description stringlengths 2.98k 3.35M | abstract stringlengths 94 10.6k | cpc int64 0 8 |
|---|---|---|
BACKGROUND OF THE INVENTION
This invention relates to a floor mat device, and more particularly to a floor mat for performing an audible message upon a person stepping thereon.
The use of electrical switches incorporated into floor mats is known. Various uses for such floor mats have been suggested such as for energizing lights, bells etc. as well as opening doors. Heretofore, such floor mat devices were interfaced with an externally displaced device such as a light, alarm or door opening mechanism. The interface required a physical connection between the external element and the switching mechanism in the mat proper. This necessity not only increased the expense of the device but also introduced additional labor costs needed to establish the interface. Also, in some cases the design of the physical interface itself, usually in the form of a hard wire or other type of current relaying device, degraded the aesthetics of the surrounding environment such as the doorway, entrance or other area in which the floor mat was to be used. Finally, the past floor mats were usually relatively complex in construction particularly as to the incorporation of the switching element utilized therein. Thus, it is desirable to have a cost-effective floor mat which avoids the above problems and defects.
In response thereto, we have invented a floor mat device incorporating a speech module which allows the user to record his/her own selectable message for playback upon a person stepping on the floor mat proper. The module may be either programmed with a user-selectable message or may contain a preprogrammed message such as "welcome,""good morning," etc. The module is releasably insertable into a mat housing which precludes the need to interface the mat with any external device. A speaker jack may be provided by which the message may be relayed to a displaced location via an external audio transducer in addition to the speech module speaker. The device is activated by pressure responsive switch mechanisms (two disclosed) which are easily constructed and embedded in the floor mat proper with minimum time, trouble and expense.
Accordingly, it is a general object of this invention to provide a floor mat which plays back an audible message upon pressure being exerted thereon.
Another general object of this invention is to provide a floor mat, as aforesaid, which plays back an audible message upon a user stepping thereon.
A further object of this invention is to provide a floor mat, as aforesaid, by which playback of the audible message is controlled by a pressure responsive switch incorporated in the mat proper.
Another object of this invention is to provide a floor mat, as aforesaid, which has a housing thereon for containing a record and/or playback speech module with power supply and speaker therein.
A particular object of this invention is to provide a floor mat with housing, as aforesaid, which allows user access to the speech module therein, either in the form of a releasable or slidable housing panel.
Another particular object of this invention is to provide a floor mat with housing, as aforesaid, which protects the speech module from the weather.
A further particular object of this invention is to provide a floor mat with housing, as aforesaid, which allows various speech modules to be easily placed therein either from the top or underside of the housing.
Another object of this invention is to provide a floor mat with housing, as aforesaid, which allows the user to have a selectable access to the speech module so as to either record a message, replace the module or otherwise affect the speech module therein.
Still another object of this invention is to provide a floor mat with switch, as aforesaid, which is impervious to the weather.
A further object of this invention is to provide a floor mat, as aforesaid, which can play back either a user selectable or a pre-programmed message.
Still another object of this invention is to provide a floor mat, as aforesaid, which incorporates an activating switch of novel design for the speech module which is relatively simple to manufacture and easily incorporated into the floor mat proper.
Another object of this invention is to provide a floor mat with housing, as aforesaid, which reasonably protects the speech module from damage upon persons stepping thereon.
Other objects and advantages of this invention will become apparent from the following description taken in connection with the accompanying drawings, wherein is set forth by way of illustration and example, an embodiment of this invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a plan view illustrating a first embodiment of the floor mat and showing in phantom lines thereon an outline of the electrical switch for activating the speech module;
FIG. 2 is a side view, taken along line 2 in FIG. 1, showing the housing with speech module, power supply and speaker in phantom lines therein;
FIG. 3 is a fragmentary view, taken along line 3 in FIG. 2, illustrating the housing in an open position to expose the power supply, speech module and speaker therein;
FIG. 4 is a view illustrating the switch mechanism used in the embodiment of FIG. 1;
FIG. 5 is a semi-exploded view of the switch mechanism shown in FIG. 4, on an enlarged scale, illustrating the construction of the switch mechanism;
FIG. 6 is an alternative second embodiment of the floor mat showing the alternative activating switch mechanism;
FIG. 7 is a schematic circuit diagram of a now preferred form of speech module utilized in the floor mat;
FIG. 8 is a top plan view showing an alternative housing for containing the speech module, power supply and speaker with the mat area being fragmentarily shown for purposes of illustration;
FIG. 9 is a side view of the housing shown in FIG. 8, on an enlarged scale, showing the housing with the speech module, power supply and speaker shown in phantom lines;
FIG. 10 is a bottom view of the housing to illustrate the access panel on the underside of the floor mat.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Turning more particularly to the drawings, FIG. 1 shows a plan view of the floor mat 100. The mat 100 generally comprises a rectangular mat 120 having a raised carpet pile 130 thereon. Incorporated in the mat 120 is an electrical switch means 300, as shown in phantom lines in FIG. 1 and in FIGS. 4 and 5, and to be subsequently described.
At one corner of the mat 120, adjacent the carpet pile 130, is affixed a raised housing 220 made of a weather and pressure impervious plastic or the like. The housing 220 includes first and second spaced apart rails 222, 224 (FIG. 3) located atop a pair of laterally spaced apart side walls 226, 228. A panel 230 is configured to slidably fit within rails 222, 224 so as to expose a 9-volt DC, power supply 240, speech module 250 and speaker 260 therein (FIG. 3). Accordingly, selectable access to the speech module 250 is provided while protecting the elements in the housing from the weather and/or a person stepping thereon.
An alternative housing 220' is shown in FIGS. 8-10. In this embodiment the top wall 230° of the housing is fixed. Access to housing 220° is provided by a back panel 229 on the underside of the mat 120.
In construction, the reverse side of the carpet pile 130 is exposed and placed within a rectangular mold for pouring a thin layer of plastic thereon. The switching mechanism 300 or 400 can then be placed atop this first poured layer. Upon pouring a subsequent layer of plastic material thereon the layers are allowed to set so as to embed the switch mechanism 300 or 400 therein. Wire leads 310, 320 or 410 extending from the switch mechanism 300, 400 are then connected to the electrical circuitry (FIG. 7) of the speech module 250.
In construction of the FIG. 8 embodiment an aperture is die cut into the plastic material of the mat 120. The housing 220' is then fixed within the die cut aperture by a suitable adhesive material.
One form of speech module 250 is the Eletech DM-2500 speech module available from Electech Electronics of Anaheim, Ca. This module is a record and playback speech system with an on-board miniature microphone. The circuitry of such module 250, as provided by Eletech, is shown in FIG. 7.
Upon sliding the panel 230 along rails 222, 224 to the open (FIG. 3) position and toggling the record button 252, four, eight or 16 second speeches may be recorded by the user for subsequent playback. A 9-volt DC battery 240 provides a power supply 240 for the speech module 250 circuitry. The speech module 250, approximately 2.5 inches by 3 inches, is releasably insertable into the housing 220 along with the power supply 240 and speaker 260. The above-described record/playback module 250 may be fixed within housing 220 or it may be interchangeable with a module having a fixed pre-recorded message with no record capability. The leads 310, 320, 410, 420 of the normally open switch 300, 400 are wired into the circuitry of either speech module such that switch closure will cause a current flow through the circuitry and activate the playback mode of the utilized speech module 250.
In the FIG. 8 embodiment the toggle switch 251' activates the power supply 240. Upon pressing the record switch 252' the user speaks into the microphone 257. An LED light 253 indicates whether the message is being recorded.
One switch 300 which may be utilized and incorporated into the mat is shown in FIGS. 4 and 5. Therein is shown a sheet of mylar 350 having a plurality of apertures 360 aligned in rows and columns therein. A single sheet 380 of plastic presents first and second panels 382, 384. Conductive ink material in the form of parallel strips are imprinted on each panel 382, 384. A plurality of parallel strips 370 are provided on panel 384 as well as a plurality of parallel strips 390 on panel 382 which are normal to panel 384 strips 370. A strip of adhesive 392 runs along the border of sheet 380. Accordingly, upon folding the panel 380 along its center line 362, closure of the same is accomplished by the mating of the facing portions of the adhesive strip 392. Upon such mating a plurality of spaced intersections of the strips 370, 390 will occur as displaced by the intermediate mylar 350. Leads 310, 320 are then connected to the circuitry of the speech modules 250. At this juncture the spatial relationship between the conductive strips 350, 370 presents a DC open precluding any current flow through the speech module 250 circuitry.
Upon pressure being exerted on the mat 100, e.g. by a person stepping thereon, the overlying strips 390 approach the underlying strips 370. The intermediate apertures 360 allow for contact of these strips 350, 370. Upon such contract, a closed current path is provided. Thus, current will flow causing playback of the previously recorded message on the speech module 250.
Alternatively, a capacitor-type switch in the form of a 22-gauge wire 400 communicating with the circuitry of the speech module through lead 410 can be used as shown in FIG. 6. One end 450 of the 22-gauge wire is left open. This arrangement presents a capacitance-type switch. Upon a user stepping on the mat 100 a change in capacitance will occur causing a change in the voltage. This voltage change will cause a current flow through the speech module 250 so as to energize the same and play back the message.
Also, as shown in FIG. 3, a speaker jack 262 is associated with speaker 260 for connection of a wire thereto from an external audio device. This jack allows for wire communication between the speech module message and a source other than the speaker 260.
Accordingly, it is apparent that the use of the switches 300 or 400 with the housing 220 or 220' encompassing the speech module 250, speaker 260 and power supply 240 eliminates the above-described problems found in the prior art. The mat 100, as above described, precludes the need for an external, unsightly interface between the switch 300 or 400 in the mat and an external device. As such, unsightly wiring or the like is eliminated which enhances the aesthetics of the surrounding environment and precludes the need for any additional installation costs. Moreover, as the speech module is enclosed in the housing 220 by either the slidable panel 230 or releasable back panel 229, easy access is made available to the housing 220, 220' upon selectable panel 229, 230 manipulation in order to change the recorded message or the entire module 250 itself. Also, the housings 220, 220' render the assembly reasonably impervious to weather so as to increase its life. Finally, the possibility of destruction of the contents of the housings 220, 220' by a person stepping on the mat is reasonably precluded.
The use of the housing 220' with panel 229 on the underside of the mat 120 further decreases the possibility of weather and pressure damage to the contents therein. Moreover, this housing 220' discourages undesirable access thereto due to the position of the releasable panel 229.
