-malonate;
ethyl benzyloxymalonate;
ethyl pyridin-4-yl-methoxymalonate;
ethyl pyridin-2-yl-methoxymalonate;
ethyl pyrimidin-2-yl-methoxymalonate;
ethyl triazin-2-yl-methoxymalonate;
ethyl pyridin-3-yl-methoxymalonate;
ethyl pyridin-3-yl-ethoxymalonate;
ethyl pyridin-4-yl-oxymalonate;
ethyl pyridin-3-yl-oxymalonate;
ethyl 4-(3,5-dimethyl-isoxazolyl)methoxymalonate;
ethyl 2-(2-thienyl)ethoxymalonate;
ethyl 2-phenylethoxy-malonate;
ethyl 2-(3,4,5-trimethoxy-phenyl)ethoxy-malonate;
ethyl 3-phenyl-propoxymalonate;
ethyl 3-(3,4,5-trimethoxy-phenyl)propoxymalonate;
ethyl (1S,2S)-10-pyranyloxy-malonate.
EXAMPLE 4
Using the methods described above by Kaloustian et al.; Juaristi et al.; Grossert et al.; Aveta et al., for the preparation of diethyl phenylthiomalonate, diethyl benzylthiomalonate, the following compounds are obtained: ethyl cyclohexylthiomalonate; ethyl 4-tetrahydropyranylthiomalonate; ethyl 3-pyridyl-methylthiomalonate; ethyl cyclohexylmethylthiomalonate; ethyl 2-cyclohexylethylthiomalonate; ethyl 4-tetrahydropyranyl-methylthiomalonate; ethyl 2-(2-ethoxyethyl)-thiomalonate; ethyl 1-(3-ethoxypropyl)-thiomalonate.
EXAMPLE 5
Under stirring and nitrogen atmosphere, 18.3 g of ethyl 2-(2-ethoxyethyl)oxy-malonate (74 mmoles) are added to a solution of sodium ethoxide in 35 ml of EtOH (prepared dissolving metal Na (1.95 g, 0.085 moles) in ethanol). Stirring is continued for 1 h at room temperature, then a solution of 3-BOC-amino-1-propylbromide (17.6 g, 74 mmoles) in EtOH (30 ml) is added dropwise. The reaction mixture is heated at 50° C. and kept overnight a this temperature. After 1h at 50° C. the formation of an abundant NaBr precipitate is observed. The progress of the reaction can be checked by TLC on SiO 2 , eluent CHCl 3 /MeOH 98:2. When the reaction is completed, the solvent is evaporated off under vacuum and the residue is partitioned between water and AcOEt. The aqueous phase is re-extracted with AcOEt (2×50 ml); the combined organic phases are washed to neutality with a 5% NaH 2 PO 4 aqueous solution and water, and finally dried over sodium sulfate. After evaporation of the solvent and purification of the residue on a silica gel column, eluent CHCl 3 /MeOH 98:1, 21 g (51.5 mmoles, 70% yield) of ethyl 5-BOC-amino-2-ethoxycarbonyl-2- (2-ethoxy)-ethyloxy!-pentanoate are obtained.
1 HNMR (CDCl 3 , ppm): 4.5 (1H, m, --NH--); 4.2 (4H, q, --CO 2 --CH 2 --, J 7 Hz); 3.7-3.6 (2H, m, --CH 2 --O--CH<(C═O) 2 --); 3.6-3.5 (2H, m, --O--CH 2 --CH 2 --O--); 3.4 (2H, q, CH 3 --CH 2 --O--, J 7 Hz); 3.1-3.0 (2H, m, --NH--CH 2 --); 2.2-2.0 (2H, dd, --CH 2 --CH 2 --C(C═O--) 2 --O--); 1.4 (9H, s, (CH 3 ) 3 --C--O--CO--; 1.2 (6, t, --CO 2 --CH 2 --CH 3 , J 7 Hz); 1.1 (3H, t, --O--CH 2 --CH 3 , J 7 Hz).
EXAMPLE 6
Using in the procedure described in example 5, one of the malonic esters described in examples 3 and 4, are obtained:
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 4-tetrahydropyranyloxy!-pentanoate; 1 HNMR (CDCl 3 , ppm): 4.55 (1H, m, --NH--); 4.22 (4H, q, --CO 2 --CH 2 --, J 7 Hz); 4.0-3.8 (1H, m, >C(--H)--O--); 4.0-3.8 3.25-3.0 (4H, m system, --CH 2 --O--CH 2 ); 3.43 (2H, dt, --NH--CH 2 --, J 1 7 Hz); 2.02 (2H, dd, 2 (O═C)>C(--O--)--CH 2 J 1 10 Hz, J 2 6 Hz); 2.0-1.45 (6H, --CH 2 --CH(--O--)--CH 2 --+--NH--CH 2 --CH 2 --CH 2 --); 1.4 (9H, s, (CH 3 ) 3 --C--O--CO--; 1.3 (6H, t, --CO 2 --CH 2 --CH 3 , J 7 Hz).
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 4-tetrahydropyranyl-methoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 4-tetrahydropyranyl-ethoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 4-tetrahydropyranyl-propoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 1,3-dioxan-5-yloxy!pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 1-BOC-piperidin-4-yloxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 1-BOC-piperidin-4-yl-methoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 1-isopropyl-piperidin-4-yl-methoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 2-(1-isopropylpi-perazin-4-yl)ethoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 2-(pyrrolidin-1-yl)-ethoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- (piperidin-1-yl)ethoxy!pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 2-(cyclopentyl)-ethoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- n-pentoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2-benzyloxy-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- pyridin-4-yl-methoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- pyridin-2-yl-methoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- pyridin-3-yl-methoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- pyridin-3-yl-ethoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- pyridin-4-yl-oxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- pyridin-3-yloxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 2-phenylthoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 2-(3,4,5-trimethoxy-phenyl)-ethoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 3-phenyl-propoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 3,4,5-trimethoxy-phenyl-propoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- (1S,2S)-10-pyranyloxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- cyclohexylthio!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 4-tetrahydropyranyl-thio!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 3-pyridylmethylthio!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- cyclohexylmethylthio!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 4-tetrahydropyranylmethylthio!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 2-(2-ethoxyethyl)-thio!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 1-(3-ethoxypropyl)thio!-pentanoate.
EXAMPLE 7
In the following, the general process for the hydrolysis of each of the esters of examples 5 and 6 is described: a solution of 50 mmoles of a diester, e.g. 5-BOC-amino-2-ethoxycarbonyl-2- (2-ethoxy)ethyloxy!-pentanoate (20.2 g) in 25 ml of MeOH is added, under stirring, with 157 ml of a 0.63 N solution of LiOH.H 2 0 in water/MeOH (1:1), equivalent to 100 mmoles of base. The mixture is stirred for 18 hours at room temperature to complete the reaction (TLC, SiO 2 , eluent BuOH/H 2 O/AcOH 3:1:1), then methanol is evaporated off under vacuum. After freeze-drying, the solid residue is repeatedly suspended and triturated in AcOEt/Et 2 O to remove any traces of unreacted material, then is dissolved in water and filtered.
The aqueous solution is then freeze-dried to give 16.82 g of 5-BOC-amino-2-carboxy-2- (2-ethoxy)ethyloxy!-pentanoic acid lithium salt, as a crystal powder.
1 HNMR (D 2 O, ppm): 3.85 (2H, t, --CH 2 --O--CH 2 --CH 2 --, J 5 Hz); 3.77 (2H, q, CH 3 --CH 2 --O--J 7 Hz); 3.6 (2H, t, --CH 2 --O--CH 2 --CH 2 --, J 5 Hz); 2.12 (2H, m, --CH 2 C(<CO 2 --) 2 --O--); 1.6 (9H, s, (CH 3 ) 3 C--O--CO--NH); 1.6-1.5 (2H, m, --NH--CH 2 --CH 2 --CH 2 --); 1.37 (3H, m, CH 3 --CH 2 --O--).
EXAMPLE 8
An aqueous solution of 5 g of 5-BOC-amino-2-carboxy-2- 4-tetrahydropyranyloxy!-pentanoic acid lithium salt 1 HNMR (D 2 O, ppm): 4.2-4.05 3.7-3.5 (4H, m, --CH 2 --O--CH 2 --); 3.8 (OH, m, --CH 2 --CH(--O--)--CH 2 --); 3.23 (2H, t, --NH--CH 2 --, J 6 Hz); 2.2-1.7 (6H, m syst., --CH 2 --CH(--O)--CH 2 --+--CH 2 C(<CO 2 )--O--); 1.6 (9H, s, (CH 3 ) 3 C--O--CO--NH); 1.6-1.5 (2H, m, --NH--CH 2 --CH 2 --CH 2 --)! is acidified to pH 4-5 by dilution under stirring with a 10% KHSO 4 aqueous solution. The separated acid is extracted repeatedly with ether ethyl and from the combined organic phases, washed with a 2% KHSO 4 aqueous solution and water to neutrality. By evaporation of the solvent under vacuum, 4.15 g of 5-BOC-amino-2-carboxy-2- 4-tetrahydropyranyloxy!-pentanoic acid are obtained. A solution of 3.5 g of the acid in EtOH is added with 2.93 g of 1-lysine in water to obtain 5.85 g of 5-BOC-amino-2-carboxy-2- 4-tetrahydropyranyloxy!-pentanoic acid 1-lysine salt. Analogously, by salification, the 5-BOC-amino-2-carboxy-2- 4-tetrahydropyranyloxy!-pentanoic acid tromethamine salt is obtained.
EXAMPLE 9
Using in the C-alkylation process of example 5, an ester selected from the group of ethyl 2-m-benzoylphenylmalonate, 6-methoxy-β-naphthylmalonate, phenylthioethylmalonate, 4-tetrahydrothiapyranyl-methoxymalonate, 4-(3,5-dimethyl-isoxazolyl)methoxymalonate, 2-(2-thienyl)ethoxymalonate and cyclohexylpropylmalonate, the following compounds are obtained:
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- m-benzoylphenyl!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 6-methoxy-β-naphthyl!pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 4-(3,5-dimethylisoxazolyl)-methoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 2-phenylthioethyl!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 2-(2-thienyl)-ethoxy!-pentanoate;
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 4-tetrahydrothiapyranylmethoxy!-pentanoate
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 3-cyclohexylprolyl!-pentanoate:
1 HNMR (CDCl 3 , ppm): 4.53 (1H, bs NH); 4.18 (4H, q. --CO 2 --CH 2 --CH 3 , J 7 Hz); 3.11 (2H, m, NH--CH 2 --); 1.9-1.85 (4H, m, --CH 2 --C(<(CO 2 ) 2 )--CH 2 --); 1.7-1.6 1.5-1.3-1.3-1.1 (17 H complex system of m --NH--CH 2 --CH 2 --+ ##STR12## 1.45 (9H, s. (CH 3 ) 3 --OCONH); 1.25 (6H, t, --CO 2 --CH 2 --CH 3 ; J 7 Hz).
EXAMPLE 10
Using in the process of example 5 ethyl 3-cyclohexyl-2-ethoxycarbonyl-propionate and a suitable halide, selected from the group of α-, β- and γ-pyridomethyl chloride or bromide, 2-BOC-aminoethyl bromide, 2-BOC-ethylaminoethyl bromide, 3-BOC-aminopropyl bromide, 3-BOC-isopropylaminopropyl bromide, (2S) (1-BOC-pyrrolidin-2-yl)-methyl bromide, (pyrrolidin-1-yl)-ethyl bromide and furfuryl bromide, the following compounds are obtained:
ethyl 3-(2-pyridyl)-2-cyclohexylmethyl-2-ethoxycarbonyl-propanoate;
ethyl 3-(3-pyridyl)-2-cyclohexylmethyl-2-ethoxycarbonyl-propanoate;
ethyl 3-(4-pyridyl)-2-cyclohexylmethyl-2-ethoxycarbonyl-propanoate;
ethyl 4-BOC-amino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-butanoate;
ethyl 4-BOC-ethylamino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-butanoate;
ethyl 5-BOC-isopropylamino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-pentanoate;
ethyl 3- (S) N-BOC-pyrrolidin-2'-yl!-2-cyclohexylmethyl-2-ethoxycarbonyl-propanoate;
ethyl 4-(pyrrolidin-1'-yl)-2-ethoxycarbonyl-butanoate;
ethyl 5-BOC-amino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-pentanoate;
ethyl 3-(fur-2-yl)-2-cyclohexylmethyl-2-ethoxycarbonyl-propanoate, which by reaction with formaldehyde and dimethylamine hydrochloride yields ethyl 3-(5-dimethylaminomethyl-fur-2-yl)-2-cyclohexylmethyl-2-ethoxycarbonyl-propanoate.
EXAMPLE 11
A solution of ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 4-tetrahydropyranyloxy!-pentanoate in CH 2 Cl 2 (20 ml), cooled at 0-5° C., is added with trifluoroacetic acid (5 ml). After a night at room temperature, the mixture is evaporated under vacuum to obtain, after trituration of the residue in ethyl ether, 3.86 g of 4,4-diethoxycarbonyl-4-(4-tetrahydropyranyloxy)-butylammonium trifluoroacetate. A suspension of the salt in AcOEt (25 ml) is neutralized, under stirring at 0-5° C., by careful addition of a 5% sodium bicarbonate aqueous solution. After separating the organic phase and re-extracting the aqueous phase with AcOEt (3×5 ml), the combined organic phases are dried over Na 2 SO 4 , and solvent is evaporated off to obtain 2.73 g of ethyl 5-amino-2-ethoxycarbonyl-2- 4-tetrahydropyranyloxy!-pentanoate.
The cleavage of the tert-butoxycarbonyl-protecting group is carried out analogously, and each of the BOC-derivatives of examples 5, 6, 9 and 10 is converted into the corresponding amine. Thus, for instance, by reacting with a molar excess of trifluoroacetic acid in CH 2 Cl 2 the BOC derivatives:
ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 1-BOC-piperidin-4-yloxy!-pentanoate; ethyl 5-BOC-amino-2-ethoxycarbonyl-2- 1-BOC-piperidin-4-yl-methoxy!-pentanoate; ethyl 4-BOC-amino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-butanoate;
ethyl 4-BOC-ethylamino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-butanoate; ethyl 5-BOC-isopropylamino-2-(cyclohexylmethyl)-2-ethoxycarbonylpentanoate; ethyl 5-BOC-amino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-pentanoate, the corresponding amines are obtained:
ethyl 5-amino-2-ethoxycarbonyl-2- piperidin-4-yloxy!-pentanoate;
ethyl 5-amino-2-ethoxycarbonyl-2- piperidin-4-yl-methoxy!-pentanoate;
ethyl 4-amino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-butanoate;
ethyl 4-ethylamino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-butanoate;
ethyl 5-isopropylamino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-pentanoate;
ethyl 5-amino-2-(cyclohexylmethyl)-2-ethoxycarbonyl-pentanoate.
EXAMPLE 12
According to the general method described by C. A. Maryanoff et al., J. Org. Chem., 51, 1882, 1986, 0.005 mmoles (0.062 g) of aminoiminomethanesulfonic acid are added at room temperature to a solution of 0.0065 mmoles (2.06 g) of ethyl 5-amino-2-ethoxycarbonyl-2- 4-tetrahydropyranyloxy!-pentanoate in acetonitrile (5 ml) to separate 3.7 g of N-(4,4-diethoxycarbonyl-4-tetrahydropyranyloxy)-butyl guanidinium sulfate.
Analogously, but using methylaminoimino-methanesulfonic and anilinoimino-methanesulfonic acids, the following compounds are obtained: N-methyl-N'-(4,4-diethoxycarbonyl-4-tetrahydropyranyl-oxy)-butyl guanidinium sulfate N-phenyl-N'-(4,4-diethoxycarbonyl-4-tetrahydropyranyl-oxy)-butyl guanidinium sulfate.
By reaction with 1-methylthio-1-methylamino-2-nitroethene, 1,1-ethenediamine,N-(4,4-diethoxycarbonyl-4-tetrahydropyranyloxy)-butyl),N'-methyl-2-nitro is obtained.
EXAMPLE 13
A solution of ethyl 5-amino-2-ethoxycarbonyl-2- cyclohexylmethylthio!-pentanoate (3.63 g, 1.05 mmoles) and dimethyl N-cyanoimidodithiocarbonate (2 g, 1.37 mmoles) in isopropanol (15 ml) is kept at room temperature for 4h; then is diluted with 30 ml of Et 2 O and the mixture is kept at room temperature overnight. 4.01 g of N- 4,4-diethoxycarbonyl-4-cyclohexylmethyltiobutyl!-N'-cyano-S-methyl-isothiourea separate.
A solution of 2 g of the compound with a 5% ethylamine solution in EtOH is refluxed to yield 1.9 g of N- 4,4-diethoxycarbonyl-4-cyclohexylmethylthiobutyl!-N'-ethyl-cyanoguanidine.
Analogously, by reaction with (R,S)-3,3-dimethyl-2-butylamine, (R,S) N- 4,4-diethoxycarbonyl-4-cyclohexylmethylthio-butyl!-N'-3,3-dimethyl-2-butyl-cyanoguanidine is obtained.
EXAMPLE 14
6 g of ethyl 2-(2-ethoxyethyl)oxymalonate (24.65 mmoles) are added to a solution of sodium ethoxide in EtOH (15 ml, prepared by dissolution of 0.65 g, 0.028 moles metal Na) under stirring and nitrogen atmosphere. Stirring is continued for 1 h at room temperature, then a solution of 3-trityloxy-1-propyl-bromide (9.4 g, 24.7 mmoles) in EtOH (20 ml) is added dropwise. The reaction mixture is heated at 50° C. and kept at this temperature overnight. When the reaction is completed, the solvent is evaporated off under vacuum and the residue is partitioned between water and AcOEt. The aqueous phase is re-extracted with AcOEt (2×50 ml), the combined organic phases are washed to neutrality with a 5% NaH 2 PO 4 aqueous solution, then with water, and finally dried over sodium sulfate. After evaporation of solvent, the resulting solution of crude ethyl 5-trityloxy-2-ethoxycarbonyl-2- (2-ethoxy)ethyloxy!-pentanoate in EtOH is treated with 0.3 g of p-toluenesulfonic.H 2 O acid and kept for 12 h at room temperature. After evaporation of solvent, the residue is dissolved in dichloromethane (15 ml) and the organic phase is washed with 2×5 of 5% aqueous NaHCO 3 , then with water to neutrality, dried over Na 2 SO 4 , the solvent is evaporated off and the residue is purified on a silica gel column (eluent CHCl 3 /MeOH 98:1.5), to obtain 6.42 g of ethyl 5-hydroxy-2- (2-ethoxy)ethyloxy!-2-ethoxycarbonyl-pentanoate.
A solution of 1.77 g of the compound in 4 ml of pyridine is reacted with 2.5 g of p-toluenesulfonyl chloride to give 2.3 g of ethyl 5-p-toluenesulfonyloxy-2- (2-ethoxy)ethyloxy!-2-ethoxycarbonyl-pentanoate, which by reaction with LiBr in acetone, yields:
ethyl 5-bromo-2- (2-ethoxy)ethyloxyl!-2-ethoxycarbonyl-pentanoate.
A solution of 1 g of ethyl 5-bromo-2- (2-ethoxy)ethyloxy!-2-ethoxycarbonyl-pentanoate in 5 ml of EtOH, added with 0.8 g of thiourea, is refluxed for 4 hours, then cooled to separate a crystalline precipitate of S-(4,4-diethoxycarbonyl-4-(2(2-ethoxy)-ethoxy)butyl isothiouronium bromide.
EXAMPLE 15
Using, in the process of example 14, ethyl 2-(1-isopropylpiperidin-4-ylmethoxy)-malonate, the following compounds are obtained:
ethyl 5-hydroxy-2- 2-(1-isopropylpiperidin-4-ylmethoxy)!-2-ethoxycarbonyl-pentanoate;
ethyl 5-bromo-2- 2-(1-isopropylpiperidin-4-ylmethoxy)!-2-ethoxycarbonyl-pentanoate;
S-(4,4-diethoxycarbonyl-4- 2-(1-isopropylpiperidin-4-yl-methoxy)!-butyl isothiouronium bromide,
and by reaction with N-butylthiourea, S-(4,4-diethoxycarbonyl-4- 2-(1-isopropylpiperidin-4-ylmethoxy)!-butyl,N-butyl isothiouronium bromide.
EXAMPLE 16
A solution of 0.1 g of potassium tert-butylate in 6 ml of THF/EtOH 1:2 is added, under nitrogen atmosphere, with 0.1 g of 2-imidazolidinethione and 0.41 g of ethyl 5-bromo-2- 2-(1-isopropylpiperidin-4-ylmethoxy)!-2-ethoxycarbonyl-pentanoate. The mixture is refluxed for 2h, the solvent is evaporated off and the residue is partitioned between AcOEt and water. After the usual work up, the solvent is evaporated off and the residue is purified on a silica gel column, to obtain 0.32 g of ethyl 5-(4,5-dihydro-imidazol-2-yl-2-thio)-2- 2-(1-isopropylpiperidin-4-ylmethoxy)!-pentanoate.
Using as mercaptans: β-pyridyl-methyl-mercaptan and 3,4,5,6-tetrahydro-2-pyrimidinothiol, the following compounds are also obtained:
ethyl 5-(β-pyridyl-methylthio)-2- 2-(1-isopropylpiperidin-4-ylmethoxy)!-2-ethoxycarbonyl-pentanoate;
ethyl 5-(3,4,5,5-tetrahydro-pyrimidin-2-yl-thio)-2- 2-(1-isopropylpiperidin-4-ylmethoxy)!-2-ethoxycarbonyl-pentanoate;
ethyl 5-(4,5-dihydro-imidazol-2-yl-2-thio)-2- (2-ethoxy)ethyloxy!-2-ethoxycarbonyl-pentanoate;
ethyl 5-(β-pyridyl-methylthio)-2- (2-ethoxy)ethyloxy!-2-ethoxycarbonyl-pentanoate;
ethyl 5-(3,4,5,5-tetrahydro-pyrimidin-2-yl-thio)-2- (2-ethoxy)ethyloxy!-2-ethoxycarbonyl-pentanoate.
EXAMPLE 17
Using, in the process of example 14, ethyl 3-cyclohexyl-2-ethoxycarbonyl-propionate and 2-trityloxyethyl bromide, 4-cyclohexyl-2,2-diethoxycarbonyl-butan-1-ol is obtained and then by reaction in dichloromethane with triphenylphosphine and tetrabromomethane, 4-cyclohexyl-2,2-diethoxy-1-butyl-bromide. A solution of 0.1 g of potassium tert-butylate in 6 ml of THF/EtOH 1:2 is added with 0.15 g of furfurylmercaptan and 0.38 g of 4-cyclohexyl-2,2-diethoxy-1-butyl bromide. The mixture is refluxed for 4 hours under nitrogen atmosphere, evaporated and partitioned between AcOEt and water. After the usual work up, the solvent is evaporated off and the residue is purified on a silica gel column, to obtain 0.34 g of ethyl 4-(fur-2-ylmethylthio)-2-ethoxycarbonyl-2-cyclohexylmethyl-butanoate.
A solution of 0.2 g of the compound in EtOH (6 ml), dimethylamine hydrochloride (0.06 g) and paraformaldehyde (0.045 g) is refluxed for 4 hours, the major part of the solvent is evaporated off, the residue is diluted with water (10 mi) and extracted with AcOEt. The organic phases are washed with 1×3 ml of water and then discarded. The aqueous phases are combined, alkalinized with potassium bicarbonate and re-extracted with AcOEt. The organic phases are combined to give, after the usual work up and purification of the residue on a silica gel column, 0.18 g of 4-(5-dimethylaminomethyl-fur-2-ylmethylthio)-2-ethoxycarbonyl-2-cyclohexylmethyl-butanoate.
EXAMPLE 18
Using, in the process of example 1, diallyl malonate, by reaction of the resulting allyl diazomalonate with morpholinylethanol and thiamorpholinylethanol, the following compounds are obtained:
allyl morpholinylethoxymalonate and allyl thiamorpholinylethoxymalonate, which are reacted according to the process of example 5 respectively with 2-benzyloxycarbonylaminoethyl bromide, 4-benzyloxycarbonylaminobutyl bromide, (S) 2-BOC-amino-propyl bromide and (S) 3-phenyl-2-BOC-amino-propyl bromide to obtain:
allyl 4-benzyloxycarbonylamino-2-(allyloxycarbonyl)-2-(morpholinyl-4-ethoxy)-butanoate;
allyl 4-benzyloxycarbonylamino-2-(allyloxycarbonyl)-2-(morpholinyl-4-ethoxy)-hexanoate;
allyl (S) 4-tert-butoxycarbonylamino-2-(allyloxycarbonyl)-2-(thiamorpholinyl-4-ethoxy)-pentanoate;
allyl (S) 5-phenyl-4-tert-butoxycarbonylamino-2-(allyloxycarbonyl)-2-(morpholinyl-4-ethoxy)-pentanoate and after cleavage of the Z and BOC protecting groups, the following compounds are obtained:
allyl 4-amino-2-(allyloxycarbonyl)-2-(morpholinyl-4-ethoxy)-butanoate;
allyl 4-amino-2-(allyloxycarbonyl)-2-(morpholinyl-4-ethoxy)-hexanoate;
allyl (S) 4-amino-2-(allyloxycarbonyl)-2-(thiamorpholinyl-4-ethoxy)-pentanoate;
allyl (S) 5-phenyl-4-amino-2-(allyloxycarbonyl)-2-(morpholinyl-4-ethoxy)-pentanoate.
EXAMPLE 19
Using, in the process of Example 9, allyl cyclohexylpropylmalonate, the following compound is obtained:
allyl 5-BOC-amino-2-allyloxycarbonyl-2- 3-cyclohexyl-propyl!-pentanoate: 1 HNMR (CDCl 3 , ppm): 4.53 (1H, bs NH); 3.11 (2H, m, NH--CH 2 --); 1.9-1.85 (4H, m, --CH 2 --C(<(CO 2 ) 2 )--CH 2 --); 1.7-1.6 1.5-1.3-1.3-1.1 (17 H complex system of m --NH--CH 2 --CH 2 --+ ##STR13## 1.45 (9H, s, (CH 3 ) 3 --OCONH); 1.25 (6H, t, --CO 2 --CH 2 --CH 3 ; J 7 Hz) which is converted into potassium 5-BOC-amino-2-carboxy-2- 3-cyclohexylpropyl!-pentanoate with potassium hexanoate and triphenylphosphine.
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Compounds of formula I: ##STR1## wherein R a , R b , Φ, B and R are as defined in the disclosure, have antagonistic activity on osteoclast hyper-reactivity.
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BACKGROUND OF THE INVENTION
[0001] The relevant background includes the fields of exhaust gas treatment systems and diagnostics therefore. As to the former field of endeavor, there have been a variety of exhaust gas treatment systems developed in the art to minimize emission of undesirable constituent components of engine exhaust gas. It is known to reduce NOx emissions using a selective catalytic reduction (SCR) system, a treatment device that includes a catalyst and a system that is operable to inject material such as ammonia (NH 3 ) into the exhaust gas feedstream ahead of the catalyst. The SCR catalyst is constructed so as to promote the reduction of NOx by NH 3 (or other reductant, such as aqueous urea which undergoes decomposition in the exhaust to produce NH 3 ). NH 3 or urea selectively combine with NOx to form N 2 and H 2 O in the presence of the SCR catalyst, as described generally in U.S. Patent Application Publication 2007/0271908 entitled “ENGINE EXHAUST EMISSION CONTROL SYSTEM PROVIDING ON-BOARD AMMONIA GENERATION”, the contents of which are incorporated by reference. For diesel engines, for example, selective catalytic reduction (SCR) of NOx with ammonia is perhaps the most selective and active reaction for the removal of NOx in the presence of excess oxygen. The NH 3 source must be periodically replenished and the injection of NH 3 into the SCR catalyst requires precise control. Overinjection may cause a release of NH 3 (“slip”) out of the tailpipe into the atmosphere, while underinjection may result in inadequate emissions reduction (i.e., inadequate NOx conversion to N 2 and H 2 O).
[0002] These systems have been amply demonstrated in the stationary catalytic applications. For mobile applications where it is generally not possible (or at least not desirable) to use ammonia directly, urea-water solutions have been proven to be suitable sources of ammonia in the exhaust gas stream. This has made SCR possible for a wide range of vehicle applications.
[0003] Increasingly stringent demands for low tail pipe emissions of NOx have been placed on heavy duty diesel powered vehicles. Liquid urea dosing systems with selective catalytic NOx reduction (SCR) technologies have been developed in the art that provide potentially viable solutions for meeting current and future diesel NOx emission standards around the world. Ammonia emissions may also be set by regulation or simply as a matter of quality. For example, proposed future European emission standards (e.g., EU 6) for NH 3 slip targets specify 10 ppm average and 30 ppm peak. However, the challenge described above remains, namely, that such treatment systems achieve maximum NOx reduction (i.e., at least meeting NOx emissions criteria) while at the same time maintaining acceptable NH 3 emissions, particularly over the service life of the treatment system.
[0004] In addition to the substantive emissions standards described above, vehicle-based engine and emission systems typically also require various self-monitoring diagnostics to ensure tailpipe emissions compliance. In this regards, U.S. federal and state on-board diagnostic regulations (e.g., OBDII) require that certain emission-related systems on the vehicle be monitored, and that a vehicle operator be notified if the system is not functioning in a predetermined manner. Automotive vehicle electronics therefore typically include a programmed diagnostic data manager or the like service configured to receive reports from diagnostic algorithms/circuits concerning the operational status of various components or systems and to set/reset various standardized diagnostic trouble codes (DTC) and/or otherwise generate an alert (e.g., MIL). The intent of such diagnostics is to inform the operator when performance of a component and/or system has degraded to a level where emissions performance may be affected and to provide information (e.g., via the DTC) to facilitate remediation.