It is to be understood that while three forms of this invention have been illustrated and described, it is not limited thereto, except insofar as such limitations are included in the following claims and allowable functional equivalents thereof. | A floor mat includes a housing for containing a power supply, speech module and speaker. A grid-like switching mechanism is closed upon a person stepping on the mat so as to provide an energizing current flow to the speech module. The speech module includes circuitry for recording and playing back a selected message. A slidable or releasable panel in the housing allows for selectable user access to the speech module. The housing precludes weather deterioration of the elements therein and cooperates with the switching mechanism so as to provide a user-selectable message to a person stepping on the mat. The mat/housing configuration allows alternative switching mechanisms to be used in connection with replaceable speech modules. | 7 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of German Patent Application No. 202 19 754.9, filed Dec. 19, 2002, the entirety of which is incorporated herein by reference.
[0002] This application is a continuation of U.S. application Ser. No. 11/154,770, filed Jun. 16, 2005, which is a continuation of International Application PCT/DE2003/004274, filed Dec. 18, 2003, the entireties of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0003] The invention relates to a deep hole drill comprising a cutter carrier, a replaceable cutting insert and at least one replaceable guide strip wherein the cutter carrier can be used for a predetermined nominal diameter range, and a range for equipping a cutter carrier for such a deep hole drill wherein a new type of equipping method can be implemented with this range.
[0004] In single-lip deep hole drills the swarf is removed by means of a supplied lubricant via the relatively large, straight-grooved machined groove as a result of the single-lip geometry. The actual cutting process takes place by means of a drill cutter which can be located on a cutting plate or a cutting insert, for example which is screwed onto the cutter carrier. At the same time, during drilling the tool is supported over its circumference in the drill hole by corresponding guide strips.
[0005] Deep hole drills with such replaceable cutting inserts/guide strips are highly economical and have good cutting performance. This is because, when the cutters or the guide strips wear, there is no need to purchase an expensive complete tool but only the relatively inexpensive cutting insert or the guide strip. In addition, the cutter carrier can be used not only for one nominal diameter but within an entire nominal diameter range.
[0006] Such a generic tool is shown for example in the prospectus “Deep hole drills type 01”, No. 01-0501-01 of the company “botek Präzisionsbohrtechnik GmbH”. This drilling tool is fitted with a drill shank soldered to a clamping sleeve and a drill head connected thereto. The drill head has corresponding seats with threaded holes for one cutting plate and for two guide strips by which means the cutting plate and the two guide strips can be screwed to the drill head. The alignment of the position of the cutting edge i.e., the adjustment of the precise nominal diameter within the nominal diameter range for which the deep hole drill is provided is accomplished in this case by means of a replaceable adjustment plate which forms a stop for the cutting plate. The stop is located on the side of the replaceable plate opposite to the minor cutting edge, i.e. before the replaceable plate is attached to the drill head, an adjustment, plate suitably selected for the desired nominal diameter is screwed onto the drill head parallel to the longitudinal axis of the tool so that the replaceable plate abuts against the adjustment plate with its side opposite to the minor cutting edge. The thickness of the adjustment plate used thus determines the position of the minor cutting edge and therefore the nominal diameter of the hole. In addition to the adjustment plate itself, an adjustment wedge is provided for pre-adjustment of the stop surface of the adjustment plate on the corresponding tool back, which can be inserted into a hole ending on the back of the adjustment plate and fixed with a screw. Thus, a plurality of time-consuming work processes are required to adjust the position of the cutting edge to the desired nominal diameter or to equip the cutter carrier with the components provided for the corresponding nominal diameter. However, no positional displacement of the guide strips is provided. The same guide strips are used for the entire nominal diameter range. Thus, accurate guidance of the drill cannot be ensured.
BRIEF SUMMARY OF THE INVENTION
[0007] It is thus the object of the invention to provide a deep hole drill comprising a cutter carrier which can be used for a plurality of nominal diameters in a nominal diameter range, as well as a replaceable cutting insert and at least one replaceable guide strip, which has a simple structure and allows easy-to-handle and rapid adjustment of the tool to the desired nominal diameter. It is a further object to provide a range of inserts for equipping a cutter carrier for deep hole drilling tools which can be used to implement a new type of cutter carrier equipping method by making available a suitable range of inserts.
[0008] This object is solved with regard to the deep hole drill by the deep hole drills and deep hole drill sets according to the present invention. The new type of equipping method which constitutes an independent invention is characterised as follows: the method allows a cutter carrier of a deep hole drill, which can be used universally within a nominal diameter range (ΔND), such as for example a drill especially according to one of the present claims, to be equipped according to the nominal diameter with a kit comprising a replaceable cutting insert and at least one replaceable guide strip provided for a certain nominal diameter. The method is characterized by the following steps:
[0009] selecting a kit provided for a certain nominal diameter from a range of kits comprising all the desired nominal diameters (ND 1 -ND 5 ) in a specified nominal diameter range (ΔND), especially where each cutting insert and each guide strip having counter-stop surfaces with which they can be fixed in position at fixed stops on the cutter carrier or where (1) the cutting inserts and the guide strips can each be screwed to the cutter carrier, (2) the cutting inserts each have a cutting insert through hole at the same distance from the respective counter-stop surfaces, and (3) the guide strips each have a guide strip through hole which extends between its counter-stop surface and a supporting surface, and
[0000] fixing the position of the cutting insert (2) and the at least one guide strip of the selected kit by means of fixed stops on the cutter carrier.
[0010] According to the invention, a selection of kits is associated with the cutter carrier used in a certain nominal diameter range. A kit comprising a cutter carrier and at least one corresponding guide strip is available for each desired nominal diameter. Cutting inserts and guide strips have counter-stop surfaces by which means they can be fixed by means of fixed universally fitting stops on the cutter carrier in the position predetermined by the stops. According to the invention, only the kit corresponding to a desired nominal diameter must be selected from a range of kits and fixed on the cutter carrier by means of the fixed stops thereon.
[0011] In this way, a simple and time-saving adjustment of the drill to the desired nominal diameter is achieved. This is because apart from attaching the desired cutting insert and the corresponding guide strips whilst fixing the position by the stops already present on the cutter carrier, no further work processes are necessary. The geometry of the cutter carrier is configured as universally fitting for all the associated kits so that the diameter adjustment is merely made by selecting the appropriate kit. On the whole, such a high accuracy of the diameter adjustment can be achieved because any incorrect adjustments are rendered impossible by the fixedly predetermined stops which merely define the position of the respective cutting insert and the guide strips. This is because any such additional adjustment is completely eliminated.
[0012] Additional components which would be necessary for such an adjustment are no longer required in the deep hole drill according to the invention. In addition to the reduced number of parts, in the deep hole drill according to the invention, increased stability and strength of the cutter carrier is achieved compared with corresponding known tools since the cutter carrier is not weakened by additional recesses and threaded holes for adjustment plates etc. but fills the predetermined space as completely as possible.
[0013] As a result, the deep hole drill according to the invention is suitable for diameters, e.g., from 16 mm up to around 40 mm, which are very small compared to the nominal diameters which can be achieved in conventional tools (botek: from 18 mm upwards). Tests have shown that good results are achieved with ratios of drilling depth to diameter of 10:1 to 80:1 with a total tool length of up to 3000 mm.
[0014] Advantageous further developments of the invention are the subject matter of the dependent claims.
[0015] The cutting insert is advantageously screwed to the cutter carrier. For this purpose a threaded hole is provided on the cutting insert seat on the cutter carrier whereas a through hole is provided on the cutting inserts so that the cutting inserts can be screwed onto the cutter carrier. In this case, the distance between the through hole and the counter-stop surfaces is the same for all cutting inserts, i.e. all cutting inserts fit the geometry predefined by the universal cutter carrier. The threaded hole on the cutting insert seat has an offset to a through hole on the cutting insert so that, the cutting insert is pressed on the stop when the cutting insert is screwed on the cutting insert seat. The offset is very small (of the order of magnitude of 1/100 mm) so that no deformation of the cutting insert or the cutter carrier occurs but merely to a fixing of the position of the cutting insert at the predetermined stop via the (elastic) deformation of the screw. In this way, equipping the cutter carrier with the cutting insert is further simplified. However, other fixing possibilities are also feasible as fixing for the cutting insert or the guide strip, for example, a guide groove on the cutter carrier into which a T-shaped wedge molded on the cutting insert is inserted.
[0016] The guide strips advantageously each have a through hole for screwing into corresponding threaded holes on the cutter carrier. The guide strips inserted in corresponding grooves on the cutter carrier are screwed into threaded holes on the cutter carrier by means of a through hole running in the radial direction. The through hole extends in each case between a supporting or outer circumferential surface and the counter-stop surface of the guide strip.
[0017] In a preferred aspect of the present invention, the distance of the through hole to the minor cutting edge of a cutting insert to the next larger increases by the same amount as the distance of the supporting surface and the counter-stop surface of the associated guide strip to the next larger guide strip. This ensures that the minor cutting edge is well supported by the guide strip(s) in the hole over the entire diameter range. The increase can be linear in the entire diameter range or it can follow any other pattern, for example, a similarity series.
[0018] Replaceable plates which can be exchanged after their cutting edge has worn have proved particularly suitable as cutting inserts. Errors which could occur as a result of using an indexable insert where a minor cutting edge or land is worn are thus avoided from the outset.
[0019] The use of precise and (disposable) replaceable plates and guide strips fabricated separately for each nominal diameter offers many advantages compared with using turnover plates having the same design for several nominal diameters which must be adjusted to the desired nominal. diameter by means of an adjusting disk, and standard guide strips which do not allow any adjustment to the nominal diameter:
[0020] A suitable set (replaceable plate and guide strip(s)) must be provided for each nominal diameter. However it is clear that the equipping or assembly of the deep hole drill is considerably simplified if the nominal diameter is simply adjusted by selecting the corresponding kit. This is because the iterative process of using turnover plate, adjustment plate, checking measurements etc. is omitted.
[0021] The adjustment of the nominal diameter is thus removed from the assembly process into a previous production process of the replaceable plates and the guide strips especially for that nominal diameter which takes place under defined conditions and in an automated fashion so that in addition to facilitating the assembly of the deep hole drill, an overall higher precision can be achieved during the adjustment of the nominal diameter.