[0005] Over the service life of the above-described exhaust treatment systems, various constituent components can wear, degrade or the like, possibly impairing overall performance. For example, degradation of either the SCR catalyst or the dosing system may impair the treatment system in meeting either or both of the NOx and NH 3 emission standards. Diagnostic methods to detect such conditions are described generally in U.S. Patent Application Publication 2010/0101214 entitled “DIAGNOSTIC METHODS FOR SELECTIVE CATALYTIC REDUCTION (SCR) EXHAUST TREATMENT SYSTEMS”, the contents of which are incorporated by reference. However, improvements are always desirable in any art.
BRIEF SUMMARY OF THE INVENTION
[0006] In a first aspect of the invention, a method is presented for fault identification of gas sensors. The method includes receiving a first output signal from a first gas sensor having an output that varies according to both the concentration of a first gas species in a gas mixture and a second gas species in the gas mixture. The method further includes receiving a second output signal from a second gas sensor having an output that varies according to both the concentration of the first gas species in a gas mixture and the second gas species in the gas mixture. The method further includes processing the first output signal and the second output signal in a diagnostic controller that implements a model of the first gas sensor and a model of the second gas sensor so as to identify a fault in the first gas sensor or the second gas sensor.
[0007] In a second aspect of the invention, a fault identification system for gas sensors includes a first gas sensor having an output that varies according to both the concentration of a first gas species in a gas mixture and a second gas species in the gas mixture. The system further includes a second gas sensor having an output that varies according to both the concentration of the first gas species in a gas mixture and the second gas species in the gas mixture. The system further includes a diagnostic controller that implements a model of the first gas sensor and a model of the second gas sensor so as to identify a fault in the first gas sensor or the second gas sensor.
[0008] Further aspects of the invention will become apparent from the detailed description provided hereafter. It is to be understood that the detailed description and examples provided are intended for purposes of illustration and are not intended to limit the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a diagrammatic and block diagram showing an exhaust treatment system in which the diagnostic methods of the invention may be practiced.
[0010] FIG. 2 is a graphical representation of the voltage across an NH 3 cell, the voltage across a NO X cell, and the voltage across an NH 3 —NO X cell, at selected partial pressures of NO X and of NH 3 in a sample gas.
[0011] FIG. 3 is a simplified electrical schematic depicting an interface between a gas sensor and an electrical apparatus.
[0012] FIG. 4 is a flow chart of a first diagnostic method incorporating aspects of the present invention.
[0013] FIG. 5 is a flow chart of a second diagnostic method incorporating aspects of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0014] Referring now to the drawings wherein like reference numerals are used to identify identical components in the various views, FIG. 1 is a diagrammatic and block diagram showing an exemplary diesel cycle internal combustion engine 10 whose combustion exhaust gas 12 is fed to an exhaust gas treatment system 14 . The exhaust gas is represented as a stream flowing through the exhaust gas treatment system 14 and is shown as a series of arrows designated 12 EO (engine out), 12 1 , 12 2 , 12 3 and 12 TP (tail pipe). It should be understood that while the invention will be described in connection with an automotive vehicle (i.e., mobile) embodiment, the invention may find useful application in stationary applications as well. In addition, embodiments of the invention may be used in heavy-duty applications (e.g., highway tractors, trucks and the like) as well as light-duty applications (e.g., passenger cars). Moreover, embodiments of the invention may find further useful application in various types of internal combustion engines, such as compression-ignition (e.g., diesel) engines as well as spark-ignition engines.
[0015] In the illustrative embodiment, the engine 10 may be a turbocharged diesel engine. In a constructed embodiment, the engine 10 comprised a conventional 6.6-liter, 8-cylinder turbocharged diesel engine commercially available under the DuraMax trade designation. It should be understood this is exemplary only.
[0016] FIG. 1 also shows an engine control unit (ECU) 16 configured to control the operation of the engine 10 . The ECU 16 may comprise conventional apparatus known generally in the art for such purpose. Generally, the ECU 16 may include at least one microprocessor or other processing unit, associated memory devices such as read only memory (ROM) and random access memory (RAM), a timing clock, input devices for monitoring input from external analog and digital devices and controlling output devices. The ECU 16 is operable to monitor engine operating conditions and other inputs (e.g., operator inputs) using the plurality of sensors and input mechanisms, and control engine operations with the plurality of output systems and actuators, using pre-established algorithms and calibrations that integrate information from monitored conditions and inputs. It should be understood that many of the conventional sensors employed in an engine system have been omitted for clarity. The ECU 16 may be configured to calculate an exhaust mass air flow (MAF) parameter 20 indicative of the mass air flow exiting engine 10 .
[0017] The software algorithms and calibrations which are executed in the ECU 16 may generally comprise conventional strategies known to those of ordinary skill in the art. Overall, in response to the various inputs, the ECU 16 develops the necessary outputs to control the fueling (fuel injector opening, duration and closing) and other aspects of engine operation, all as known in the art.
[0018] In addition to the control of the engine 10 , the ECU 16 is also typically configured to perform various diagnostics. For this purpose, the ECU 16 may be configured to include a diagnostic data manager or the like, a higher level service arranged to manage the reports received from various lower level diagnostic routines/circuits, and set or reset diagnostic trouble code(s)/service codes, as well as activate or extinguish various alerts, all as known generally in the art. For example only, such a diagnostic data manager may be pre-configured such that certain non-continuous monitoring diagnostics require that such diagnostic fail twice before a diagnostic trouble code (DTC) is set and a malfunction indicator lamp (MIL) is illuminated. As shown in FIG. 1 , the ECU 16 may be configured to set a corresponding diagnostic trouble code (DTC) 24 and/or generate an operator alert, such an illumination of a MIL 26 . Although not shown, in one embodiment, the ECU 16 may be configured so as to allow interrogation (e.g., by a skilled technician) for retrieval of such set DTCs. Generally, the process of storing diagnostic trouble codes and subsequent interrogation and retrieval is well known to one skilled in the art and will not be described in any further detailed.
[0019] With continued reference to FIG. 1 , the exhaust gas treatment system 14 may include a diesel oxidation catalyst (DOC) 28 , a diesel particulate filter (DPF) 30 , a dosing subsystem 32 including at least (i) a reductant (e.g., urea-water solution) storage tank 34 and (ii) a dosing unit 36 , and a selective catalytic reduction (SCR) catalyst 38 . In addition, FIG. 1 shows various sensors disposed in and/or used by the treatment system 14 . These include a DOC inlet temperature sensor 39 configured to generate a DOC inlet temperature signal 41 (T DOC-IN ), a NOx sensor 40 configured to generate a NOx signal 42 (NOx) indicative of a sensed NOx concentration, a first exhaust gas temperature sensor 44 , located at the inlet of the SCR catalyst 38 , configured to generate a first temperature signal 46 (T IN ), an optional second exhaust gas temperature sensor 48 configured to generate a second temperature signal 50 (T OUT ), a first pressure sensor 52 configured to generate a first pressure signal 54 (P IN ), a second pressure sensor 56 configured to generate a second pressure signal 58 (P OUT ), and an ammonia (NH 3 ) concentration sensor 60 configured to generate an ammonia concentration signal 62 indicative of the sensed NH 3 concentration. In many commercial vehicles, a NOx sensor 64 is provided for generating a second NOx signal 66 indicative of the NOx concentration exiting the tail pipe. However, such is shown for completeness only.
[0020] The DOC 28 and the DPF 30 may comprise conventional components to perform their known functions.
[0021] The dosing subsystem 32 is responsive to an NH 3 Request signal produced by a dosing control 80 and configured to deliver a NOx reducing agent at an injection node 68 , which is introduced in the exhaust gas stream in accurate, controlled doses 70 (e.g., mass per unit time). The reducing agent (“reductant”) may be, in general, (1) NH 3 gas or (2) a urea-water solution containing a predetermined known concentration of urea. The dosing unit 32 is shown in block form for clarity and may comprise a number of sub-parts, including but not limited to a fluid delivery mechanism, which may include an integral pump or other source of pressurized transport of the urea-water solution from the storage tank, a fluid regulation mechanism, such as an electronically controlled injector, nozzle or the like (at node 68 ), and a programmed dosing control unit. The dosing subsystem 32 may take various forms known in the art and may comprise commercially available components.
[0022] The SCR catalyst 38 is configured to provide a mechanism to promote a selective reduction reaction between NOx, on the one hand, and a reductant such as ammonia gas NH 3 (or aqueous urea, which decomposes into ammonia, NH 3 ) on the other hand. The result of such a selective reduction is, as described above in the Background, N 2 and H 2 O. In general, the chemistry involved is well documented in the literature, well understood to those of ordinary skill in the art, and thus will not be elaborated upon in any greater detail. In one embodiment, the SCR catalyst 38 may comprise copper zeolite (Cu-zeolite) material, although other materials are known. See, for example, U.S. Pat. No. 6,576,587 entitled “HIGH SURFACE AREA LEAN NOx CATALYST” issued to Labarge et al., and U.S. Pat. No. 7,240,484 entitled “EXHAUST TREATMENT SYSTEMS AND METHODS FOR USING THE SAME” issued to Li et al., both owned by the common assignee of the present invention, and both hereby incorporated by reference in their entirety. In addition, as shown, the SCR catalyst 38 may be of multi-brick construction, including a plurality of individual bricks 38 1 , 38 2 wherein each “brick” may be substantially disc-shaped. The “bricks” may be housed in a suitable enclosure, as known.
[0023] The NOx concentration sensor 40 is located upstream of the injection node 68 . The NOx sensor 40 is so located so as to avoid possible interference in the NOx sensing function due to the presence of NH 3 gas. The NOx sensor 40 , however, may alternatively be located further upstream, between the DOC 28 and the DPF 30 , or upstream of the DOC 28 . In addition, the exhaust temperature is often referred to herein, and for such purpose, the temperature reading from the SCR inlet temperature sensor 44 (T IN ) may be used.
[0024] The NH 3 sensor 60 may be located, in certain embodiments, at a mid-brick position, as shown in solid line (i.e., located anywhere downstream of the inlet of the SCR catalyst 38 and upstream of the outlet of the SCR catalyst 38 ). As illustrated, the NH 3 sensor 60 may be located at approximately the center position. The mid-brick positioning is significant. The sensed ammonia concentration level in this arrangement, even during nominal operation, is at a small yet detectable level of mid-brick NH 3 slip, where the downstream NOx conversion with this detectable NH 3 can be assumed in the presence of the rear brick, even further reducing NH 3 concentration levels at the tail pipe to within acceptable levels. Alternatively, in certain embodiments, the NH 3 sensor 60 may be located at the outlet of the SCR catalyst 38 . The remainder of the sensors shown in FIG. 1 may comprise conventional components and be configured to perform in a conventional manner known to those of ordinary skill in the art.
[0025] The dosing control 80 is configured to generate the NH 3 Request signal that is sent to the dosing unit 36 , which represents the command for a specified amount (e.g., mass rate) of reductant to be delivered to the exhaust gas stream. The dosing control 80 includes a plurality of inputs and outputs, designated 18 , for interface with various sensors, other control units, etc., as described herein. Although the dosing control 80 is shown as a separate block, it should be understood that depending on the particular arrangement, the functionality of (the dosing control 80 may be implemented in a separate controller, incorporated into the ECU 16 , or incorporated, in whole or in part, in other control units already existing in the system (e.g., the dosing unit). Further, the dosing control 80 may be configured to perform not only control functions described herein but perform the various diagnostics also described herein as well. For such purpose, the dosing control 80 may include conventional processing apparatus known in the art, capable of executing pre-programmed instructions stored in an associated memory, all performing in accordance with the functionality described herein. That is, it is contemplated that the control and diagnostic processes described herein will be programmed in a preferred embodiment, with the resulting software code being stored in the associated memory. Implementation of the invention, in software, in view of the foregoing enabling description, would require no more than routine application of programming skills by one of ordinary skill in the art. Such a control may further be of the type having both ROM and RAM, a combination of non-volatile and volatile (modifiable) memory so that the software can be stored and yet allow storage and processing of dynamically produced data and/or signals.
[0026] The ammonia (NH 3 ) concentration sensor 60 may comprise a gas sensor as described generally in U.S. Patent Application Publication 2010/0032292 entitled “AMMONIA GAS SENSOR”, the contents of which are incorporated by reference. This sensor includes a first electrode material that is sensitive to an NH 3 concentration in the sensed gas but which is also vulnerable to cross-interference from NO 2 concentration in the sensed gas. A second electrode material is also provided that has an electrochemical sensitivity to NO 2 that is greater than its sensitivity to NH 3 or NO. The disclosure of Patent Application Publication 2010/0032292 details how signals from the two sensor electrode materials can be processed to provide an improved determination of NH 3 concentration. While the details of this disclosure will not be repeated here, it is useful to discuss the characteristics of the disclosed sensor electrode materials as an aid to appreciating aspects of the present invention.
[0027] Referring to FIG. 2 , a graphical representation 100 of the voltage outputs of a gas sensor is shown. The tested sensor had a BiVO 4 (5% MgO) NH 3 electrode, a TbMg 0.2 Cr 0.8 O 3 NO x electrode, and a Pt reference electrode. The sensor was operated at 560° C. The graphical representation includes a line representing the voltage (line 102 ) across the NH 3 sensing cell, a line representing the voltage (line 104 ) across the NO x sensing cell, and a line 106 representing the voltage across the NH 3 —NO x cell. The graphical representation 100 further includes four intervals representing NO 2 and NO concentrations: a first interval 108 where NO and NO 2 concentrations are 0 ppm (parts per million), a second interval 110 where NO concentration is 400 ppm and NO 2 concentration is 0 ppm, a third interval 112 where NO concentration is 200 ppm and NO 2 concentration is 200 ppm, and a fourth interval 114 where NO concentration is 0 ppm and NO 2 concentration is 400 ppm.
[0028] Each of the intervals 108 , 110 , 112 , 114 , include seven subsections representing NH 3 concentrations: a first subsection 116 where the NH 3 concentration is 100 ppm, a second subsection 118 where the NH 3 concentration is 50 ppm, a third subsection 120 where the NH 3 concentration is 25 ppm, a fourth subsection 122 where the NH 3 concentration is 10 ppm, a fifth subsection 124 where the NH 3 concentration is 5 ppm, a sixth subjection 126 where the NH 3 concentration is 2.5 ppm, and a seventh subjection 128 where the NH 3 concentration is 0 ppm. The remaining gas is composed of 10% O 2 , 1.5% of H 2 O and balanced by N 2 .