[0022] In a preferred aspect of the present invention, a recess is located on the cutter carrier at the tip of the deep hole drill in the tool face, which is defined by a cutting insert seat by two side surfaces, forming a two-sided stop for the cutting insert. It is particularly easy to equip the cutter carrier thus configured since the cutting insert can be fixed in position in all three coordinate directions using a handle and only needs to be screwed on. If the two stop surfaces span an angle smaller than 90° and the side surfaces facing the two stop surfaces span a larger angle, it is additionally ensured that no uncertainty arises in the position of the cutting insert as a result of tolerance deviations in the inclination of the side surfaces towards one another but in any case two-sided stopping of the replaceable cutting plate or the cutting insert is provided.
[0023] The deep hole drill is advantageously embodied as a single cutter or single-lip deep hole drill. However, the invention is not restricted to single-lip tools. In particular, double-lipped embodiments would also be feasible where a further replaceable plate is provided instead of a guide strip per kit, for example. Triple cutters with three replaceable plates per kit would also be feasible.
[0024] The use of hard metal cutting inserts and guide strips ensures that the kits for the deep hole drill according to the invention have a particularly high wear resistance. Alternatively thereto, the cutting insert and guide strip have a hard material coating. A combination, that is hard-or soft-coated hard-metal cutting inserts and guide strips would also he feasible, likewise ceramic cutting inserts and guide strips. In this case, hard metals consist of metallic hard materials which can be described as relatively brittle because of their high hardness and binders or binder metals predominantly from the iron group (iron, cobalt, zinc) which are relatively soft and tough and are sintered together with the hard materials. Mixtures of ceramics and metals (cermets) are also included among the hard metals. In the hard metal the high hardness and therefore wear resistance of the metallic hard material is combined with the toughness of a binder metal. The desired properties of the drill shank can be adjusted exactly according to the mixing ratio. In addition t,o nitride-hardened layers, cubic boron nitride, corundum, sialone or other nonmetallic materials are suitable as coating materials.
[0025] On the whole, various alternatives are provided whereby the drilling tool can be used in a universal spectrum of materials for processing, whether this be rock, metal, CFK etc.
[0026] Heat-treatable steel has proved to be an advantageous material for the cutter carrier, especially with regard to toughness and torsional resistance i.e. the transferable torque. It would also be feasible to use a cutter carrier equipped with replaceable cutting plates, which is itself made of HSS or hard metal.
[0027] In a preferred aspect according to the present invention, the cutter carrier is a drill head joined to the drill shank in a material-closing fashion, for example, brazed on the drill shaft. The drill head which is subject to higher loading can then be made of a more expensive material and can have a geometry which is more expensive to produce, especially the internal cooling channel(s) whereas the drill shank which is subject to lower loading is made of a cheaper material which is easier to machine and receives its simpler geometry in its own production method.
[0028] The internal cooling channel has, for example, one or two circular cross-sections at the drill tip whereas a circular through hole is inserted on the drill shank.
[0029] In another preferred aspect of the present invention, the drill shank consists of a formed tube of heat-treatable steel. The straight-running machined groove can be impressed into the tube in an easily managed and fast pressing or rolling processing step wherein favourable forming for the internal cooling channel can be achieved at the same time.
[0030] The individual features of the embodiments according to the claims can be arbitrarily combined as far as this seems logical.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
[0031] Preferred embodiments of the invention are explained in detail subsequently with reference to the schematic drawings. In the figures:
[0032] FIG. 1 . is a perspective exploded view of an embodiment of the deep hole drill according to the invention;
[0033] FIG. 2 is a plan view of the drill tip of the single-lipped deep hole drill shown in FIG. 1 ;
[0034] FIG. 3 is a plan view of the drill tip of a modified embodiment;
[0035] FIG. 4 is a detailed view of the inserted replaceable cutting plate of the deep hole drill from FIG. 1 ;
[0036] FIG. 5 is a detailed view of the inserted replaceable cutting plate of a modified embodiment;
[0037] FIG. 6 is a nominal diameter range which includes five nominal diameters;
[0038] FIG. 7 shows the kits associated with the nominal diameters from FIG. 4 .
DETAILED DESCRIPTION OF THE INVENTION
[0039] Reference is first made to FIGS. 1 and 2 which show a single-lipped embodiment of the deep hole drill according to the invention. The reference number 1 designates a drill head which is soldered onto a drill shank 15 which in turn is soldered into a clamping sleeve 16 . The machined groove is substantially v-shaped where the angle spanned by the machined and unmachined surface is approximately 90°.
[0040] At its tip, on the machined surface of the machined groove 13 the drill head has a recess which with its rear surface 5 and the two side surfaces 10 , 14 forms a seat for a replaceable cutting plate 2 . A central threaded hole 7 is drilled into the rear surface 5 which receives a screw 6 guided through a through hole in the replaceable cutting plate 2 .
[0041] Furthermore, at the axial height of the replaceable cutting plate seat two recesses for guide strips 3 are provided over the circumference of the drill, which abut against a stop surface 9 with their radially-pointing plane counter-stop surfaces 109 . Each surface 9 has a central threaded hole for screwing the guide strips 3 .
[0042] In the same way as the guide strips 3 , the replaceable cutting plate 2 has a through hole 8 which, when inserted, is in alignment with a corresponding threaded hole 7 with a minimal offset so that the replaceable cutting plate 2 and also the guide strips 3 can each be screwed rapidly using a single screw 6 .
[0043] In the embodiment shown the fixed stop for the guide strips consists in each case of the rear surface 9 of the guide strip seat on the drill head whereas the width of the guide strips is the same for all nominal diameters. The guide strips of the kits for different nominal diameters thus differ only in respect, of their radial thickness, i.e., the distance between the outer circumferential surface and the counter-stop surface 109 which is defined by the respective nominal diameter of the tool.
[0044] In order to explain the positioning of the replaceable cutting plate 2 over the threaded hole 7 and the through hole 8 , reference is made to FIG. 4 which shows an enlarged plan view of the inserted replaceable plate 2 . It can be seen that the through hole 8 , shown by a solid line, and the threaded hole 7 , shown by a dashed line, are at a small offset with respect to one another which has the result that when the replaceable cutting plate 2 is screwed on, the plate 2 is pushed with its counter-stop side surface 110 against the stop side surface 10 of the cutting plate seat. However this offset is shown clearly oversized here.
[0045] Furthermore, with its second counter-stop side surface 114 running orthogonally to the first, the plate 2 impacts against a point located on the second stop side surface 14 of the cutting plate seat and its position is thus determined by the surfaces 5 , 10 , 14 in all three coordinate directions.
[0046] It is clear that all replaceable cutting plates 2 for any nominal diameter always have a through hole 8 at a predetermined distance from the two counter-stop side surfaces 114 , 110 . This can be seen particularly clearly from FIG. 7 which is explained further below.
[0047] It can also be seen from FIG. 4 that the two stop side surfaces 10 , 14 are inclined at an angle α of 80° with respect to one another whereas the two counter-stop surfaces 110 , 114 span an angle β of 90°. In this case, the cutting plate 2 preferably abuts against the stop surface 10 with the entire counter-stop side 110 . A linear stop would also be feasible, as is shown by an inclined stop surface 10 ′ with a dashed line. The angular shaping of the stop ensures that, inadequate abutment of the replaceable cutting plate 2 on the cutter carrier (the drill head 1 ) does not occur as a result of tolerance deviations.
[0048] FIG. 5 shows a modification where linear contact, of the cutting plate 2 on the stop 10 is achieved by the base surface 5 of the cutting plate seat and the stop surface 10 spanning an angle smaller than 90° whereas the back of the cutting plate 2 and the counter-stop surface 110 are at an angle of 90° with respect to one another.
[0049] The embodiment of the deep hole drilling tool according to the invention shown in FIG. 1 comprises a single-lipped deep hole drill with a cutter on the replaceable plate 2 which is supported by means of two guide strips 3 over its diameter in the hole. With reference to the views of the drills tip shown in FIGS. 2 and 3 , this embodiment is compared with a further embodiment which has only one guide strip 30 . It is found that the invention can be realized in the same way using this type of deep hole drill. In this case, the additional advantage arises that more space is available for the internal cooling channel (see outlet openings 12 , 11 ).
[0050] FIG. 7 shows five kits, each comprising a replaceable cutting plate and two guide strips for equipping the drill shown in FIG. 1 .
[0051] The kits cover five nominal diameters ND 1 to ND 5 which lie in a nominal diameter range ΔND (see FIG. 6 ). For better clarity, the through hole 8 , the counter-stop surfaces 110 , 114 and the minor cutting edge 120 are only designated on the replaceable cutting plate for the largest nominal diameter ND 1 and on a relevant guide strip, the counter-stop surface 109 and the supporting surface 50 .
[0052] In FIG. 6 the hatched area shows the nominal diameter range ΔND in which the universally fitting drill head of the deep hole drill from FIG. 1 can be adjusted to the five nominal diameters ND 1 to ND 5 by replacing the cutting plates and guide strips. In this case, the through hole 8 on all cutting plates has the same distance c from the counter-stop surface 114 and b from the counter-stop surface 110 . The distance of the through hole from the minor cutting edge which determines the hole diameter, increases on the other hand from the value a 0 at the nominal diameter ND 5 and specifically from ND 5 to ND 4 by the value Δa. It can be seen that the radial thickness of the guide strip, i.e. the length of the through hole (shown dashed) increases accordingly.
[0053] Naturally, deviations from the variants shown are also possible without departing from the basic idea of the invention. | A deep hole drill comprising a cutter carrier, a replaceable cutting insert and at least one replaceable guide strip. The cutter carrier is embodied in such a way that it can be used for a predetermined nominal diameter range. In order to adjust the deep hole drill to the various desired nominal diameters in a quicker and more precise manner, a separate kit consisting of a cutting insert and at least one guide strip is associated with each nominal diameter. Fixed stops are provided on the cutter carrier for said kit. | 8 |
TECHNICAL FIELD
[0001] The invention relates to a cold work tool steel.
BACKGROUND OF THE INVENTION
[0002] Vanadium alloyed powder metallurgy (PM) tool steels have been on market for decades and attained a considerable interest because of the fact that they combine a high wear resistance with an excellent dimensional stability and because they have a good toughness. These steels have a wide rang of applications such as for knives, punches and dies for blanking, piercing and cold extrusion. The steels are produced by powder metallurgy. The basic steel composition is firstly atomized and thereafter the powder is filled into a capsule and subjected to hot isostatic pressing (HIP) in order to produce an isotropic steel. The performance of the steels tends to increase with increasing content of vanadium. A high performance steel produced in this way is CPM®10V. It has high carbon and vanadium contents as described in U.S. Pat. No. 4,249,945. Another steel of this kind is disclosed in EP 1 382 704 A1.
[0003] Although the known (PM) steel has a higher toughness than conventionally produced tool steels, there is a need for further improvements in order to reduce the risk for tool breakage, such as chipping and fracture and to further improve the machinability. Until now the standard measure to counteract chipping is to reduce the hardness of the tool.
DISCLOSURE OF THE INVENTION
[0004] The object of the present invention is to provide a powder metallurgy (PM) produced cold work tool steel having an improved property profile leading to an increased life time of the tool.
[0005] Another object of the present invention is to optimize the properties, while still maintaining a good wear resistance and at the same time improve the machinability.
[0006] A particular object is to provide a martensitic cold work tools steel alloy having an improved property profile for cold working.
[0007] The foregoing objects, as well as additional advantages are achieved to a significant measure by providing a cold work tool steel having a composition as set out in the alloy claims.
[0008] The invention is defined in the claims.
DETAILED DESCRIPTION
[0009] The importance of the separate elements and their interaction with each other as well as the limitations of the chemical ingredients of the claimed alloy are briefly explained in the following. All percentages for the chemical composition of the steel are given in weight % (wt. %) throughout the description.
Carbon (2.2-2.4%)
[0010] Carbon is to be present in a minimum content of 2.2%, preferably at least 2.25%. The upper limit for carbon may be set to 2.4% or 2.35%. Preferred ranges are 2.25-2.35% and 2.26-2.34%. In any case, the amount of carbon should be controlled such that the amount of carbides of the type M 23 C 6 and M 7 C 3 in the steel is limited to less than 5 vol. %, preferably the steel is free from said carbides.
Chromium (4.1-5.1%)
[0011] Chromium is to be present in a content of at least 4.1% in order to provide a good hardenability in larger cross sections during heat treatment. If the chromium content is too high, this may lead to the formation of high-temperature ferrite, which reduces the hot-workability. The chromium content is therefore preferably 4.5-5.0%. The lower limit may be 4.2%, 4.3%, 4.4% or 4.5%. The upper limit may be 5.1%, 5.0%, 4.9% or 4.8%.
Molybdenum (3.1-4.5%)
[0012] Mo is known to have a very favourable effect on the hardenability. Molybdenum is essential for attaining a good secondary hardening response. The minimum content is 3.1%, and may be set to 3.2%, 3.3%, 3.4% or 3.5%. Molybdenum is a strong carbide forming element and also a strong ferrite former. The maximum content of molybdenum is therefore 4.5%. Preferably Mo is limited to 4.2%, 3.9% or even 3.7%.
Tungsten (≦2%)
[0013] In principle, molybdenum may be replaced by twice as much tungsten. However, tungsten is expensive and it also complicates the handling of scrap metal. The maximum amount is therefore limited to 2%, preferably 1%, more preferably 0.3% and most preferably no deliberate additions are made.
Vanadium (7.2-8.5%)
[0014] Vanadium forms evenly distributed primary precipitated carbides and carbonitrides of the type M(C,N) in the matrix of the steel. In the present steels M is mainly vanadium but significant amounts of Cr and Mo may be present. Vanadium shall therefore be present in an amount of 7.2-8.5. The upper limit may be set to 8.4%, 8.3%, or 8.25%. The lower limit may be 7.3%, 7.4%, 7.5%, 7.6%, 7.7%, 7.75%, and 7.8%. The upper and lower limits may be freely combined within the limits set out in claim 1 . Preferred ranges include 7.7-8.3%.
Nitrogen (0.02-0.15%)
[0015] Nitrogen may optionally be introduced in the steel in an amount of 0.02-0.15%, preferably 0.02-0.08% or 0.03-0.06%. Nitrogen helps to stabilize the M(C,N) because the thermal stability of vanadium carbonitrides is better than that of vanadium carbides.
Niobium (≦2%)
[0016] Niobium is similar to vanadium in that it forms carbonitrides of the type M(C,N) and may in principle be used to replace vanadium but that requires the double amount of niobium as compared to vanadium. Hence, the maximum addition of Nb is 2.0%. The combined amount of (V+Nb/2) should be 7.2-8.5%. However, Nb results in a more angular shape of the M(C,N). The preferred maximum amount is therefore 0.5%. Preferably, no niobium is added.
Silicon (0.1-0.55%)
[0017] Silicon is used for deoxidation. Si is present in the steel in a dissolved form. Si increases the carbon activity and is beneficial for the machinability. Si is therefore present in an amount of 0.1-0.55%. For a good deoxidation, it is preferred to adjust the Si content to at least 0.2%. Si is a strong ferrite former and should preferably be limited to ≦0.5%.
Manganese (0.2-0.8%)
[0018] Manganese contributes to improving the hardenability of the steel and together with sulphur manganese contributes to improving the machinability by forming manganese sulphides. Manganese shall therefore be present in a minimum content of 0.2%, preferably at least 0.22%. At higher sulphur contents manganese prevents red brittleness in the steel. The steel shall contain maximum 0.8%, preferably maximum 0.6%. Preferred ranges are 0.22-0.52%, 0.3-0.4 and 0.30-0.45%.
Nickel (≦3.0%)
[0019] Nickel is optional and may be present in an amount of up to 3%. It gives the steel a good hardenability and toughness. Because of the expense, the nickel content of the steel should be limited as far as possible. Accordingly, the Ni content is limited to 1%, preferably 0.3%. Most preferably, no nickel additions are made.
Copper (≦3.0%)
[0020] Cu is an optional element, which may contribute to increasing the hardness and the corrosion resistance of the steel. If used, the preferred range is 0.02-2% and the most preferred range is 0.04-1.6%. However, it is not possible to extract copper from the steel once it has been added. This drastically makes the scrap handling more difficult. For this reason, copper is normally not deliberately added.
Cobalt (≦5%)
[0021] Co is an optional element. It contributes to increase the hardness of the martensite. The maximum amount is 5% and, if added, an effective amount is about 4 to 5%. However, for practical reasons such as scrap handling there is no deliberate addition of Co. A preferred maximum content is 1%.
Sulphur (≦0.5%)
[0022] S contributes to improving the machinability of the steel. At higher sulphur contents there is a risk for red brittleness. Moreover, a high sulphur content may have a negative effect on the fatigue properties of the steel. The steel shall therefore contain ≦0.5%, preferably ≦0.03%.
Phosphorus (≦0.05%)
[0023] P is an impurity element, which may cause temper brittleness. It is therefore limited to ≦0.05%.
Be, Bi, Se, Ca, Mg, O and REM (Rare Earth Metals)
[0024] These elements may be added to the steel in the claimed amounts in order to further improve the machinability, hot workability and/or weldability.
Boron (≦0.6%)
[0025] Substantial amounts of boron may optionally be used to assist in the formation of the hard phase MX. Lower amounts of B may be used in order to increase the hardness of the steel. The amount is then limited to 0.01%, preferably ≦0.004%. Generally, no boron additions are made.
Ti, Zr, Al and Ta
[0026] These elements are carbide formers and may be present in the alloy in the claimed ranges for altering the composition of the hard phases. However, normally none of these elements are added.
[0000] Steel production
[0027] The tool steel having the claimed chemical composition can be produced by conventional gas atomizing. Normally the steel is subjected to hardening and tempering before being used.
[0028] Austenitizing may be performed at an austenitizing temperature (T A ) in the range of 950-1200° C., typically 1000-1100° C. A typical treatment is hardening at 1020° C. for 30 minutes, gas quenching and tempering at 550° C. for 2×2 hours. This results in a hardness of 59-61 HRC.
EXAMPLE
[0029] In this example, a steel according to the invention is compared to the known steel CPM®10V. Both steels were produced by powder metallurgy.
[0030] The basic steel composition was melted and subjected to gas atomization.
[0031] The steels thus obtained had the following composition (in wt. %):
[0000]
Inventive steel
CPM ® 10V
C
2.3
2.4
Si
0.37
0.89
Mn
0.37
0.45
Cr
4.78
5.25
Mo
3.6
1.26
V
8.0
9.85
Mo/V
0.45
0.13
balance iron and impurities.
[0033] The steel were austenitized at 1100° C. for 30 minutes, hardened by gas quenching and tempering twice at 540° C. for 2 hours (2×2 h) followed by air cooling. This results in a hardness of 63 HRC for both materials.
[0034] The composition of the matrix and the amount of primary MX at three different austenitizing temperatures were calculated in a Thermo-Calc simulation with the software version S-build-2532. The results are shown in Table 1.
[0000]
TABLE 1
C
Si
Mn
Cr
Mo
V
MX (%)
Inventive steel
1020° C.
0.43
0.43
0.42
4.6
1.54
0.39
15.8
1050° C.
0.47
0.42
0.42
4.6
1.65
0.48
15.5
1080° C.
0.52
0.42
0.42
4.7
1.76
0.59
15.2
CPM ® 10V
1020° C.
0.34
1
0.58
5.1
0.51
0.39
17.2
1050° C.
0.38
1
0.58
5.1
0.54
0.48
17
1080° C.
0.42
1
0.57
5.2
0.58
0.58
16.7
[0035] Table 1 reveals that the amount of hard phase in the inventive steel was only about 1.5% lower than the amount in the comparative steel. In addition, the simulation indicates that the matrix contained significantly higher amounts of carbon and molybdenum than in the comparative steel. Hence, an improved tempering response, as well as a higher hardness, are to be expected from this simulation. This was also confirmed by the calculated values, which indicated a higher hardness for the inventive steel. Moreover, the inventive steel is less sensitive to hardness decrease at high temperatures such that higher tempering temperatures can be used for removing retained austenite without impairing the hardness.
[0036] Surprisingly, it was found that the inventive steel also had a much better toughness. The un-notched impact energy in the transverse direction was 41 J as compared to 11 J for the comparative steel. The reason for this improvement is not fully clarified but it would appear that the low Si-content in combination with a high Mo-content improve the strength of the grain boundaries. Hence, the improved toughness of the inventive steel makes it possible to maintain a high hardness without problems with chipping and therefore improve the durability and lifetime of cold working tools.
Machinability Testing
[0037] Machinability is a complex topic and may be assessed by a number of different tests for different characteristics. The main characteristics are: tool life, limiting rate of material removal, cutting forces, machined surface and chip breaking. In the present case the machinability of the hot work tool steel was examined by drilling.