[0029] As shown in FIG. 2 , the line 102 representing the voltage across the NH 3 sensing cell is identical in intervals 108 and 110 where NO 2 is excluded from the gas being measured. However, the voltage across the NH 3 sensing cell represented by line 102 has a lower value (higher absolute value) in section 112 and 114 where NO 2 is present, thereby demonstrating the cross-interference effect of NO 2 on the NH 3 sensing cell.
[0030] Similarly, FIG. 2 also shows the cross-interference effect of NH 3 on the NO 2 sensing cell. Within any of the intervals 110 , 112 , 114 where NOx is present, the line 104 representing the voltage across the NOx sensing cell shows the influence of NH 3 concentration as the NH 3 concentration is varied from 100 ppm in subsection 116 of each interval to 0 ppm in subsection 128 of each interval.
[0031] The system and method disclosed herein take advantage of these mutual cross-interference effects to enable improved fault determination of the sensors. In an aspect of the system and method of the invention, the output signals produced by each of the two electrode materials are compared to determine if the effects produced by concentrations of NH 3 and NO 2 are consistent with the known cross-interference characteristics of the electrode materials. These aspects will be further described by way examples to follow.
[0032] FIG. 3 is a schematic diagram that depicts how the sensors may be connected in a system. In FIG. 3 , a sensor assembly is depicted generally as 160 , with the sensor assembly 160 including a first sensing cell 162 , a second sensing cell 166 , and a heater 170 thermally coupled to both sensing cells 162 and 166 . The sensing cell 162 produces a voltage EMF 1 that is related to the concentrations of gas species, and the sensing cell 166 produces a voltage EMF 2 that is related to the concentrations of gas species. The sensing cells 162 and 166 may be considered to include associated source impedances 164 and 168 respectively. Both the emf EMF 1 , EMF 2 and the source impedance 164 , 168 of a sensing cell 162 , 166 are influenced by the temperature of the sensing cell, and the heater 170 is controlled to maintain the temperature of the sensing cell 162 , 166 at a desired level. The sensor 160 may also include a temperature sensor (not shown) to sense a temperature produce by the heater 170 . It will be appreciated that, while FIG. 3 shows two emf cells in thermal communication with a single heater, the emf cells may be contained in separate physical embodiments, and each emf cell may have its own associated heater.
[0033] Still referring to FIG. 3 , the sensor 160 is electrically connected to an interface apparatus generally depicted as 180 . Apparatus 180 is depicted as including a measurement means 186 to measure the voltages produced by the sensing cells 162 , 166 . Apparatus 180 also includes a heater control means in electrical communication with the heater 170 to maintain the heater 170 at a desired temperature. Additionally, apparatus 180 is shown as containing a first pull-up resistor 182 connected from the output of the first sensing cell 162 to a voltage source V+, and a second pull-up resistor 184 connected from the output of the second sensing cell 166 to a voltage source V+. Reference will be made to FIG. 3 in the discussion of the following examples.
EXAMPLE 1
Sensor Rationality Test during Reductant Dosing
[0034] A first diagnostic method may be used during intervals when reductant is being added to the exhaust gas, e.g. when a urea solution is being injected. During such a time interval, the gas to which the exhaust sensor is exposed will have a relatively high concentration of NH 3 . As illustrated in FIG. 2 , both the NH 3 sensing cell (whose output is shown in trace 102 ) and the NOx sensing cell (whose output is shown in trace 104 ) are influenced by the concentration of NH 3 in the sensed gas. In the discussion that follows, the output of the NH 3 sensing cell will be denoted as EMF 1 , and the output of the NOx sensing cell will be denoted as EMF 2 .
[0035] Referring to FIG. 4 , the first diagnostic method 200 includes the step 205 of receiving EMF 1 and EMF 2 values from the NH 3 sensing cell and the NOx sensing cell respectively. In decision step 210 , the measured values of EMF 1 and EMF 2 received in step 205 are each compared to a predetermined range for the respective sensor. As will be appreciated from FIG. 3 , a value of EMF 1 measured during reductant dosing that is too low may be an indication of a short circuit across or other damage to sensing cell 162 . A value of EMF 2 measured during reductant dosing that is too low may be an indication of a short circuit across or other damage to sensing cell 166 . A measured value of EMF 1 or EMF 2 that is too high may be the result of a high impedance in sensing cell 162 or 166 as may be caused by a damaged sensor or improper operation of heater 170 or heater control 188 . A high measured value of EMF 1 may also be the result of an open conductor or connector in the circuit between measurement means 186 and sensing cell 162 , resulting in measurement means 186 receiving V+ through pull-up resistor 182 . A high measured value of EMF 2 may also be the result of an open conductor or connector in the circuit between measurement means 186 and sensing cell 166 , resulting in measurement means 186 receiving V+ through pull-up resistor 184 . If EMF 1 and/or EMF 2 stay at a constant value in excess of a predetermined amount of time, this may be an indication that the sensing cells 162 and/or 166 may be isolated from the exhaust gas, for example because of a sensor shield or coating layer being plugged by soot or by chemicals that are poisonous to the sensor. If the result of decision step 220 is that the measured value of EMF 1 and/or EMF 2 is outside a predetermined range, the process flow proceeds to step 240 .
[0036] In step 215 , the concentration of NH 3 is determined from the received values of EMF 1 and EMF 2 . The concentration of NH 3 may be determined based on a calculation involving a predetermined characteristic equation relating EMF 1 and EMF 2 to NH 3 concentration. An exemplary characteristic equation is disclosed in U.S. patent application Ser. No. 12/974,266 titled “METHOD AND DEVICE FOR CHARACTERIZATION AND SENSING OF EXHAUST GAS AND CONTROL OF ENGINES AND COMPONENTS FOR AFTERTREATMENT OF EXHAUST GASES” filed Dec. 21, 2010, the contents of which are hereby incorporated by reference. Alternatively, the concentration of NH 3 may be determined in step 215 by means of a lookup table that uses EMF 1 and EMF 2 as inputs.
[0037] In step 220 , the concentration of NH 3 that was determined in step 215 is used to determine a predicted EMF 2 value, based on a predetermined relationship describing the sensitivity of the NOx sensing cell to NH 3 concentration. The predicted value of EMF 2 may be determined based on a calculation based on a predetermined mathematical model for the NOx sensing cell that relates EMF 2 to NH 3 concentration. Alternatively, the predicted value of EMF 2 may be determined by means of a table look-up using NH 3 concentration as an input.
[0038] Still referring to FIG. 4 , the method includes a further sequence of decision steps 225 , 230 , and 235 . Step 225 compares the predicted value of EMF 2 based on the NH 3 concentration to a predetermined range. If the predicted value of EMF 2 is outside of the predetermined range, this is indicative of degradation of one or both of sensing cells 162 , 166 , such as may result from cell aging or poisoning. If the result of decision step 225 is that the predicted value of EMF 2 is outside a predetermined range, the process flow proceeds to step 240 .
[0039] If the test in step 225 does not indicate a fault condition, the method continues to step 230 . In this step, the difference (predicted value of EMF 2 —measured value of EMF 2 ) is compared to a predetermined threshold. If this difference is below the threshold, this may be an indication of a malfunction in the NH 3 sensing cell, resulting in an underestimation of NH 3 concentration in step 210 and a corresponding underestimation of the predicted value of EMF 2 in step 215 . If a malfunction is indicated, the method proceeds to step 240 .
[0040] If the test in step 230 does not indicate a fault condition, the method continues to step 235 . In this step, the difference (predicted value of EMF 2 —measured value of EMF 2 ) is compared to a predetermined threshold. If the difference is above this threshold, this may be an indication of a malfunction in the NOx sensing cell, resulting in the cell not exhibiting the cross-influence effect to NH 3 that is known to be a characteristic of the NOx sensing cell. If a malfunction is indicated by step 230 , the method proceeds to step 240 . If no malfunction is detected, the diagnostic routine 200 is exited.
[0041] Step 240 in method 200 is entered upon detection of a fault condition by any of the decision steps 220 , 225 , 230 , or 235 . Step 240 indicates the appropriate fault condition. The response of the system to a fault condition may depend on the nature of the fault condition. For example, a diagnostic trouble code (DTC) may be set and/or a malfunction indicator lamp (MIL) may be illuminated. Depending on the nature of the fault condition, control of the engine or exhaust treatment systems may be changed to a failsafe backup mode to preserve driveability and/or to prevent damage to other components.
EXAMPLE 2
Sensor Rationality Test during Intervals of No Reductant Dosing
[0042] A second diagnostic method may be executed during times when no reductant is being added to the exhaust gas. During such a time interval, the gas to which the exhaust sensor is exposed will contain a substantial quantity of NO 2 which may be predetermined by engine mapping or by direct measurement, and will contain essentially zero NH 3 . Again, in the discussion that follows, the output of the NH 3 sensing cell will be denoted as EMF 1 , and the output of the NOx sensing cell will be denoted as EMF 2 .
[0043] Referring again to FIG. 2 , it will be appreciated that under conditions of negligible NH 3 (as seen in subsections 128 in intervals 108 , 110 , 112 , and 114 ), EMF 1 (shown as line 102 ) shows appreciable sensitivity to NO 2 concentration. Recall that intervals 108 and 110 represent conditions in which NO 2 is excluded from the gas being measured, interval 112 represents 200 ppm NO 2 , and interval 114 represents 400 ppm NO 2 . An aspect of the present invention takes advantage of this cross-interference effect of NO 2 on the NH 3 sensing cell at low NH 3 levels to provide additional diagnostic information.
[0044] Referring to FIG. 5 , the second diagnostic method 300 includes the step 305 of receiving EMF 1 and EMF 2 values from the NH 3 sensing cell and the NOx sensing cell respectively.
[0045] In step 315 , predicted values of EMF 1 and EMF 2 are determined. The determination of predicted values of EMF 1 and EMF 2 may be based on predetermined engine mapping information relating the levels of NO and NO 2 in the exhaust to the engine operating conditions. Alternately, predicted values of EMF 1 and EMF 2 may be determined based on measured NOx levels from another sensor such as, for example, sensor 40 in FIG. 1 . The determination of predicted values of EMF 1 and EMF 2 may further be based on predetermined sensor characterization relating EMF 1 and EMF 2 to levels of NO and NO 2 in the exhaust. The determination of predicted values of EMF 1 and EMF 2 may be accomplished by means of look-up tables, calculations utilizing equations, or a combination thereof. Alternatively, the measured values of EMF 1 and EMF 2 may be utilized to calculate NO and NO 2 (NOx) based on a predetermined sensor model. The calculated NO and NO 2 (NOx) may be compared with predicted values of NO and NO 2 NOX) based on predetermined engine mapping, or with another NOx sensor such as sensor 40 .
[0046] Step 320 in method 300 compares the predicted value of EMF 1 determined in step 315 to the measured value of EMF 1 received in step 305 . If the difference between the predicted and measured values is outside of a predetermined range, this is indicative of a fault condition. For example, a measured value of EMF 1 that is significantly less than the predicted value of EMF 1 may indicate a short circuit across or other damage to sensing cell 162 . A lower than predicted value of EMF 1 may also result from thermal damage (meltdown) or chemical poisoning of sensing cell 162 .
[0047] A measured value of EMF 1 that is significantly greater than the predicted value of EMF 1 may be indicative of a high impedance in sensing cell 162 as may be caused by a damaged sensing cell 162 or improper operation of heater 170 or heater control 188 . A higher than predicted value of EMF 1 may also be the result of an open conductor or connector in the circuit between measurement means 186 and sensing cell 162 , resulting in measurement means 186 receiving V+ through pull-up resistor 182 . If the result of decision step 320 is that the measured value of EMF 1 differs from the predicted value of EMF 1 in excess of a predetermined amount, the process flow proceeds to step 340 .
[0048] If the test of EMF 1 in step 320 does not indicate a fault condition, step 325 performs a similar test on EMF 2 by comparing the predicted value of EMF 2 determined in step 315 to the measured value of EMF 2 received in step 305 . If the difference between the predicted and measured values is outside of a predetermined range, this is indicative of a fault condition. For example, a measured value of EMF 2 that is significantly less than the predicted value of EMF 2 may indicate a short circuit across or other damage to sensing cell 166 . A lower than predicted value of EMF 2 may also result from thermal damage (meltdown) or chemical poisoning of sensing cell 166 .
[0049] A measured value of EMF 2 that is significantly greater than the predicted value of EMF 2 may be indicative of a high impedance in sensing cell 166 as may be caused by a damaged sensing cell 166 or improper operation of heater 170 or heater control 188 . A higher than predicted value of EMF 2 may also be the result of an open conductor or connector in the circuit between measurement means 186 and sensing cell 166 , resulting in measurement means 186 receiving V+ through pull-up resistor 184 . If the result of decision step 325 is that the measured value of EMF 1 differs from the predicted value of EMF 1 in excess of a predetermined amount, the process flow proceeds to step 340 . If no malfunction is detected, the diagnostic routine 300 is exited
[0050] Step 340 in method 300 is entered upon detection of a fault condition by either of the decision steps 320 or 325 . Step 340 indicates the appropriate fault condition. The response of the system to a fault condition may depend on the nature of the fault condition. For example, a diagnostic trouble code (DTC) may be set and/or a malfunction indicator lamp (MIL) may be illuminated. Depending on the nature of the fault condition, control of the engine or exhaust treatment systems may be changed to a failsafe backup mode to preserve driveability and/or to prevent damage to other components.
[0051] In the foregoing examples, the indicated orders of the steps of the method are for illustration purposes only. One skilled in the art will appreciate that certain steps may be performed in different orders without departing from the inventive concepts disclosed herein. While this invention has been described in terms of the embodiments thereof, it is not intended to be so limited, but rather only to the extent set forth in the claims that follow.
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A method for fault identification of gas sensors exposed to a gas mixture is disclosed for gas sensors having an output that depends on concentrations of two gas species in the gas mixture. The method includes receiving output signals from two such sensors, processing the output signals in a controller that implements a model of the sensors so as to identify a fault in the first gas sensor or the second gas sensor; and providing an indication of any identified faults.
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BACKGROUND OF THE INVENTION
The invention relates to a progressing cavity fluid motor for directly driving a drill bit. Motors of this kind based on the Moineau principle find application to a considerable extent in deep drilling as direct drive bits or so-called "bottom motors". In these situations they are provided with an upper junction end on the housing for a connection with the drilling pipe. The motor drives the drill bit or similar drilling tool by way of a flexible shaft connecting the motor with the drilling tool. In this type of motor the flushing medium (drilling mud) is pumped downwards under high pressure into the progressing cavity work space in the motor between a stator forming the housing and the rotor forming the shaft. On its helical path through the motor a part of the pressure energy of the drilling mud is converted into rotational energy for the shaft. The pressure drop inside such motors, depending on the constructional design and direct drive drilling carried out in practice, is in the order of 25 or 60 bars.