[0038] The turning machinability test was carried out on a NC Lathe Oerlikon Boehringer VDF 180 C. The work-piece dimensions were Ø115×600 mm.
[0039] The V30-value was used to compare the machinability of the steels. The V30-value is specified as the cutting speed, which gives a flank wear of 0.3 mm after 30 minutes of turning. V30 is a standardized test method described in ISO 3685 from 1977. The turning operation was performed at three different cutting speeds until the flank wear of 0.3 mm. The flank wear was measured using light optical microscope. The time to reach the 0.3 mm flank wear was noted. Using values of cutting speeds and the corresponding turning times, the Taylor double logarithmic graph—time versus cutting speed V×T α =constant was plotted, from which it was possible to estimate the cutting speed for the required tool life of 30 minutes. The turning machinability test was carried out without cooling using a Coromant S4 SPGN 120304 hard metal insert, a feed of 0.126 mm/revolution and a cutting depth of 1.0 mm.
[0040] The inventive steel, which had a V30-value of 51 m/min, was found to perform better than the comparative steel, which only had a V30-value of 39 m/min.
INDUSTRIAL APPLICABILITY
[0041] The cold work tool steel of the present invention is particular useful in applications requiring good wear resistance in combination with a high resistance chipping. | The invention relates cold work tool steel. The steel includes the following main components (in wt. %): C 2.2-2.4, Si 0.1-0.55, Mn 0.2-0.8, Cr 4.1-5.1, Mo 3.1-4.5, V 7.2-8.5, balance optional elements, iron and impurities. | 2 |
PRIORITY
[0001] This application is a continuation-in-part application claiming the priority of U.S. application Ser. No. 11/257,968 filed Oct. 24, 2005 and titled “NEW VISIBLE POLARIZING GLASS AND PROCESS” and naming as inventors Nicholas F. Borrelli, George B. Hares, David J. McEnroe and Joseph F. Schroeder. This continuation-in-part application retains all the foregoing as inventors and names as additional inventors Sasha Marjanovic and Katherine R. Rossington.
FIELD OF THE INVENTION
[0002] The invention is directed to polarizing glasses and a method for making such glasses. In particular, the invention is directed to a silver-containing glass composition and a noble metal from the group consisting of platinum, palladium, osmium, iridium, rhodium and ruthenium, and a method for making the polarizing glass that does not require a reducing atmosphere step.
BACKGROUND OF THE INVENTION
[0003] A polarizing effect can be generated in glasses containing silver, copper or copper-cadmium crystals. These crystals can be precipitated in a boroaluminosilicate glasses having compositions containing suitable amounts of an indicated metal and a halogen other than fluorine.
[0004] The polarizing effect is generated in these crystal-containing glasses by stretching the glass and then exposing its surface to a reducing atmosphere, typically a hydrogen containing atmosphere. The glass is placed under stress at a temperature above the glass annealing temperature. This elongates the glass, and thereby elongates and orients the crystals. The shear stress that acts on the particles is proportional to the viscosity of the glass and the draw speed during elongation. The restoring force that opposes the deformation by the shear force is inversely proportional to the particle radius. Hence, the optimum conditions for producing a desired degree of particle elongation and a resulting polarizing effect at a given wavelength involves a complex balance of a number of properties of the glass and the redrawing process. Once the glass has been elongated, the elongated glass article is then exposed to a reducing atmosphere at a temperature above 120° C., but not over 25° C. above the glass annealing point. This develops a surface layer in which at least a portion of metal halide crystals present in the glass are reduced to elemental silver or copper.
[0005] The use of silver halide as a polarizer material capitalizes on two properties of the silver halide that are (1) the liquid particle is very deformable, and (2) it is easier to make larger and controlled particles sizes. The disadvantages of using silver halide are (1) that one cannot make polarizers that operate at wavelengths shorter than red (approximately 650 nm) because of the refractive index of the silver halide and (2) that the process required a hydrogen reduction step. It is possible to stretch silver particles in glass as described in by E. H. Land in U.S. Pat. No. 2,319,816 and later by S. D. Stookey and R. J. Araujo in Applied Optics, Vol. 7, No. 5 (1968), pages 777-779. However, the problems encountered are the control of particle size and distribution, especially for visible polarizer application where the aspect ratio of the particle is smalls, typically 1.5-2 to 1.
[0006] The production of polarizing glass, as is described in the patent references provided below, broadly involves the following four steps:
1. Melting a glass batch containing a source of silver, copper or copper-cadmium and a halogen other than fluorine, and forming a body from a melt; 2. Heat treating the glass body at a temperature above the glass strain point to generate halide crystals having a size in the range of 500-2000 Angstroms (Å); 3. Stressing the crystal-containing glass body at a temperature above the glass annealing point to elongate the body and thereby elongate and orient the crystals; and 4. Exposing the elongated body to a reducing atmosphere at a temperature above 250° C. to develop a reduced surface layer on the body that contains metal particles with an aspect ration of at least 2:1.
[0011] Glass polarizers, the material compositions and the methods for making the glasses and articles made from the glasses have been described in numerous United States patents. Products and compositions are described in U.S. Pat. Nos. 6,563,639, 6,466,297, 6,775,062, 5,729,381, 5,627,114, 5,625,427, 5,517,356, 5,430,573, 4,125,404 and 2,319,816, and in U.S. Patent Application Publication No. 2005/0128588. Methods for making polarizing glass compositions and or compositions containing silver, and/or articles made from polarizing or silver-containing glasses have been described in U.S. Pat. Nos. 6,536,236, 6,298,691, 4,479,819, 4,304,584, 4,282,022, 4,125,405, 4,188,214, 4,057,408, 4,017,316, and 3,653,863. Glass articles that are polarizing at infrared wavelengths have been described in U.S. Pat. Nos. 5,430,573, 5,332,819, 5,300,465, 5,281,562, 5,275,979, 5,045,509, 4,792,535, and 4,479,819; and in non-U.S. patents or patent application publications JP 5-208844 and EP 0 719 741. The Japanese patent publication describes a copper-based polarizing glass instead of a silver-based polarizing glass.
[0012] While there have been considerable efforts in the art to improve polarizing glasses and the methods used to make them, there is still considerable need for further improvement. In particular, it would be advantageous to have a glass and a method for making the glass that does not require the use of a reducing atmosphere step. While it possible to stretch silver (Ag) particles, there are very considerable problems with regard to controlling particle size and distribution. These difficulties are particularly pronounced regarding visible light polarizers where the aspect ratio is small, typically 1.5-2 to 1. Accordingly, it is the object of the present invention to provide a polarizing glass composition that does not require a reducing atmosphere step and a method for making such glass. In particular, it is an object of the present invention to provide a polarizing glass composition utilizing silver and an additional selected noble metal, wherein the additional noble metal is used to nucleate atomic silver to silver metal particles without the use of a reducing atmosphere step, and a method for making such glass.
SUMMARY OF THE INVENTION
[0013] The present invention is directed to a silver-containing polarizing boroaluminosilicate glass composition that has been doped with an additional noble metal selected from the group consisting of platinum (Pt), palladium (Pd), gold (Au), iridium (Ir), rhodium (Rh) and ruthenium (Ru), wherein the additional noble metal is used to nucleate atomic silver to form silver particles without the need for a reduction step. In its broadest embodiment the noble metal is present at a concentration in the range of >0 to 0.5 wt %.
[0014] The invention is further directed to visible polarizers where in one embodiment, the noble metal, or mixture of noble metals, is present in an amount in the range of 0.0001 wt. % to 0.5 wt. % (1-5000 ppm) measured as total zero-valent noble metal. In another embodiment the noble metal or mixture of noble metals is present in an amount in the range of 0.001 to 0.3 wt. % (10-3000 ppm). In yet a further embodiment the noble metal or mixture of noble metals is present in an amount in the range of 0.01 wt % to 0.3 wt %. In another embodiment the noble metal is platinum (Pt) and is present in an amount in the range of 0.0001 to 0.5 wt. %. In a further embodiment the noble metal is platinum and is present in an amount in the range of 0.001 wt. % to 0.3 wt. %. In an addition embodiment the noble metal is platinum and is present in an amount in the range of 0.01 wt % to 0.3 wt %. The noble metal can be added to the glass composition as a halide, nitrate or nitrite, or complex, for example, without limitation, acetylacetonate, oxalate and crown ether complexes, and other complexes known in the art, or as a solution of any of the foregoing.
[0015] The invention is further directed to a silver-containing boroaluminosilicate polarizing glass composition that has been doped with platinum to thereby nucleate silver ions to form silver metal particles without requiring the use of a reducing atmosphere step or other reductants known in the art such as antimony, starch, sugar or cerium.
[0016] The invention is additionally directed to a method for making a silver-containing polarizing boroaluminosilicate glass composition containing silver and an additional selected noble metal, preferably platinum, to nucleate atomic silver to form silver particles without the use of a reducing atmosphere step.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] FIG. 1 illustrates the polarized transmittance spectrum of two redrawn Pt-doped glass compositions having a heat treatment at temperatures of 600 and 650° C., respectively, prior to drawing.
[0018] FIG. 2 illustrates transmittance in the null (“N”) and through (“T”) for the two glasses of FIG. 1 .
[0019] FIG. 3 illustrates visible light polarizer bars that have been drawn, with a finished bar on the right and an as-poured bar on the left.
[0020] FIG. 4 illustrates a glass bar after drawing on right, drawn glass ribbon in the middle and a root or gob of glass from start-up.
[0021] FIG. 5 illustrates a furnace, load cell and glass bar suspended in the furnace.
[0022] FIG. 6 illustrates an alternative furnace, load cell, downfeed and glass bar suspended in the furnace.
[0023] FIG. 7 illustrates the pulling device (tractor) system of the alternative furnace as used in attenuating the glass down during the draw.
[0024] FIG. 8 illustrates a ribbon of glass exiting the alternative furnace and being drawn down.
[0025] FIG. 9 illustrates a comparison of polarized transmittance of redrawn ribbon from the two different drawing systems.
[0026] FIGS. 10A-10D are an illustration comparing the absorption spectra of glasses having different levels of Pt that have been heat treated at 685° C. for different lengths of time.
DETAILED DESCRIPTION OF THE INVENTION
[0027] The term “noble metal”, as used herein with the regard to the metal dopant added to the silver containing glass, refers to the one or more metals selected from the group consisting of platinum (Pt), palladium (Pd), gold (Au), iridium (Ir), rhodium (Rh), osmium (Os) and ruthenium (Ru). The term “noble metal” as used herein also excludes the silver contained in the glass compositions of the invention. As also used herein the term “ppm” means “parts-per-million by weight”.
[0028] The method of making a polarizing article by redrawing at high stress a glass containing a silver halide (“Ag X” where X is a halogen) phase is well documented. For example, see U.S. Pat. Nos. 6,536,236, 6,298,691 and 4,304,584, and other method patents cited herein. The utility of this process, invented by Coming Incorporated, was in the recognition that it was easier to elongate the silver halide particle at the size distribution that was formed in photochromic glass than it was to elongate a silver particle in an arbitrary glass. Once the Ag halide particle was elongated, it was then reduced in a hydrogen-containing atmosphere to form the required elongated metallic silver particle. Although the direct elongation of a metallic silver particle is possible, the elongation requires a much higher stress. However, this fact does not preclude the situation where, if one finds a glass composition and a process where large silver crystals can be controllably formed, that one would not be able to reduce the stress required to provide reasonable elongation of metallic silver particles. One advantage of the direct metallic silver particle elongation process is that in the resulting product the material surrounding the silver has a lower refractive index relative to the bulk glass. This keeps the surface plasmon resonance at a shorter wavelength, which is important for making polarizers that operate in the visible portion of the spectrum.
[0029] The glass composition of the invention that has the property of controllable large silver particles is derived from the compositions used for gradient index lenses (see U.S. Pat. No. 6,893,991 B2). In gradient index lens glass compositions the glass contains a high concentration of a polarizable ion, for example, Ag + or Cu 2+ , and the ion can be readily ion-exchanged. In the present invention it was important to have a glass composition retain some silver as atomic silver until it can be nucleated to metallic silver is conducted as described herein.
[0030] The base glass composition according to the invention contains the following range of materials in weight percent [wt. %].
TABLE 1 SiO 2 20-60 Al 2 O 3 5-20 B 2 O 3 10-25 Ag 15-40
In making the base glass composition the Si, Al and B materials can be added as oxides and Ag is added as the nitrate or as a mixture of silver nitrate and silver peroxide. Additionally, at least one noble metal salt or salt solution is added to the base glass composition and the resulting composition is mixed. The noble metal, or mixture of noble metals if more than one is used, is selected from the group consisting of platinum, palladium, gold, osmium, iridium and ruthenium salts, and mixtures of two or more of the foregoing. The noble metal can be added as a halide, nitrate, nitrite, a complex (for example without limitation, an acetylacetonate, diamine dihalide, oxalate or crown ether or other complex known in the art), or as a solution of any of the foregoing. In one embodiment the noble metal, or mixture of noble metals, is present in an amount in the range of 0.0001 wt. % to 0.5 wt. % (1-5000 ppm measured as total zero-valent noble metal), and it can be added as a halide, nitrate, nitrite, a complex (for example without limitation, an acetylacetonate, diamine dihalide, oxalate or crown ether or other complex known in the art), or as a solution of any of the foregoing. In a further embodiment the noble metal is present in an amount in the range of 0.0001 to 0.3 wt. %. In an additional embodiment the noble metal in present in an amount in the range of 0.001 to 0.3 wt %.
[0031] In a selected embodiment according to the invention, the glass composition according to the invention is approximately (in weight percent ±2 wt. %):
TABLE 2 SiO 2 34 Al 2 O 3 17 B 2 O 3 14 Ag 35
and the noble metal is Pt in amount in the range of 0.0001 wt. % to 0.5 wt. % (measured as total zero-valent noble metal). In another selected embodiment the glass composition is as shown in Table 2 and the noble metal is Pt in an amount in the range of 0.0001 to 0.3 wt %. In a further selected embodiment the glass composition is as shown in Table 2 and the noble metal is Pt in an amount in the range of 0.0005 to 0.3 wt. %. In yet another embodiment the glass composition is also the same as shown in Table 2 and the Pt is present in an amount in the range of 0.02 wt. % to 0.2 wt. %.
[0032] When the base glass composition alone is melted in a quartz crucible at approximately 1350° C. for approximately 16 hours, a clear, slightly yellow glass is produced. The slightly yellow color of the glass is indicates that substantially all of the silver is dissolved in the glass composition as the silver +1 ion. The glass also fluoresces under ultraviolet light indicating that al least some of the silver is present at atomic silver. Upon adding only a slight amount of a noble metal, for example, platinum, to the base glass composition the slightly yellow color of the glass turns to a deep red-brown color that is indicative of the presence of large colloidal silver particles. Small silver particles produce a yellow color whereas the large particles produce a light scattering effect in addition to the absorption. This is the appearance of a Pt-doped glass; that is the color is deeper and darker due to the light scattering effect. The level of Pt, or other noble metal(s), needed to induce this change is in the range of 0.0001 to 0.5 wt. %. Once the nucleation or formation of metallic silver has been carried out, one can further increase the density of the color (that is, the amount of precipitated colloidal silver particles) by heat treating the glass to a temperature in the range of 500-800° C. for a time in the range of 5 minutes to 10 days, preferably to a temperature in the range of 600-750° C. for a time in the range of 10 minutes to 48 hours at temperature. This ability for further effect precipitation gives one additional control over the amount of silver that is present as metallic silver crystals in the glass. In addition, a further heat treatment at a temperature in the range of 500-800° C. for a time in the range of 0.5 to 6 hours enables one to grow larger silver crystals.
[0033] Once the nucleation/precipitation has been completed, the glass is than shaped prior to drawing, for example, by molding or by cutting a glass boule into a desired shape, and Blanchard ground into bars, for example bars that are 10 to 40 inches long, 3-4 inches wide by approximately 0.25 to 0.6 inch thick. To allow higher draw forces on the glass, an etching process, or a thermal treatment, or both, is used to remove or heal surface and subsurface defects that are introduced during the grinding process. When a glass surface is mechanically removed (for example by grinding), many surface and/or subsurface fractures or flaws can either result or become exposed. Under an applied stress these fractures or flaws can propagate into the glass body causing the glass to fracture. By chemically etching and/or thermally treating the glass surface the flaws are healed by rounding out the fracture (flaw) surface, or by closing it using a thermal treatment. Thermal treatments are generally carried out at a temperature near (within 25-50° C.) the softening point of the glass composition. As an example of etching, prior to drawing the glass, the glass bar is immersed in a dilute hydrofluoric acid solution for a period of time sufficient to remove a portion of the surface to remove contamination and flaws. If deemed necessary, visual inspection, with or without the use of magnification, can be used to determine when the process is completed. The glass bars are then drawn under conditions where the draw temperature allows a glass viscosity greater than 10 6 poise and a pulling velocity that is sufficient to apply a force greater than 3500 psi (>3500 psi) to elongate the silver particles.
[0034] FIG. 1 illustrates the polarized transmittance spectrum (uncorrected for reflectance) of a redrawn Pt-doped glass having the composition given in Table 2. It was determined that at pulling velocities less than 3500 psi (<3000 psi) the elongated silver particle aspect ratio is small and therefore the null direction transmission increases at lower wavelengths. For a polarizing glass operating at lower wavelengths, for example, in the visible range, this increase in null direction transmission is undesirable. When the applied force to stretch the silver, which force is controlled by the viscosity of the glass and velocity of the draw speed, is greater than 3500 psi, a glass material with an acceptable polarizing behavior in the visible range was obtained. Further, it is preferable to apply to the drawn glass as great a force as the mechanical strength of the glass and the equipment will permit in order to achieve the desired elongation of the silver particles. The unpolished glass sample illustrated in FIG. 1 had a transmission is 60% in the pass or through direction (that is, light passing through the glass in the direction perpendicular to the direction of elongation) and essentially 0% transmission in the null or stop direction (that is, no light passing through the glass in the direction parallel to the direction of elongation).
[0035] FIG. 2 illustrates on a single graph the polarized transmittance spectrum (uncorrected for reflectance) in the range of 400-800 nm (visible range) of two samples of a drawn Pt-doped glass having the composition given in Table 2. Sample A (illustrated by the solid line, and which is the same as the sample as illustrated in FIG. 1 ), was given a pre-draw heat treatment at 650° C. and Sample B (illustrated by the dashed line) was given a per-draw heat treatment at 600° C. For each sample light transmission in the direction perpendicular (through or pass direction) and parallel (null or stop direction) to the direction of elongation of the silver particles it shown by the capital letters “T” and “N”, respectively.
[0036] FIG. 2 illustrates that one can selectively determine the wavelength or wavelength range in which light will be polarized when a silver-containing glass is doped with a noble metal, heat treated and drawn in accordance with the invention to thereby elongate the silver particles therein. For Sample A, the glass composition was heat treated at 650° C. prior to drawing. As one can see from the graph, transmittance in the null direction (N) direction is essentially zero in the range of approximately 475-550 nm. Sample B, which is the same glass composition as Sample A, was heat treated at 600° C. prior to drawing. For this sample the transmittance in the null direction is below 10 in the approximate range of 425-480 nm. For both glass sample transmittance in the through (“T”) direction are similar through the range measured. This comparison illustrates the aspect of the invention which is that by use of a noble metal in a silver containing glass, one can tailor the null range of the glass by appropriate heat treatment prior to drawing the glass. As a result, one is able to form a glass that selectively polarized a selected wavelength range. As shown in FIG. 2 , by controlling the heat treatment one can determine the performance of a glass at a given wavelength by regulating the silver particle size. In FIG. 2 , the further the null peaks are shifted to the right. The shift of the null peak represents better elongation of the particles or greater aspect ratio, and based on the assumption that larger particles are easier to elongate, it is concluded that the particles in the glass are larger. Thus, the curves also show that when a glass is heat treated at lower temperatures we have smaller particles that are more difficult to elongate during draw.
[0037] FIGS. 10A-10D are absorption spectra comparisons of high silver aluminoborosilicate glasses containing various levels of Pt. The glasses were heat treated at 685° C. for times of 20, 25, 30, 35, 40, 45 and 50 minutes, which times are represented by the letters A, B, C, D, E, F and G, respectively. The amount of Pt used for FIGS. 10A, 10B , 10 C and 10 D was 0.001, 0.01, 0.002 and 0.05 wt %, respectively. The data indicates that the absorption spectra for 0.001% Pt glass (the lowest level of the four figures) has the strongest absorption. While the samples evaluated in FIGS. 10A-10D were heat treated at 685° C. for the times indicated above and in the Figures, the heat treatment can be carried at temperatures in the range of 500-800° C. for times in the range of 5 minutes to 10 days, recognizing that long thermal treatments would not be very cost effective. In selected embodiments the heat treatments are carried out at a temperature in the range of 500-800° C. for a time in the range of 10 minutes to 48 hours. In additional selected embodiments the heat treatments are carried out for a time in the range of 20 minutes to 24 hours at a temperature in the range of 600-750° C.