With the well-known fluid motors the stator is in the form of a helical female thread and has an inner lining of an elastic deformable material secured to the housing. Inner linings of this kind are expensive to manufacture. For a satisfactory operation of the motor it is important that the molded helical thread surface in the working space be in contact with sufficient amount of the male helical rotor surface to seal against leakage. However excess pressure between the molded stator surface and the rotor results in increased wear of the molded surface and the performance of the motor drops; the design value of the motor will not be achieved. The determining contact pressure for the molded surfaces for an acceptable sealing in the contact areas of such fluid motors is usually determined so as to be in excess of a minimum; in so doing the pressure of the flushing medium is taken into account in the work space of the motor which tends to separate the motor surfaces from one another. In addition to pressure one must consider the temperature conditions under which a motor has to operate. This means that for the achievement of optimum operating conditions for the motor the latter must be adjusted for the existing operating conditions in the drill hole within narrow limits. This requires not only an expensive multiplicity of motors but also a most exact prognostication or predetermination of the drilling operating conditions in order to be able to prepare a suitable motor construction design. If the actual operating conditions deviate from the former which were established for the motor design either a loss of efficiency or increase in wear will occur.
With the aid of differential load measurements the contact pressures for the molded surfaces can be determined only within a limited extent with the result that with the help of such motors the torque capable of being generated is limited. While one can get by with relatively low torques with a single threaded helical motor chamber. With larger torque motors the helical shaped surfaces have a kind of a multiple thread interlacing gearing, that is the shafts for example have nine helical gears and the housings have ten screw threads. Such multiple designs however are often not sufficient to produce the necessary torque, in which cases integral drive parts are introduced in which several motors are connected in series coaxially. Integral drive parts of this kind, however, are not only extraordinarily large but also extraordinarily expensive and indeed not only in manufacturing but also in maintenance.
THE PRIOR ART
Typical Moineau type motors are shown in U.S. Pat. Nos. 3,894,818 and 3,879,094. An older patent showing a Moineau type motor having pressure equalization on the stator element is shown in J. L. Lummus et al U.S. Pat. No. 3,443,482. A similar U.S. patent to Schlecht U.S. Pat. No. 3,435,772 shows a radially compressible stator element in a Moineau pump. Seinfeld U.S. Pat. No. 2,695,565 illustrates a Moineau pump or motor wherein a stationary flexible diaphragm surrounds the rotor and the diaphragm is expandible outwardly against the stator; the diaphragm does not rotate with the rotor.
SUMMARY OF THE INVENTION
The refinement according to the present invention makes it possible to adapt the controlling equipment pressure between the areas existing in contact between the helically shaped surfaces at the pressure and temperature conditions of the drilling mud for sealing action and thus provide that under all operating conditions on the one hand the desired sealing is obtained and on the other hand a minimum amount of wear occurs. This is preferably achieved by providing a rotor with a threaded surface which is formed of an elastically deformable sleeve supported by a carrier shaft. Means are provided for preventing rotary motion between the elastically deformable sleeve and the carrier shaft. Means are arranged for introducing a pressure medium inside of the elastically deformable sleeve to provide a presssure for expanding the sleeve radially outwardly, this pressure being greater than the fluid pressure existing in the working cavity between the facing surfaces of the male and female threads. In the preferred embodiment the fluid pressure behind the deformable sleeve is changed as a function of the working pressure in the drilling mud. The appearances of wear are, in so doing, directly equalized by means of the elastic expansion of the deformable sleeve. The deformation of the sleeve is very precise and uniform with a simultaneous assurance of an efficient torque transmission between the sleeve body and its carrier shaft over the length and circumference of the sleeve. The practicable accommodation during the operation is assured in connection therewith not only by a running of the motor under optimum working conditions but also relieves the necessity of having a variety of types of motors of various designs in order to be able to make allowances in each case for operating requirements. With significantly reduced construction size and correspondingly lower costs, moreover, essentially higher efficiencies are achieved since already with a design with a single threaded screw gearing of stator and rotor pressure differences between inlet and outlet of the work space in the order of magnitude of 120 bars, and more, at high volumetric efficiency are achievable. With introduction of the motor according to the invention under normal drilling conditions, the motor can be constructed with a nine threaded screw gearing in a length of about 1 meter. In so doing such a drive delivers an essentially higher torque than conventional motors which for normal drilling conditions have a construction length of about 3 to 4 meters. The molded rotor body sleeve forms a relatively simple wear part which is easily replaceable.
DETAILED DESCRIPTION
Reference should be had to the following detailed description in conjunction with the drawings in which several non-limiting examples of the invention are further illustrated.
FIG. 1 is a fragmentary logitudinal cross section through an initial design of a fluid motor according to the invention with a rotor reproduced partly in section and partly as a side view.
FIG. 2 is a section according to line 2--2 in FIG. 1 with various designs of the elastic sleeve on the carrier shaft above and below the medium plane.
FIG. 3 is a section illustrated similar to FIG. 2 of an altered second design.
FIG. 4 is an illustration similar to FIG. 1 of another design with two collective drive units arranged in tandem.
FIGS. 5 and 6 are sectional illustrations similar to FIG. 2 of various different expandible sleeves.
FIG. 7 is a detail of a reinforcing element of FIG. 6.
The fluid motor illustrated in FIGS. 1 and 2 for a deep drilling motor comprises in particular an outside cylindrical housing 1 of for example stainless steel which on its upper inlet end has a conical inner thread 2 for a screw connection with an outside threaded attachment 3 of a tubular part 4. The latter on its part is provided in the upper region with a conical inner thread 5 for screw connection with a threaded attachment 6 on the lower end which forms the lower end of a pipe line for deep drilling. On its lower outlet end the housing 1 has a conical inner thread 8 for a screw connection with an attachment 9 provided with an outside thread of a tubular part 10 which receives any well-known or appropriate bushing arrangement. The parts 1, 4, 7 and 10 are arranged coaxially to a common longitudinal central axis 11.
On its inner side the housing 1 presents a female helical shaped surface 12 which is formed from the material of the housing and can be provided with a corrosion inhibitor for wear minimizing as well with a suitable surface coating. The specific shape of the helical surface is defined by means of screw threads left or right handed. In the example illustrated the helical surface is formed by a ten threaded screw thread. The housing constitutes a stator in the design illustrated. In housing 1 there is arranged a helical rotor which is rotatable and radially displaceable to a limited extent. The rotor as a whole is designated as 13 and consists of a carrier shaft 14 of steel or the like and a sleeve 15 of elastomer, for example rubber of polyurethane. The latter can in a given case be reenforced with glass fibers, metal filaments for example steel wire or the like.
Various modifications of sleeve construction are discussed in connection with FIGS. 5, 6 and 7.
The sleeve 15 has on its outside a helical surface 16 whose shape is synchronized to engage helical surface 12 of the housing 1. In the example illustrated the sleeve surface is composed of helical shaped threads which correspond to a nine threaded screw thread. It is obvious that the number of threads can be selected to fit desired design requirements. In addition, it is obvious that instead of the single stage of the helical screw thread course a two, or more, stage motor can be provided. The helical surfaces 12 and 16 intermesh in a kind of a screw gearing and mutually define a work space 17 which, in multi-threaded rotor-stator design, comprise a corresponding number of helical thread-shaped progressing cavities which serve to drive the motor.
On its lower side the rotor 13 is connected by joint 18 to an intermediate shaft 19 (whose lower end is not illustrated) which in turn is supported by a universal joint (not shown) or the like on a coaxially rotatable part mounted with bearings to a shaft to which the drilling tool can be connected. The intermediate shaft 19 forms the only axial support for the rotor 13 and permits the latter the necessary eccentric wobble movement for the function in operation.
The sleeve 15 of elastic material is supported on the center shaft or carrier 14 and is radially limited and displaceable. The shaft 14 in connection therewith is provided, on and along its outer side, with ribs 20 or 21 arranged and distributed over the circumference. The sleeve 15 is provided with corresponding flutes 22 or 23 or its inner side, the two being mutually in locking contact. Such a spline linkage assures nevertheless radial displacement motions of the sleeve 15 occurring in relation to its carrier 14 while providing a constant, uniformly distributed torque transmission to the exclusion of relative distortion movements to each other as well as to the uncontrolled deformations in individual areas or zones of the sleeve 15. The side surfaces of each rib and flute run parallel with each other so that with radial displacement movements of the sleeve 15 the snug surface contact between the ribs and the flute side walls is retained.
FIG. 2 illustrates in its upper half a type model of ribs 20 and flutes 22 which have a spiral shaped pattern around the shaft axis 24. The pattern of the flutes 22 in the sleeve is, is in connection therewith, adapted to the pattern of the screw threads. The lower half FIG. 2 illustrates a design in which the ribs 21 and the flutes 23 have a smaller radial dimension and accordingly can be arranged in a screw thread pattern to the shaft axis 24 which is independent from the pattern of the screw threads. The screw thread pattern assures a uniform take up of axial forces occurring between the sleeve and the carrier which must be taken up in a conceivable systematic axial pattern of ribs and flutes through separate means.
On its upper and lower ends the sleeve 15 is attached to the carrier 14 in an appropriate way by an inwardly projecting shoulder 25 or 26 with which it grips from behind sealing radial frontal surfaces 27 or 28 of the carrier 14. The carrier 14 is provided with an axial central hole 29 which is constructed as a passage way hole. A valve (V) is provided in the lower area of the central hole 20 which is described even further below. From the central hole 20 radial connecting channels 30 branch out which open out into the pressure spaces 31 between the ribs 20 or 21. These pressure spaces 31 between the sleeve 15 and its carrier 14 extend over the axial length of the sleeve 15 and terminate on the shoulders 25 or 26 and provide a pressure space extending around the carrier 14.
Since the central hole 20 is in open connection with the inlet area of the drive, the sleeve 15 in operation is directed radially outward by pressure in the working medium (drilling mud). This deformation force endeavors to expand the outside helical surface 16 of sleeve 15 and forces it against the helical surface 12 in the housing 1. The open connection between the central hole 29 to the working medium on the inlet side of the drive is made in the example according to FIGS. 1 and 2 by way of a coaxial pipe connection part 32 which acts effectively providing a restrictor at the inlet. This restrictor is formed in the example illustrated by an annular body 33 attached in the tubular part 4 having a central nozzle channel 34 by way of whose inlet plane 35 the end of the pipe connection part 32 is moved up to its inlet opening 36. Accordingly a higher pressure prevails on the back side of the sleeve 15 than is present in the working medium in the working space 17.
If now, for the driving of a drilling tool, a flushing medium is pumped downward through the pipe line, then a transient pressure increase occurs in the direction of the arrow 37 to the inlet end of the housing 1. First of all, as a result of the restrictors 33, 34, the working medium subsequently passing through the restrictors suffers a pressure drop before entering the work space 17. As the fluid flows through space 17 it imparts a rotary motion to rotor 13. As a result of admission of fluid on the inside of the sleeve 15 with the pressure derived from the work medium above the restrictors the helical surfaces 12 and 16 are held pressed together. This pressure introduced by the work medium, continually guarantees a dependable seal, and reduces to a minimum the wear occurring; and indeed is independent of it. In connection therewith the sleeve 15 is continually in a stressed condition.
FIG. 3 shows a construction which corresponds in principle to that of FIGS. 1 and 2. For analogous construction parts thereof reference symbols are used only for similar parts by increasing the number by 100. In the difference in construction from FIGS. 1 and 2 the rotor 113 has the shape of a single threaded spiral with a corresponding spiral surface 116 which in each radial section has a circular cross section outline. This shape of the spiral surface 116 is appropriate to the spiral surface 112 in the housing 101 while maintaining the difference in the number of threads. The expansion of the sleeve 115 with a pressure derived from the work medium takes place in the ways already explained in FIGS. 1 and 2 or by a method further explained following in connection with FIG. 4. The valve (V) provided in the central passage hole 29 according to FIG. 1 has a ball valve 48 as a valve body. This ball valve 48 operates together with a valve seat which is formed by a conical reducer 49 of the central passage hole 20 to a coaxial continuation area 50 joining to the passage hole in the carrier 14. To the hole area 50 is connected coaxially a reduced hole area 51 once again in cross section which in the region of its sealed end is connected by way of radial channels 52 with the outlet side of the drive beneath the work space 17 FIG. 1.
In the hole area 50 a spiral pressure spring 53 is provided on which the ball valve 48 is supported on the upper side. The spiral pressure spring 53 is adjusted in such a way that the ball valve 48 only arrives in contact with it valve seat 49 if the pressure difference between upper side and lower side of the ball valve exceeds a desired predetermined amount. By this means the beginning of a closing of the central hole 29 can be made for a flow from the inlet to the outlet side of the drive dependent upon the building of a pressure difference. This is made possible after disconnecting the drive by means of stopping a downward pumping of flushing medium to draw up the drive together with the drilling tube line while the flushing medium in the drilling tube line can run down freely below. At the same time the presence of the valve (V) makes possible a lowering of the motor into a drill hole with flushing in an opposite direction.
FIG. 4 illustrates a construction corresponding to FIGS. 1 and 2 in which in place of a direct connection of the pressure space between sleeve 15 and carrier 14 with the work medium on the inlet side of the drive, the latter is preferably constructed as a sealed chamber and is filled with a separate pressure medium. A piston 38 which is impinged on by the work medium pressure acts as an equalizing piston and pressure transmitter to the separate pressure medium. This piston 38 is formed as a differential piston and has a piston part 30 with a larger surface and a piston part 40 with a smaller pressure surface; accordingly this piston forms a pressure multiplier. Instead of a piston a membrane can be used, not only in a pressure multiplying but also in a construction having a direct pressure derivation without multiplication.
The hole pocket 29 forms in its upper area a cylinder space 54 to which is joined a cylinder hole 55 having an enlarged diameter. Within the cylinder holes or spaces 54, 55 the differential pistons 38 interwork, the upper piston part 39 being contained in the cylinder hole 55 and the lower piston part 40 being contained in the cylinder hole 54. The upper side of the upper piston part 39 is turned in the direction of the arrow 37 to the flowing work medium and is impinged by the pressure from the latter on the basis of the presence of an inlet opening 58. This inlet opening 58 makes a connection to an upper cylinder chamber 57.
Below the upper piston part 39 in the cylinder hole 55 is a lower cylinder chamber 56. The cylinder chamber 56 is connected now by way of an axial connecting channel, as well as by way of any one connecting channels 59 radially adjoined to connecting channel 60 with the outlet side of the drive. Correspondingly a pressure prevails in cylinder chamber 56 which is equal in pressure to that in the working medium on the outlet side of the drive. Correspondingly the upper piston part 39 an essentially higher pressure difference is displayed which moreover is still dependent on pressure reduction in the drive and changes with the latter. This means that the pressure impingment of the form body in the sense of expansion is adjusted according to the performance of the drive, that is to each moment of delivered torque of the operation.