[0038] As indicated above, the 0.001% Pt glass spectrum has the strongest absorption of all the glasses measured. It is believed that what is being observed is that more silver(+1) is being reduced with 0.001% Pt glass than is the case when the Pt concentration is at a higher level; for example, at a Pt concentration of 0.01% or more. Without being held to any particular theory, it appears that lowering the Pt concentration increases the amount of reduced silver, and it is also believed to lessen the amount of Pt colloids. The color of the as-made glass at the higher Pt concentrations is gray-green, while at lower levels it is yellow. This suggests that the difference observed in the as-made glasses is the result of colloidal Pt. It has been observed that even when the glass is initially yellow, one can strike to a level of silver (Ag 0 ) that exceeds the level obtained at higher Pt concentrations. One possible explanation is that when the Pt concentration is “high”, during the melting process there is a failure to reach thermodynamic equilibrium between platinum and silver, and that the resulting glass has a higher concentration of Pt +4 . The additional Pt +4 , that is, the amount in excess of the thermodynamic equilibrium, results in less silver reduction. If this is correct, then decreasing the amount of Pt to a selected level should result in optimized silver reduction. However, if the Pt concentration is decreased too much, then the opposite effect occurs and insufficient silver is less than the optimized level because there is insufficient Pt present.
[0039] A further advantage of the glass according to the invention that when stretched it has both good transmission and contrast values at 535 nm (green polarizer application). Moreover, these values are attained without the need for hydrogen or other reducing atmosphere treatment. The Pt-doped glass according to the invention represents a totally new glass composition for polarizer applications.
[0040] The process according to the invention was developed to allow a high through put of different glass compositions in order to investigate their potential for polarization applications using a redraw technique. The AMPL (for Corning's Advanced Material Processing Laboratory) draw tower (purchased from Heathway Ltd, now Herbert Arnold GmbH & Co. KG, Weilburg, Germany) as shown in FIG. 5 is comprised of a downfeed system, furnace 40 and pulling tractors (not illustrated) that were used to stretch-down glass bars under high tension. Various glass compositions were melted in a crucible then poured into a bar form using a mold. The bars were then either machined finished or used as-poured in the drawing process (see FIGS. 2 and 3 , described below). For the testing described herein, the bars 30 are approximately 2 inches wide by 10 to 40 inches long, and were of varying thicknesses ranging from 0.25 to 0.60 inches. Holes were drilled on each end of the bars (see FIG. 3 illustrating one end of a bar); one hole being used to hang the bar from a metal cylinder 22 on the downfeed system and the other hole was used to grasp the bar to start the drawing process. A load cell 20 was attached to a metal cylinder 22 that was held in the place in the downfeed chuck 24 and the other end of the load cell supported the glass bar. The furnace 40 was a graphite resistance furnace that can span a wide temperature range. The furnace was controlled using a pyrometer and programmable controller. The glass bar was suspended in the furnace by a wire 26 connected to the metal cylinder 22 plus load cell 20 as shown in FIG. 5 .
[0041] After placing the bar in the furnace, the furnace temperature was raised to a temperature at which the glass was soft enough to enable pull-down. For the platinum-doped glass of the invention a temperature of 725° C. was used for drawing the glass. Once the glass was initially pulled down, the downfeed which lowers the glass bar into the furnace at a controlled rate was started. The feed rate of lowering the glass down was set at 13 mm/min. The tractor unit is comprised of two motor driven belts (located below the furnace) opposing each other and rotating in opposite directions so that the motion through the belts is downward. The distance between the belts can be set so that the glass being drawn through can be grasped by the belts and does not slip in the belts.
[0042] FIG. 3 illustrates visible polarizer bars that have been drawn as described above. The bar on the left, colored a light yellow, is a bar as-poured that was drawn without the addition of a noble metal and the bar at the right, dark reddish-brown, is a finished bar containing noble metal and drawn as described herein. FIG. 4 illustrates a glass bar on the right, a drawn glass ribbon in the middle, and a root or gob of glass on the bottom of the bar from start-up. When the bottom portion of the glass bar is drawn down it is a large gob (root) and has to be hand drawn down through the tractor unit, which is approximately two feet below the furnace bottom. Once the root of glass is passed through the tractor belts the smaller ribbon of glass is placed in between the belts and the belts closed so that they are pulling the glass (see FIG. 5 ). The tractor belt speed is then set to a rate that is pulling the glass ribbon down to a specific size. For the platinum doped glass of the invention, a tractor speed of 2.04 m/minute was used. The ribbon can vary in size until all the draw parameters stabilize. In the example shown in FIG. 4 the final size of the ribbon was approximately 3.5 mm (0.138 in.) by 0.50 mm (0.02 in.).
[0043] The purpose of the draw is to induce a tensional force to stretch the polarizing component in the glass, which is usually accomplished at high tensions. The load cell records the force being applied on the glass bar as it is being pulled down by the tractor belts. The load being applied on the glass can be adjusted by changing temperature, downfeed rate or tractor speed. Typically, at the start of the draw the load is small and incremental adjustments, typically by changing temperature, are made to increase the tension on the glass. Sometimes several adjustments are required before a high enough tension is present on the glass. If the load is too great, the ribbon of glass will break and the start up process has to be repeated. Once a high load is achieved, the glass ribbon is marked, the draw parameter(s) recorded, and the ribbon saved. The ribbon geometry is also recorded in order to calculate the force per area applied on that particular piece of glass.
[0044] A second draw apparatus (the PRC draw apparatus) was used for further development of the silver based polarizing glass which had been used on Polarcor™ development. This draw consists of a seven zone rectangular furnace 50 , a downfeed system 52 , load cell 54 (see FIG. 6 ) and a tractor pulling unit 56 (see FIG. 7 ). FIGS. 6 and 7 illustrate the PRC draw system which is similar to the AMPL system with regard to processing, except that the furnace and tractor are not incorporated on a tower structure. The other major difference between the two draw systems is the seven zone furnace on the PRC system. This allows tighter control of the temperatures and the ability to adjust different zones to provide the thermal profile best for drawing.
[0045] The two benefits the PRC draw is the ability to draw larger (wider) bars resulting in wider ribbon and the tractor unit allows greater pulling stresses to be applied to the glass. FIG. 8 shows a picture of the ribbon exiting out of the furnace above the pulling tractor unit. The tractor incorporates wider and longer belts to provide more surface area in contact with the ribbon which eliminates slippage in the tractor.
[0046] The procedure for drawing the glass on the PRC draw is the same as described above with the AMPL draw. The draw parameters for the PRC system that resulted in good polarizing ribbon were in the range of 6 to 8 inch/min. draw speed and a temperature between 620° C. to 650° C. The resulting ribbon geometry is on the order of 15 to 20 mm wide and 0.8 to 1.3 mm thick. Samples were collected during the draw along with the load and draw parameters and then analyzed in a spectrophotometer.
[0047] Results from the PRC draw are shown in FIG. 9 compared to a result from the AMPL draw. It is seen that the Null curve is broader and has a steeper slope at longer wavelengths. This correlates to the PRC draw system ability to apply higher stress and elongating the silver particles to greater extent. This result provides a wider polarization wavelength window and a greater contrast ratio.
[0048] While the invention has been described with respect to a limited number of embodiments, those skilled in the art, having benefit of this disclosure, will appreciate that other embodiments can be devised which do not depart from the scope of the invention as disclosed herein. Accordingly, the scope of the invention should be limited only by the attached claims. | The invention is directed to a silver-containing polarizing boroaluminosilicate glass composition that has been doped with a noble metal selected from the group consisting of Pt, Pd, Os, Ir, Rh and Ru, including mixtures thereof, to nucleate and precipitate silver ions to silver metal without the need for a reducing atmosphere step. The invention is further directed to a method for making the glass composition of the invention. Using the composition and method of the invention, one can prepare a glass having a selected null transmission range. | 2 |
PRIORITY INFORMATION
[0001] This application claims the benefit of U.S. Provisional Application No. 60/339,030 on Oct. 30, 2001.
FIELD OF THE INVENTION
[0002] The field of this invention is inflatable packers and more particularly those that can be deflated and subsequently advanced downhole without swabbing.
BACKGROUND OF THE INVENTION
[0003] Saving trips in a completion procedure saves money. Recently, screens have been run into open hole and expanded as a technique to replace the need to gravel pack. In these situations it is desirable to isolate the formation pressure from the upper part of the well as the screens are run in. The problem in the past has been that once the inflatable is deflated, trying to advance it further into the wellbore to total depth can cause a condition known as swabbing. In an inflatable, the element has a lower movable collar, which rides uphole as the element is inflated. When the element is deflated the lower collar is free to move on the mandrel. Thus if the screen, which had before deflation been tagged into the inflatable, is advanced with the deflated inflatable, the lower collar will ride up when any portion of the element engages the borehole wall. The element will then ball up in a phenomenon known as swabbing.
[0004] The present invention addresses this problem by using the downhole force to advance the deflated inflatable with the screen to also keep the deflated element in a stretched condition to avoid swabbing. Those skilled in the art will appreciate the scope of the invention from the illustrative example of the preferred embodiment, which appears below and more particularly for the appended claims based thereon.
SUMMARY OF THE INVENTION
[0005] A latching assembly for a lower collar on an inflatable is provided. After deflation, the lower collar is engaged to the mandrel so that the deflated inflatable can be advanced with other connected downhole equipment, such as screens to be expanded, in a location further downhole without swabbing.