In place of the differential piston it is also conceivable to provide a piston without gradation in cases in which a pressure multiplication is not required. In addition it is conceivable in place of the piston to install a membrane. In place of a membrane or a membrane combination a bellows combination can also find application and indeed not only in refinement with but also in a refinement without multiplication.
FIG. 4 illustrates a drive which is constructed of two drive units which are connected in a series in so doing each drive unit corresponds in the basic construction described above.
The two rotors 13 of the drive units are jointed beneath each other by means of a kind of universal joint for assurance of synchronous rotational movements so that without this connection the radial displacements of the individual rotors inside their connected housings 1 are not prevented. For joining of the two housings 1 the latter are equipped in each case at their upper inlet ends with a conical attachment provided with outer threads 2' while they are provided on the outlet side unchanged ends with a conical inner thread 8.
The universal joint for the shaft connection consists in particular of an intermediate shaft 61 which on its upper and lower ends is provided in each case with a slightly convex shaped outer gearing 62 or 63. On the lower end of the rotor 13 of the upper drive unit a firmly attached clutch coupling box 64 is mounted to the shaft which has an inner gearing 65 below the salient area which with the upper slightly convex outer gearing 62 of the intermediate shaft 61 interacts. Also on the lower end of the shaft 13 of the lower drive unit such a clutch coupling box 64 is attached whose gearing 65 interacts with a slightly convexed outer gearing 62' to an intermediate shaft 19' which performs the function of the intermediate shaft 19 explained in connection with FIG. 1.
The clutch coupling boxes 64 have a radial flange area 66 which performs the function of the shoulder 26 of the sleeve 15 in construction according to FIG. 1 or 6. Correspondingly the flange 66 joins the pressure space 31 touching and sealing to the lower end of the sleeve 15 in so doing the flange 66 at the same time fulfills even the function of an axial pressure take up.
In place of the above shoulder 25 of the sleeve 15 according to FIG. 1 on each upper end of the rotor 13 a flange ring 67 is provided for the sealing of the pressure space 31 which performs the function of flange 66 at this spot.
The rotor 13 of the lower drive unit is provided on its upper end on its part with its firmly joined clutch coupling box 68 which in an upper broadened hole area is inserted in the shaft. This clutch coupling box 68 has an inner gearing 69 which is in contact with the slightly convex lower outer gearing 63 of the intermediate shaft 61. Connecting channels 70 are made through the clutch coupling box 68 making a connection between work medium in the outlet area to the drive unit and to the cylinder space 57 above the upper piston part 39 of the pressure transmission piston.
The gearing between the intermediate shaft 61 and the clutch coupling box 64, 68 can run in the work medium. In the construction illustrated however they run sealed in a bellows of an elastic pipe body or the like 71 and a space filled with lubricant in order to reduce wear.
Such a casing is also provided in the connection area between the clutch coupling box 64 and the intermediate shaft 19'.
The rotor 13 also of the above drive unit has on its upper end in each case a clutch coupling box 68 as was described previously, if it is planned to join the above drive unit illustrated in FIG. 4 on the upper side with additional drive units in a modular way. For the case that this is not provided, in place of the clutch coupling box 68 illustrated, another inserted construction part can be provided which takes over the additional function further described below of a bearing support.
In two or more drive units connected in series in the manner illustrated in FIG. 4 axial forces occur which can indeed be taken up basically jointly by a support as it was mentioned in connection with FIG. 1. For distribution of the axial forces and at the same time for specific axial location of the rotor 13, it is however advantageous to provide these rotors in each case with an axial bearing on the upper side of the drive units connected in series. In the construction according to FIG. 4 this axial bearing consists in particular of a support ring 72 screwed on between it and the housing 1 and defined in this way that on the under side two or more flexible guide rods 73 engage.
On their bottom ends these guide rods 73 are flexibly joined with an outside spacer 74 which correspondingly floats that is is suspended displaceable in a radial direction. This outer spacer 74 surrounds the upper end area of the carrier 14 and contains at least one axial bearing 75. In the type model illustrated two axial bearings are arranged over each other by which the lower inwards projecting shoulder of the spacer 74 is supported. The upper axial bearing 75 is overlapped by an outward projecting shoulder 76 of the clutch coupling box 68 so that the bearings 75 defined between the spacer 74 and the carrier 14 of the shaft 13 are supported. A corresponding bearing is also found on the upper end of the rotor 13 of the upper drive unit although there the representation on a schematic view of the guide rod 73 for the support of the spacer 74 is limited. The foregoing described axial bearings ensure the cited specific axial bearing of the shaft 13 of the drive units, in so doing length changes or axial displacements which result from temperature expansions and bearing wear inside the gearing between the intermediate shafts 61, 19' and the clutch coupling boxes interacting with the latter are taken up.
The axial bearings are illustrated in the working medium, they can however also be enclosed by a suitable medium and then operate wear protected in a special lubricant.
According to the performance of the drive or of a drive unit it can be necessary by way of the above mentioned sheathing of the elastomer material of the sleeve 15 to provide the sleeve 15 with reenforcement in order to transfer to the latter for take up of the loads in the bearing.
FIG. 5 shows (in the left-hand side) a first construction of a reenforcement or sheathing which consists of a metallic cylindrical tube bushing 77. On this tube bushing 77 is cemented or vulcanized on the outside of the sleeve 15' which offers in its turn a corresponding cylindrical inner surface and itself is not ribbed or fluted. The pressure space 31 for the take up of the pressure medium is correspondingly accomplished on the inner side of the tube bushing 77 which with pressure impingement together with the sleeve 15' performs a radial expansion movement. On its inner side the tube bushing 77 has welded on or in otherwise appropriate ways attached ribs 78 which interact with the flutes 79 in the carrier body 14. Between the bottoms of the flutes 79 and the inner side of the frontal surfaces of the ribs 78 are left slit shapes intermediate spaces 31 which by way of individual connecting channels not illustrated are connected with the pressure space 31 and form a component of this pressure space. The ribs 78 and flutes 79 preferably run screw threaded on the bases for the take up of axial forces. They can, however, also be arranged concentrically.
The improvement according to FIG. 5 assumes a significant expansion capability for the tube backing 77 which may not be accommodatable, in all cases, in the elastic region. The construction according to the right-hand side of FIG. 5 shows a reenforcement in the form of an inner lining 80 which is adjusted to the flute profile of the inner side of the sleeve 15. The inner lining 80 correspondingly has a nearly dentiform cross sectional profile. In this arrangement the sleeve 15 is cemented onto or vulcanized onto the inner lining 80. Also the inner lining 80 consists of metal, however, here an outwardly directed expansion deformation is not made possible by means of tangential expansion as in the construction according to the left side of FIG. 5 but rather by a bending deformation of the inner lining 80. In the flutes 22 covered by the inner lining 80 of the sleeve 15 the ribs 20 of the carrier body 14 interlock like that illustrated in principle in the upper half of FIG. 2 and in connection with it has been described.
While in the constructions according to FIG. 5 a direct contact between the elastomer material of the sleeve and the metallic material of the carrier 14 is completely eliminated, the construction illustrated in the right side of FIG. 6 provides that in the sleeve 15 a reenforcement 82 is imbedded which essentially follows in its cross section pattern form the helical surface 16 of the sleeve 15. The reenforcement 82 can have a corresponding corrugated spiral shape which extends in the sleeve continuously around the shaft over the length of it. The reenforcement can also be formed by a plurality of imbedded, corrugated ring bodies spaced along the sleeve. Finally it is also conceivable to construct the reenforcement 82 for example in the form of a perforated corrugated tube which is vulcanized on or cast on in the sleeve 15. Also constructions in the form of a hose of fabric, weave, pleat, string or the like are conceivable in which in addition to textile material glass fibers or metal filaments come into consideration for reenforcements of this kind.
The construction of the reenforcement according to the left side of FIG. 6 consists of metallic rings 83 whose approximate shape can be inferred in particular from FIG. 7 which illustrate in perspective representation a section of such a ring.
The rings 83 arranged radially spaced and superimposed imbedded in the elastomer material of the sleeve 15 and comprise the limited areas 84 and 85 by each other by which the regions 85 have a coaxial surface alignment to the axis of the regions 84 and a radial alignment. In the regions 84 flute shaped clearances 86 are provided bordering on the inner edge which are intended for a direct gearing contact with the ribs 21 of the carrier 14, as was already described above in connection with the lower half of FIG. 2. Correspondingly the main power transmission takes place in the peripheral direction of the ribs 21 on the regions 84 of the rings 83 from avoidance of a noteworthy power transmission by the ribs 21 on the elastomer material of the sleeve 15. The limited transmission area 87 situated between the areas 84, 85 of the rings in each case offers the possibility of an elastic deformation of the rings in the sense of an expansion if in the material for reenforcement of this kind glass fibers or metal filaments are taken into consideration.
While the invention was described as a motor for the direct drive of drill bits it is obvious that motors according to the invention are not limited to such a preferred application area but can be applied in other application areas in which analogous operating conditions are present. Also an application applying pumps under analogous conditions is conceivable. Also applications to temporary forms are conceivable in which housing and shaft revolve with a variable rate of speed even if rectified. A conceivable application case for this is for example the introduction of one of the described constructions as a direct drive drill bit on the lower end of a moving drill casing line turning on its part. In addition to the aforesaid applications described in detail as a direct drive drill bit the drive can also basically be employed for all rotary drive tasks as they are required in a given case in a drill hole or drill tube.
In a reversal of the type model illustrated it is also conceivable for special cases to allow the housing 1 to operate as a rotor and the shaft as a stator without fundamental change of the construction form illustrated in which case the bit or otherwise would be connected to a driving tool to the housing and the shaft after extension out over the housing with the bore rods or the like.
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A progressing cavity fluid motor for driving a drill bit for deep drilling tools is described. Such a motor is mounted on a drill string and is powered by a fluid such as drilling mud. The pump includes a housing, a stator with female helical threads within the housing and a rotor with male helical threads mounted inside of the stator. The drill bit is connected to the rotor. In the present invention the rotor has a threaded surface which is formed of an elastically deformable sleeve supported by a carrier shaft. The sleeve is mounted on the carrier shaft in such a manner as to prevent rotation between the two so that the sleeve drives the shaft by positive engagement between these two elements. Means are arranged for introducing a pressure inside of the elastically deformable sleeve for expanding the sleeve radially outwardly. This pressure is greater than the fluid pressure existing in the working cavity between the facing surfaces of the male and female threads and preferably changes as a function of the working pressure in the drilling mud.
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This application is a continuation of application Ser. No. 13/612,952, filed Sep. 13, 2012, now U.S. Pat. No. 8,462,552, which is a continuation of application Ser. No. 13/031,966, filed Feb. 22, 2011, now U.S. Pat. No. 8,345,478, which is a continuation of application Ser. No. 12/484,418, filed Jun. 15, 2009, now U.S. Pat. No. 7,898,859, which are hereby incorporated by reference in their entireties.
FIELD OF THE INVENTION
Embodiments described herein relate to flash memory devices and more particularly to flash memory devices having emerging non-volatile (NV) memory elements used therewith.
BACKGROUND
Memory can generally be characterized as either volatile or non-volatile. Volatile memory, for example, most types of random access memory (RAM), requires constant power to maintain stored information. Non-volatile memory does not require power to maintain stored information. Various types of non-volatile memories include read only memories (ROMs), erasable programmable read only memories (EPROMs), and electrically erasable programmable read only memories (EEPROMs).
Flash memory is a type of EEPROM that is programmed and erased in blocks as opposed to cells. A conventional flash memory device includes a plurality of memory cells, each cell is provided with a floating gate covered with an insulating layer. There is also a control gate which overlays the insulating layer. Below the floating gate is another insulating layer sandwiched between the floating gate and the cell substrate. This insulating layer is an oxide layer and is often referred to as the tunnel oxide. The substrate contains doped source and drain regions, with a channel region disposed between the source and drain regions. In a flash memory device, a charged floating gate represents one logic state, e.g., a logic value “0”, while a non-charged floating gate represents the opposite logic state e.g., a logic value “1”. The flash memory cell is programmed by placing the floating gate into one of these charged states. Charges may be injected or written on to the floating gate by any number of methods, including e.g., avalanche injection, channel injection, Fowler-Nordheim tunneling, and channel hot electron (CHE) injection. The floating gate may be discharged or erased by any number of methods including e.g., Fowler-Nordheim tunneling. This type of flash memory element is a transistor-based non-volatile memory element.
The “NAND” and “NOR” architectures are two common types of flash memory architectures. NAND flash memory has gained widespread popularity over NOR flash memory because it can pack a greater number of storage cells in a given area of silicon, providing NAND with density and cost advantages over other nonvolatile memory. A NAND flash memory device typically utilizes a NAND flash controller to write data to the NAND in a page-by-page fashion. An example NAND memory array 10 is illustrated in FIG. 1 . Pages 12 are typically grouped into blocks 14 , where a block is the smallest erasable unit of the NAND flash memory device. For example, and without limitation, a typical NAND flash memory device contains 2,112 bytes of memory per page 12 and 64 or 128 pages of memory are contained in a block 14 . FIG. 1 illustrates blocks 14 comprising 64 pages 12 . For a page 12 having 2,112 bytes in total, there is a 2,048-byte data area 16 and a 64-byte spare area 18 . The spare area 18 is typically used for error correction code (ECC), redundancy cells, and/or other software overhead functions. The smallest entity that can be programmed in the illustrated array 10 is a bit.
FIG. 2 illustrates a NAND flash memory device 110 having a memory array 120 and sense circuitry 130 connected to the memory array 120 by data lines, which are commonly referred to as bitlines (BL). The array 120 comprises typical transistor-based non-volatile flash memory elements. When data is to be written into the NAND memory array, the data is initially loaded into the sense circuitry 130 . Once the data is latched, a programming operation is used to write a page of data into one of the pages of memory cells in the memory array 120 . The sense circuitry 130 typically comprises volatile static or dynamic memory elements.
A simplified schematic of a portion of the sense circuitry 130 is illustrated in FIG. 3 . As can be seen, there is sense operation circuitry 132 comprising three n-channel MOSFET transistors 134 , 136 , 138 , a data latch 140 , cache latch 150 and additional n-channel MOSFET transistors 160 , 162 , 164 , 166 , 168 . The data latch 140 is illustrated as comprising cross-coupled inverters 142 , 144 . The cache latch 150 is illustrated as comprising cross-coupled inverters 152 , 154 . The inverters 142 , 144 , 152 , 154 may each consist of e.g., an n-channel CMOS transistor and a p-channel CMOS transistor configured such that their gates are coupled together and at least one source/drain node of the n-channel transistor is coupled to a source/drain node of the p-channel transistor. Thus, the data and cache latches 140 , 150 in the illustrated example are implemented as static memory elements, which would lose their contents if power were removed from the circuit 130 . Thus, a situation could arise where latched data could be lost if power to the array 110 ( FIG. 2 ) were lost before the latched data was copied into the NAND memory arrays. Accordingly, the inventor of the present application appreciated that it would be desirable to prevent latched information from being lost in the event of a power failure or similar condition.
Continuing with the FIG. 3 example, data Da, Db is input into the sense circuitry 130 through the cache latch 150 when a data load/output enable signal data_load/out_en, connected to the gates of transistors 166 , 168 , is activated. Typically, data Da is the complement of data Db, and vice versa. A data signal Data connected at the gate of transistor 160 couples the data latch 140 to the cache latch 150 . When the data signal Data is at a level that activates transistor 160 , latched data is transferred from the cache latch 150 to the data latch 140 . A verify enable signal, verify_en, is used to activate transistor 162 , which is connected to transistor 164 . The gate of transistor 164 is connected to the data latch 140 . The same node of transistor 160 that is connected to the data latch 140 is also connected to a node of transistor 138 within the sense operation circuitry 132 . A precharge enable signal, precharge_en, controls transistor 136 while a bitline sensing signal, blsn, controls transistor 134 . A node of transistor 134 is connected to a write multiplexer (wmux) where data-to-be written, dw, based on the input data, is sent to and eventually stored in a conventional non-volatile memory array, which utilizes transistor-based memory elements.
As can be seen from the illustrated example, many transistors are required to implement the sense circuitry 130 . It is desirable to reduce the circuitry used in sense circuitry 130 . It is also desirable to increase the speed of sense circuitry 130 .
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates an example NAND flash memory array.
FIG. 2 illustrates an example NAND flash memory device having a memory array and sense circuitry.
FIG. 3 illustrates a schematic view of the sense circuitry used in the array of FIG. 2 .
FIG. 4 illustrates an example flash memory device constructed in accordance with an embodiment described herein.
FIGS. 5 and 6 illustrate schematic views of example sense circuitry with emerging NV elements used in the array of FIG. 4 .
FIG. 7 illustrates an example flash memory device constructed in accordance with another embodiment described herein.
FIG. 8 illustrates an example flash memory module comprising an emerging NV cache constructed in accordance with an embodiment disclosed herein.
FIG. 9 illustrates example packaging of an emerging NV cache chip stacked with a flash memory chip constructed in accordance with an embodiment disclosed herein.
FIG. 10 shows a processor system incorporating at least one flash memory device constructed in accordance with an embodiment disclosed herein.
FIG. 11 shows a universal serial bus (USB) memory device incorporating at least one flash memory device constructed in accordance with an embodiment disclosed herein.
DETAILED DESCRIPTION
Embodiments described herein refer to emerging NV (non-volatile memory elements). As used herein, and in accordance with the general understanding of one skilled in the relevant memory art, “emerging NV memory elements” means a non-transistor-based, non-volatile memory element such as phase change random access memory (PCRAM), magnetoresistive random access memory (MRAM), resistive random access memory (RRAM), ferroelectric random access memory (FeRAM), spin-transfer-torque random access memory (STTRAM), nano-tube memory, and equivalent non-volatile memory elements.
Referring to the figures, where like reference numbers designate like elements, FIG. 4 illustrates an example NAND flash memory device 210 constructed in accordance with an embodiment described herein. The device 210 includes a memory array 120 and sense circuitry including an emerging NV memory circuit 230 connected to the memory array 120 by bitlines (BL). The array 120 comprises typical transistor-based non-volatile flash memory elements. As will be discussed below in more detail, the flash memory device 210 differs from the conventional device 110 ( FIG. 2 ) in that it includes emerging NV memory elements instead of the conventional cross-coupled inverters used in data and cache latches 140 , 150 ( FIG. 3 ). By replacing the latches with emerging NV memory elements, the illustrated embodiment can help prevent data loss during programming of the NAND memory array if power to the device 210 (or a device incorporating the device 210 ) is interrupted. In addition, in standby mode, power to the emerging memory could be cut off to reduce standby power consumption without loss of data. Due to their construction, the emerging NV memory elements are usually smaller than the conventional latches and could possibly be implemented in metal 1 and 2 layers of the flash memory device, giving them a smaller device footprint.
A simplified schematic of an example portion of the sense circuitry with emerging NV memory elements 230 is illustrated in FIG. 5 . As can be seen, there is sense operation circuitry 132 comprising three n-channel MOSFET transistors 134 , 136 , 138 , which is the same as the sense operation circuitry 130 used in the conventional NAND device 110 ( FIG. 3 ). In the illustrated embodiment, however, the cross-coupled inverters of data latch 140 and cache latch 150 are replaced with emerging NV memory circuits 240 , 250 . The first emerging NV memory circuit 240 is controlled by a first control signal (or signals) control 1 and the second emerging NV memory circuit 250 is controlled by a second control signal (or signals) control 2 .
Data Da, Db is input into the sense circuitry 230 through emerging NV memory circuit 250 when control signal control 2 is activated. Typically, data Da is the complement of data Db, and vice versa. A data signal Data connected at the gate of transistor 160 couples circuit 250 to circuit 240 . When the data signal Data is at a level that activates transistor 160 , the stored data is transferred from circuit 250 to circuit 240 , which is controlled by control signal control 1 . The same node of transistor 160 that is connected to circuit 240 is also connected to a node of transistor 138 within the sense operation circuitry 132 . A precharge enable signal, precharge_en, controls transistor 136 while a bitline sensing signal, blsn, controls transistor 134 . A node of transistor 134 is connected to a write multiplexer (wmux) where data-to-be written, dw, based on the input data, is sent to and eventually stored in a NAND memory array.
It should be appreciated that it may be desirable to reduce the number of emerging NV memory elements used in the sense circuitry 230 . FIG. 6 illustrates a simplified schematic for another example of sense circuitry 230 ′. Circuitry 230 ′ differs from circuitry 230 ( FIG. 5 ) in that only one emerging NV memory circuit 255 is used to store data Da, Db before it is programmed into a NAND memory array. In the illustrated embodiment, the emerging NV memory circuit 255 is controlled by a control signal (or signals) control. It should also be appreciated that the emerging NV memory elements could be used with latches to provide additional functionality to the circuitry 230 , 230 ′, if desired.
It should also be appreciated that the illustrated control signals and input data may vary from the illustrated embodiment depending upon the type of emerging NV memory element used in the actual implementation of a device, such as device 210 . That is, for example, a PCRAM memory element may require a different control signal than the control signal, used for an RRAM memory element. As such, the illustrated embodiments are not to be limited to the example number of control signals and data bits shown in FIGS. 5 and 6 .
It should be appreciated that other benefits may be obtained by using emerging NV memory elements in other areas of, and to implement other functions in, a conventional memory device. For example, as illustrated in FIG. 7 , one or more blocks of emerging NV memory elements 370 can be included within a device 310 that includes a conventional NAND array 120 . The NV blocks 370 can be used, for example, to achieve faster writes from an external source of data. As such, the blocks of emerging NV memory elements 370 can serve as a high speed interface to the external source of data. Once the data is within one of the blocks of emerging NV memory elements 370 , the data can be copied into other blocks 370 before it is stored in the NAND memory array 120 (either through the sense circuitry 330 as shown in FIG. 7 or without going through the sense circuitry 330 ). This way, the blocks 370 can also or alternatively serve as a high speed cache memory for the device 310 . It could be desirable to use as many blocks of emerging NV memory elements 370 as the application design will allow. Accordingly, the illustrated embodiment is not to be limited to the example number of blocks of emerging NV memory elements 370 shown in FIG. 7 .
It should be appreciated that better block management can be achieved by storing data in the blocks of emerging NV memory elements 370 prior to programming the NAND array 120 in the device 310 . That is, fragment fixing, error correction and other data and memory cleaning operations can be performed while the data is in the faster emerging NV blocks 370 . In addition, it is also possible to use some of the blocks 370 as redundant memory as part of the bad block management that is typically performed on flash memory devices. That is, the bad block management function of the flash memory device can replace bad blocks of memory elements in the NAND array 120 with a good block of emerging NV memory elements. The device 310 can be operated to map a bad NAND memory block to a block of emerging NV memory elements and then copy data (to be stored in the array 120 ) into the block of emerging NV memory elements.
It should also be appreciated that that emerging NV memory blocks could be used to initially store data so that required data adjustments can be performed before the data is stored in a NAND block. For example, there are times when an entire NAND block's data is needed to carry out adjustments to counter interference effects sometimes present in the NAND array. Once the adjustments are done in the emerging NV memory elements, then the data can be safely stored in the NAND block; thus, improving the NAND device's reliability.
FIG. 8 illustrates a memory module 400 having a conventional NAND flash memory device 410 and an emerging NV cache memory 420 housed on the same circuit board 402 . Bond wire connections 404 (or printed circuit board traces) may be placed along the sides of the flash memory device 410 die to connect it to the emerging NV cache memory device 420 . The module 400 also includes pins 406 serving as an interface to the conventional device 410 and for providing ground and power to the device 410 , and pins 408 serving as an interface to the emerging NV cache memory device 420 and for providing ground and power to the device 420 . It should be appreciated that the number of pins and connections shown in FIG. 8 is only an example number of pins and connections and that the actual implementation of the module 400 could have more or less pins and connections. In the illustrated embodiment, the emerging NV cache memory device 420 can serve as a high performance non-volatile cache for the flash device 410 , which provides the data loss prevention and other advantages described above. Although not shown, the circuit board 402 could also include a memory controller; in such a case, the module 400 /circuit board 402 , could be used as a cache for a cheaper storage device such e.g., as a hard drive.
FIG. 9 illustrates a memory chip package 500 comprising an encasement 502 having a cavity 504 where in an emerging NV cache 520 is stacked with a NAND flash memory device 510 . As with other embodiments, the emerging NV cache 520 can serve as a high performance non-volatile cache for the NAND flash device 510 , which could provide the data loss prevention and other advantages described above.
FIG. 10 illustrates a processor system 600 utilizing a memory device, e.g., a flash memory device 210 , 310 , 400 , 500 constructed in accordance with embodiments described above. That is, the memory device 210 , 310 , 400 , 500 is a NAND flash memory device incorporating one or more emerging NV memory elements as set described above. The system 600 may be a computer system, camera system, personal digital assistant (PDA), cellular telephone, smart telephone, a process control system or any system employing a processor and associated memory. The system 600 includes a central processing unit (CPU) 602 , e.g., a microprocessor, that communicates with the flash memory 210 , 310 , 400 , 500 and an I/O device 612 over a bus 610 . It must be noted that the bus 610 may be a series of buses and bridges commonly used in a processor system, but for convenience purposes only, the bus 610 has been illustrated as a single bus. A second I/O device 614 is illustrated, but is not necessary to practice the embodiments described above. The system 600 also includes random access memory device 616 and may include a read-only memory device (not shown), and peripheral devices such as a floppy disk drive 604 and a compact disk (CD) ROM drive 606 that also communicate with the CPU 602 over the bus 610 as is well known in the art.
FIG. 11 shows a universal serial bus (USB) memory device 700 incorporating at least one flash memory device 400 , 500 constructed in accordance with an embodiment disclosed herein. The device 700 includes a USB connector 702 electrically and mechanically connected to a printed circuit board 710 . The connector 702 allows the device 700 to be inserted within a USB port of a computer or other device to allow data to be exchanged between the device 700 and the computer, etc. Moreover, power for the device 700 will also come from the USB port. The printed circuit board 710 comprises a USB interface (I/F) chip 712 electrically connected to the USB connector 702 . The USB interface 712 is electrically connected to and communicates with a controller 714 . The controller 714 controls and communicates with the flash memory device 400 , 500 over a bus 720 . The controller 714 also controls a light emitting diode 718 , via the bus 720 . Typically, the light emitting diode 718 is controlled to blink when the flash memory device 400 , 500 is being accessed. FIG. 11 also illustrates an oscillator 716 , which is used as a clock for the device 700 .
It should be appreciated that, although the embodiments have been described as using NAND flash memory arrays, other types of non-volatile flash memory could be used to practice the embodiments. For example, NOR and AND type flash memory arrays could be used in any of the illustrated embodiments. It should also be appreciated that the emerging NV memory elements can also be used to store data that has been read out of the conventional memory cells. In addition, it should be appreciated that the emerging NV memory elements can be used to store trim and fuse information as well as diagnostic data (e.g., program time, erase time, cycling information, number of failed bits or blocks) that can be acquired through out the life of the NAND chip regarding its performance and reliability.
The above description and drawings illustrate various embodiments It should be appreciated that modifications, though presently unforeseeable, of these embodiments that can be made without departing from the spirit and scope of the claimed invention, which is defined by the following claims.
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Memory devices and methods of operating memory devices are provided, such as those that involve a memory architecture that replaces typical static and/or dynamic components with emerging non-volatile memory (NV) elements. The emerging NV memory elements can replace conventional latches, can serve as a high speed interface between a flash memory array and external devices and can also be used as high performance cache memory for a flash memory array.
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BACKGROUND OF THE INVENTION
1. Field of Invention
The present invention relates generally to a control method and system for a device to be connected to the internal combustion engine of a vehicle, especially an automobile, which supplies a reformed fuel to the internal combustion engine.
2. Description of the Prior Art
A partial oxidation method has been available for reforming a liquid fuel, but the reaction in this method being an exothermic one, causes heavy loss of the energy in the liquid fuel, resulting in an increased consumption of fuel. A gas yielded through reformation of fuel, hereafter called "reformed gas," unlike a liquid fuel, such as gasoline, possesses a very wide range of combustion and a high octane value. Thus, use of a reformed gas as a fuel, with appropriate selection of an internal combustion engine and appropriate combination with a car-mounted fuel reformer, hereafter called "reformer," will bring about an increased overall efficiency of energy utilization and a saving of fuel consumption. The main component of hydrocarbons in the reformed gas is methane (CH 4 ). Since methane (CH 4 ) is poor in photochemical reactivity and stable in combustability, when used at the same rate of air excess as gasoline, methane will lower the content of hydrocarbons in the exhaust gas. Moreover, when the reformed gas is burned as a lean mixture, the generation of harmful components in the exhaust gas, such as nitrogen oxides and carbon monoxide, can be substantially inhibited.
Namely, operation with a combination of a reformer and an internal combustion engine will be far more advantageous than operation with a direct supply of liquid fuel, like gasoline or gaseous low-class hydrocarbons, to the internal combustion engine, but an appropriate control is needed for this purpose.
Now the reformer is to be considered. Partial oxidation of n-heptane, as an example of liquid fuel, can be expressed by:
C.sub.7 H.sub.16 + 3.50.sub.2 - 7CO + 8H.sub.2
(calorific value: 146 Kcal/mol)
The air/fuel ratio in this reaction is about 4.8. It is known that the air/fuel ratio has to be slightly higher than the above value for the purpose of maximizing hydrogen generation, but this is restricted by the material quality of the reformer, the lower limit of the optimum reaction temperature, and segregation of carbon and thermal efficiency, while for this purpose of adapting the reformed gas to the internal combustion engine, the calorific value per unit volume and the octane value of the reformed gas have to be limited. Only when all these conditions are satisfied can lean-burning, which characterizes the reformed gas, take place efficiently and effectively. Thus, to give full play to the merit of the reformed gas, the operating condition of the reformer has to be swiftly and properly changed, corresponding to changes in the running conditions of the internal combustion engine, such as, for example, the rpm thereof.
Generally, the reaction temperature, the air/fuel ratio and the reaction volume (material supply rate) in the reformer have influence on the quality and quantity of the reformed gas. For instance, the driver, when he wants an increase in the output of the engine, has to increase the air inflow to the reformer and, depending on the air inflow, also increase the supply of liquid fuel. Meanwhile, for the sake of increased output of the engine, it is desirable not only that the supply of the reformed gas to the engine be increased, but also that the calorific value of the reformed gas per unit volume be also increased. Thus, it is necessary to increase the rate of air inflow to the reformer and decrease the air/fuel ratio. In this way, not only the calorific value per unit volume of the reformed gas generated in the reformer can be increased, but also excessive rise in the reformer temperature can be prevented.
On the contrary, the driver, when he wants a decrease in the engine output, has to decrease the rate of air inflow to the reformer and at the same time decrease the supply of liquid fuel to the reformer. Thereby, since a decrease in the reaction volume is liable to lower the catalyst bed temperature, it is desirable that the air/fuel ratio be increased to prevent a temperature drop.
Thus, in a practical run, the reformer is required to perform an extremely wide range of reactions and, understandably, the air/fuel ratio has to be changed depending on the reaction volume.
Next, the control of gas drawn into the engine is to be considered. The air/fuel ratio of the gas mixture to be burned in the engine is desirably changed to correspond to the running conditions. The internal combustion engine burns a reformed gas generated in a reformer or a liquid fuel which does not pass the reformer or a mixture of these two. When a reformed gas generated in the reformer or a mixture of such with a conventional liquid fuel is employed, the burning range is greatly enlarged, thus enabling lean-burning. Thus, the contents of harmful components, especially of nitrogen oxides, in the exhaust gas can be substantially decreased, while, at the same time, the fuel consumption per unit output can be decreased, as is well-known. However, gaseous fuel, like the reformed gas, is characteristically poor in drawing or sucking efficiency and, accordingly, the maximum output drops unavoidably in the practical range of air/fuel ratios. For this reason, the driver, when he wants a high output, reduces the air/fuel ratio in the gas mixture to be drawn into the engine; increases the air/fuel ratio in the practical working range; and, in a very low speed range or in an idling condition, he increases the air/fuel ratio further or decreases the air/fuel ratio with the throttle valve closed. Thus, control of the ratio of air and fuel drawn into the engine is far more complicated than in the reformer.
For this reason, it is necessary to develop a method and system by which the driver can swiftly and properly effect the aforementioned complicated control by a simple manipulation.
SUMMARY OF THE INVENTION
Accordingly, a primary object of the present invention is to recognize the driver's consciousness of driving and to effect a change in the volume of air inflow to the reformer according to such recognized consciousness or, in other words, to link the driver's handling of an output control device, such as an accelerometer, directly and instantly with the action of the reformer.
Another object of the present invention is to computerize the action of the whole reformer system to attain the constructive transfer of the driver's consciousness of driving into a corresponding change in volume of the air flow into the reformer.
Yet another object of the present invention is to provide preferential control of the composition of a reformer-generated gas, thereby preventing undesirable phenomena in the reformer, such as overheating, overcooling and carbon segregation.
Still another object of the present invention is to control the air inflow to a reformer, thereby increasing the calorific value per unit volume of the gaseous fuel generated in the reformer.
Still another object of the present invention is to provide a fine control of a whole reformation system by automatically and exactly maintaining the ratio of air and fuel supplied to the reformer and the ratio of the gaseous fuel generated in the reformer and supplied to the internal combustion engine and the air drawn thereinto.
Still another object of the present invention is to cause leanburning of a reformed gas from a reformer, thereby minimizing the harmful contents in the exhaust gas, such as nitrogen oxides and carbon monoxide.
The foregoing and other objects are attained by the present invention which provides a control method and system for swiftly adapting the air/fuel ratio of a reformer and the air/fuel ratio of an internal combustion engine connected to the reformer, respectively, to the optimum conditions therefor by converting the driver's consciousness of driving output requirements into terms of a changing air inflow to the reformer. In other words, it is so arranged that his consciousness of driving can be sensitively reflected directly as a rise or fall in the volume of air inflow to the reformer. Information on a rise or fall in the volume of air inflow is processed by a computer to optimize the volume of liquid fuel supplied to the reformer and the composition and volume of the gas mixture drawn into the internal combustion engine.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects, features and attendant advantages of the present invention will be more fully appreciated as the same becomes better understood from the following description when considered in connection with the accompanying drawings wherein:
FIG. 1 is a schematic view of a preferred embodiment of the present invention;
FIG. 2 shows a basic configuration of a computer to be used in the embodiment of the present invention shown in FIG. 1;
FIG. 3 is a characteristic diagram illustrating the relation between the propeller frequency and the drawn air volume; and
FIG. 4 is a characteristic diagram illustrating the relation between the jet duration and the propeller frequency.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the Drawings, and more particularly to FIG. 1, there is shown a general composition of a car-mounted fuel reformer system, the major components of which are an air pump 10, a valve 12 interlocked mechanically or electrically with an accelerator pedal 11, a reformer 13, an air pipe 15 equipped with a mixer 14, and a computer 16. The air pump 10 comprising an air suction pipe 17 and a blower pipe 18 is given a torque via a belt 27 from the internal combustion engine, not shown. The blower pipe 18 is connected via a flowmeter 19 to the valve 12 and has attached thereto a pressure adjustment valve 20. By setting this valve 20 at a desired pressure, for instance about 0.6 kg/cm 2 , the air pressure in the blower pipe 18 can be desirably adjusted. The valve 12 is connected to the air intake of the reformer 13 through a pipe member 18'. The liquid fuel intake of the reformer 13 is connected to a liquid fuel supply pipe 21, which is fitted with a blow rate control valve 22, for instance, and electromagnetic valve. A reformed gas jet pipe 23 at the outlet of the reformer 13 is connected to the mixer 14 attached to the air pipe 15. The reformed gas goes through the reformed gas jet hole 14a opening provided in air pipe 15 and then into the air pipe 15 itself. In the upstream part of the air pipe 15 there is disposed an air flowmeter 24 and in the downstream part of the air pipe 15 there is disposed a butterfly valve 25. The butterfly valve 25 interlocks with a servo-motor 26 for being opened and closed. The upstream end of the air pipe 15 connects to an air cleaner, not shown, while the downstream end connects to the intake manifold of an internal combustion engine, also not shown. The flowmeter 19, the flow rate control valve 22, the air flowmeter 24 and the servo-meter 26 are respectively connected to the computer 16.
During the starting phase of the operation of the present invention, air flowmeter 24 generates a signal to the computer 16 and, in turn, to servo-motor 26 which serves to open butterfly valve 25 so as to allow for a proper secondary air and reformer gas mixing with introduction into the internal combustion engine for the purpose of starting the same. Furthermore, the mixing ratio of the reformed gas and the secondary air which are supplied into the air pipe 15 can be controlled by varying the opening degree of the butterfly valve 25, thus maintaining the total ratio of air and fuel, which are fed into the internal combustion engine, at a constant level. Control of the opening degree of butterfly valve 25 is accomplished by servo-motor 26 as controlled by the computer 16.
At the starting phase of the internal combustion engine, a driver depresses the accelerator pedal 11 to open valve 12, thereby introducing air into the reformer 13 through the air pump 10. Then, the volume of air supplied to the reformer 13 is detected by the flow meter 19 and the thus detective value is transmitted to the computer 16. The computer 16 controls the control valve 22 according to the detected value of the flowmeter 19, thus adjusting the amount of fuel supplied to the reformer through the control valve 22 to the volume of air supplied to the reformer 13, so as to maintain the air/fuel ratio in the reformer 13 at constant level. The amount of the reformed gas generated by the reformer 13 is proportional to the air amount detected by the flowmeter 19.
On the other hand, the amount of the secondary air detected by the flowmeter 24 is transmitted to the computer 16. According to the thus detected value of the secondary air, the computer 16 controls the opening degree of the butterfly valve 25, thereby maintaining the total air/fuel ratio of the mixing gas composed of the reformed gas and the secondary air, which are both supplied into the air pipe 15, at a constant level.
The reformer 13 may be a conventional one, for instance the one illustrated in FIG. 1, in which a granullar catalyst 13c is inserted between two opposed metal screens 13a, 13b. The flowmeter 19 provided midway in the blower pipe 18, which is intended for measurement of a relatively low flow rate, may be a propeller type flowmeter, but is not limited to being propeller type. In the propeller type flowmeter 19, a proportional relation, as illustrated in FIG. 3, holds between the volume of air flowing in the blower pipe 18 and the propeller frequency or rpm. The rpm of the propeller type flowmeter is fed to the computer 16, which calculates the necessary supply of fuel. The propeller rpm is converted to a frequency signal in an rmp/frequency transducer 16a, shown in FIG. 2, consisting of a radiative diode-photo transistor. The frequency signal is then converted to a voltage signal in a frequency/voltage transducer 16b and the voltage signal goes into an arithmetic operation circuit 16e. Meanwhile, the engine rpm signal from a distributor terminal 28 has its waveform rectified in a waveform rectifying circuit 16c and is converted to a voltage signal in a frequency/voltage transder 16d, which signal goes into the arithmetic operation circuit 16e. In the arithmetic operation circuit 16e, the signal from the propeller type flowmeter 19 is divided by the signal from the distributer terminal 28, thereby giving the air flow rate in each revolution of the engine. From the present diagram of fuel jet duration vs. air volume, the necessary fuel jet duration can be found, as illustrated in FIG. 4. The fuel jet duration signal is then sent to a correction circuit 16f, where it is added with various factors to give a more appropriate fuel jet duration signal, which is then converted to a frequency signal by a voltage/frequency transducer 16g. The frequency signal is sent to a fuel supply control valve drive amplifier 16 h, where it is changed to an output with enough power to drive the fuel flow rate control valve 22. The opening of this valve 22 is set depending on this output. When this valve 22 is electromagnetic valve, the open-close timing of the valve will depend on this output.
In operation, the torque of an internal combustion engine, not shown, is directly or indirectly, through a transmission member like belt 27, transmitted to the air pump 10. The primary air supplied from the air pump 10 is set to a desired pressure, as already indicated, by the pressure adjust valve 20 and this air is introduced through the flowmeter 19 and the valve 12 into the reformer 13. Upon the output control device 11, for instance the accelerator pedal, being operated by the driver, the valve 12 interlocked therewith acts to control the flow rate of primary air, increasing the flow rate when the output is to be increased. The flow rate of primary air is converted to an electrical signal at the flowmeter 19. When this signal is fed to the computer 16, a control valve, such as the electromagnetic valve 22, provided in the fuel supply pipe 21, reacts to this signal, thereby controlling the flow rate of liquid fuel and supplying the fuel to the reformer 13. At the same time the flowmeter 24 provided in the air pipe 15 converts the flow rate of the drawn secondary air to an electrical signal, which is then fed to the computer 16. The servo-motor 26 reacts to this signal and causes the valve 25 in the air pipe 15 to control the volume of drawn air such that the air/fuel ratio of the gas mixture supplied to an internal combustion engine, not shown, may settle to a value corresponding to the volume of gaseous fuel flowing in through the mixer or venturi 14. In this way, the driver can swifly and adequately control the operating condition of the reformer and the internal combustion engine by mere operation of the output control device, or more simply, the accelerator pedal. Thus, the practical value of the present invention is extremely high.
According to the present invention, in which the whole system is placed under the control of a computer, fine control is practicable, the exhaust gas can be clean, fuel consumption can be decreased, and with the composition of the gaseous fuel produced in the reformer being preferentially controllable, the reformer can be maintained at the right temperature and segregation of carbon can be prevented.
The internal combustion engine which burns a gaseous fuel, which contains much hydrogen and contains carbon monoxide or methane as the main combustible element, is more heavily affected by the calorific value of fuel than by the air/fuel ratio. Therefore, according to the present invention, which can swiftly control the composition of gaseous fuel, an internal combustion engine can run under different conditions without misfiring or stopping. Moreover, since the air/fuel ratio can be finely adjusted, the air/fuel ratio can be very smoothly held at a present value.
The effect of applying the present invention is illustrated in the following example:
Experimental Conditions
Road : flat, smooth
Vehicle : passenger car weighing 1,100 Kg
Internal combustion engine : 1,600 cc 4-cylinder
Reformer : partial oxidation type
Catalyst : nickel
Liquid Fuel : non-leaded gasoline
______________________________________Experimental results Catalyst Air/fuel ratioCar speed Output NO.sub.x temp. in reformer(km/hr) (ps) (ppm) (° C) (weight ratio)______________________________________30 2.2 90 850 5.260 7.2 110 870 4.590 13.8 205 950 3.8______________________________________
In the above example, it is designed that with an increased volume of air inflow to the reformer, the air/fuel ratio may gradually drop. As is evident from the above table, even when the engine rpm rises and the load is increased, the NO x content of the exhaust gas is held at a low level and the catalyst temperature is in the range of 800° C. ˜ 1,100° C. in which the catalyst can be highly active.
Depending on the structure and material quality of the reformer practically employed, the air/fuel ratio should be properly corrected. For instance, the air/fuel ratio under maximum load is restricted by the highest allowable temperature of the catalyst or structural material, the reaction volume, the calorific capacity of the reformer, etc., while the air/fuel ratio under minimum load is restricted by the lowest allowable reaction temperature necessary for reforming reaction. Further, the air/fuel ratio under medium output is affected by a change in the engine output depending on the composition of gaseous fuel produced by reforming and by a change in the composition of exhaust gas. Moreover, these air/fuel ratios under maximum and minimum loads may be re-corrected.
As many apparently widely different embodiments of this invention may be made without departing from the spirit and scope thereof, it is to be understood that within the scope of the appended claims the invention may be practiced otherwise than as specifically described herein.
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A control method and system for efficient operation of an internal combustion engine by controlling the volume of gas mixture supplied from a car-mounted fuel reformer to the internal combustion engine and the mixing ratio, as well as the volumes of air and fuel supplied to the car-mounted fuel reformer. To be more specific, efficient operation of the internal combustion engine is provided by controlling the mixing ratio of air and liquid fuel supplied to a car-mounted fuel reformer, which produces a hydrogen-containing gas from a liquid fuel through the reaction of partial oxidation, and at the same time adding a controlled volume of air to the hydrogen-containing gas discharged from the car-mounted fuel reformer and supplying the resultant mixture of the hydrogen-containing gas and air to the engine.
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