DETAILED DESCRIPTION OF THE DRAWINGS
[0006] [0006]FIG. 1 is a schematic view, showing the inflatable being run in;
[0007] [0007]FIG. 2 shows the inflatable being set;
[0008] [0008]FIG. 3 shows a screen assembly being tagged into the set inflatable;
[0009] [0009]FIG. 4 shows the inflatable being deflated;
[0010] [0010]FIG. 5 shows the assembly of the de3flated inflatable and the screen advanced downhole, where the screen is to be deployed;
[0011] [0011]FIG. 6 is a half section view of the inflatable and the latch system in the run in position;
[0012] [0012]FIG. 7 is the view of FIG. 6 with the inflatable set;
[0013] [0013]FIG. 8 is the view of FIG. 7 with the inflatable deflated and latched
[0014] [0014]FIG. 9 is the view of FIG. 8 with the deflated element stretched out from being advanced downhole.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0015] The overview of the present invention is shown in FIGS. 1 - 5 . The inflatable 10 is run in the wellbore 12 on drill pipe, coiled tubing or electric wireline 14 . It is set, as shown in FIG. 2, effectively isolating the top of the wellbore 12 from the formation below the now set inflatable 10 . At this time, other downhole equipment can be run into the wellbore 12 without the use of a lubricator at the surface. In FIG. 3, a screen assembly 15 is tagged into the inflated inflatable 10 . At the conclusion of the tagging procedure, the inflatable is deflated by mandrel manipulation, in a known manner. As will be later explained, the deflation of the inflatable 10 secures its inflatable element 16 to the mandrel 18 via a latch system 20 (see FIG. 8). Thereafter, as shown in FIGS. 5 and 9, the element 16 is stretched to its run in position, as the mandrel 18 is advanced downhole with the screen assembly 15 . Those skilled in the art will appreciate that other equipment can be tagged into the inflatable 10 than screen assembly 15 . The inflatable 10 can be run downhole and inflated in a variety of ways. The new feature of the latch system 20 can be executed in a variety of ways to allow a stretching force to be transmitted to the element 16 after it is deflated. This stretching force prevents the element 16 from swabbing, as it is advanced downhole after being inflated and deflated.
[0016] In the preferred embodiment, the latching system is in the form of a ratchet. As shown in FIG. 6, in the run in position, the inflatable 10 has its element 16 in the stretched position to facilitate insertion. Typically the element 16 has a slidably mounted lower collar 22 , which rides up when the element 16 is inflated, as shown in FIG. 7. In the present invention, the mandrel 18 has an extension 24 secured at thread 26 . Extension 24 has ratchet teeth 28 . Collar 22 has a sleeve 30 attached at thread 32 . Sleeve 30 supports teeth 34 , which selectively engage teeth 28 , as will be explained below. Teeth 34 are retained by end cap 36 , which is secured to sleeve 30 at thread 38 .
[0017] As the element 16 is inflated, the collar 22 and sleeve 30 both ride up. This movement, shown in FIG. 7, tends to bring teeth 34 further away from teeth 28 . It should be noted that during run in and set, there has been no engagement of the teeth 34 and 28 .
[0018] When the screen assembly 15 has been tagged into the inflatable 10 (see FIG. 3), the inflatable is deflated in a known manner by setting down weight and then picking up. As shown in FIG. 8, when the pickup force is applied the teeth 28 ratchet past teeth 34 . Subsequent downhole movement of the mandrel 18 with the extension 24 pulls teeth 34 down, since opposed relative movement is precluded by the orientation of teeth 28 and 34 . As shown in FIG. 9, the downward force on the mandrel 18 and extension 24 , pulls the deflated element 16 toward its retracted or run in position. The occurs because the lower collar 22 is forcibly pulled down by the latch system 20 while the upper collar (not shown) on the element 16 remains in position with respect to the advancing mandrel 18 carrying with it the lower collar 22 .
[0019] Those skilled in the art will appreciate that the element 16 will not swab if it is stretched out using the latch system 20 of the present invention. The screen assembly 15 can then be run further downhole and expanded into place against the open hole. Those skilled in the art will appreciate that the present invention encompasses all techniques to grab the element and stretch it out after deflation. The ratchet teeth engagement depicted in the Figures is but one embodiment that is preferred. The full scope of the invention is delineated in the claims, which appear below. Modifications from the embodiment described above are clearly contemplated to be within the scope of the invention particularly if the result is an extension of the element after deflation so that upon further advancement into the wellbore, it will be prevented from swabbing. Apart from ratchets, the stretching of the element can be accomplished with a pressure responsive piston, a J-slot mechanism, or engaging a thread, to mention a few variations.
[0020] While the preferred embodiment has been described above, those skilled in the art will appreciate that other mechanisms are contemplated to accomplish the task of this invention, whose scope is delimited by the claims appended below, properly interpreted for their literal and equivalent scope.
[0021] The foregoing disclosure and description of the invention are illustrative and explanatory thereof, and various changes in the size, shape and materials, as well as in the details of the illustrated construction, may be made without departing from the spirit of the invention. | A latching assembly for a lower collar on an inflatable is provided. After deflation, the lower collar is engaged to the mandrel so that the deflated inflatable can be advanced with other connected downhole equipment, such as screens to be expanded, in a location further downhole without swabbing. | 4 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a toilet which includes a bowl and water flushing source operatively coupled together, and in particular, relates to a means for protecting the surrounding area from water damage should the bowl overflow.
2. Description of the Relevant Art
Although a toilet including a bowl and water flushing source have been in use for many years the Applicant is unaware of any type of protection operating therewith to prevent the overflow of water from the bowl should it become clogged for any reason. The overflow of water to the surrounding floor area frequently causes excessive damage, especially when the flushing apparatus is activated more than once in an attempt to overcome the blockage therein. One of the objects of the present invention is to provide a simple apparatus for protecting the surrounding floors should the bowl overflow because of a blockage therein.
Another object of the present invention is to provide a means for indicating when the overflow water has reached a predetermined level in an auxiliary container utilized therefor.
A further object of the present ivention is to provide a means for preventing the flow of water into the toilet bowl when the overflow therefrom has reached a certain water level.
Another object of the present invention is to provide a simple overflow protection device which may be repeatedly used and may be readily re-set once activated.
SUMMARY OF THE INVENTION
An overflow protection apparatus for use with a toilet including a bowl and water flushing source operatively coupled together providing a water flow path therebetween and a water input flow path for said flushing source, according to the principles of the present invention, comprises in combination, a bowl having an outwardly extending spout with an exit level disposed below the surface of said bowl, and including an inlet aperture for receiving the water from the flushing source. Also included, is an auxiliary reservoir disposed proximate the bowl which is provided with an inlet orifice. The bowl has a capacity approximately equal to the amount of water provided by the flushing source in one flush. A flexible coupling means is also provided and is connected between the bowl spout and the reservoir inlet orifice to provide a continuous water flow path.
The subject matter which I regard as my invention is particularly pointed out and distinctly claimed in the concluding portion of the specification. My invention, itself, however both as to its organization and method of operation, together with further objects and advantages thereof may best be understood by reference to the following description taken in connection with the accompanying drawing.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a pictorial representation of a toilet including a bowl and water flushing source coupled to an auxiliary reservoir, in accordance with the principles of the instant invention;
FIG. 2 is a side view in elevation of the apparatus of FIG. 1 with the auxiliary reservoir placed behind the bowl instead of alongside it;
FIG. 3 is a partial enlarged view of a particular embodiment of a float and activating means connected to a valve in the water flow path to the toilet bowl;
FIG. 4 is an enlarged partial view in cross-section of the shut-off valve and float shown in FIG. 3; and
FIG. 5 is an alternate embodiment of a float and shut-off valve utilized with the auxiliary reservoir to shut off the water input flow path to the flushing source.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the figures, and in particular FIG. 1, which discloses an overflow protection apparatus 10 coupled to a toilet that includes a bowl 12 and a water flushing source or tank 14 conventionally found coupled thereto. The tank 14 is of conventional design and has coupled thereto by means of a water pipe 16 and valve 18 the normal source of water used for flushing the contents in the bowl 12. The tank 14 is provided with a conventional type of trip handle 20 disposed in the upper lefthand corner thereof. The tank, water input line and valve associated therewith are conventional as well as the shut-off apparatus found in the tank and will not be described any further herein.
Although the tank is shown in FIG. 1 as appearing directly above and proximate to the toilet bowl, it is understood that a tank located at a remote position or a pressure type of system which uses a conventional check valve may also be utilized with the present invention.
The bowl 12 is provided with an outwardly extending spout 22 which provided a liquid exit level below the upper surface of the bowl. The surface 24 of the spout 22 is preferably elongated and provided with vertically extending walls 26 forming a channel. This is preferred since an aperture would more readily become clogged whereas an open spout forming a channel as described would be more effective to handle any overflow and small debris which may be floating in the overflow water.
The spout is provided with sufficient outwardly extending surface area to permit a flexible coupling 28 to be connected thereto by either frictional forces or a conventional clamping arrangement, not shown, may be utilized. The other end of the flexible coupling 28 is connected to an inlet orifice provided on the upper surface of an auxiliary reservoir 32 which is disposed, preferably, alongside the bowl 12. Alternately, the reservoir 32 may be placed behind the bowl and beneath the tank 14 if sufficient space is available at the particular installation of the toilet. Although the spout 22 is shown extending outwardly from one side of the bowl 12 it is contemplated that its location may be at any convenient position on the periphery of the bowl depending on the available space at a particular installation.
The reservoir 32 is preferably provided with an air vent 34 which permits the air therein to escape as liquid enters the container. A window 36 may be provided in the reservoir 32 to indicate the level of the water therein at any particular time. If the water should be above an acceptable level, a person observing the water level may readily disconnect the flexible coupling and empty the contents of the reservoir 32 so that it will be ready for use again. Handles 38 are disposed on the end walls of the reservoir 12 and aid in the positioning and removal of the water therefrom.
FIG. 2 shows the reservoir 32 placed behind the bowl 12 in an inconspicuous, out of the way position.
FIG. 3 shows a conventional float mechanism 40 disposed in the reservoir 32. The float mechanism 40 has coupled to its shaft a lever 42. Float mechanism 40, in a conventional manner, will exercise a force on lever 42 causing it to rotate output shaft 44 which will cause flap valve 46 mounted on shaft 44 to rotate therewith and close off the opening 48 in the fluid flow path to the bowl 12. The housing 50 for the output shaft 44 and flap valve 46 may be provided in a separate assembly capable of being connected to the output of a conventional water tank, with the connection presently made to the tank connected to the bottom or underside of the housing 50 in a conventional manner.
FIG. 5 discloses an alternate arrangement wherein the reservoir 32 has incorporated therein a float mechanism 40 which is coupled to a valve assembly 52 disposed on a side wall of the reservoir 32 and is coupled, preferably by copper tubing, to the input water valve 18 conventionally found connected to water tanks 14. The tubing 54 is connected to the valve 52 and then in turn to the input tubing or pipe 16 in the same manner as shown in FIG. 1.
In operation, if the water in the bowl 12 should reach above the level of the surface 24 of spout 22 it would overflow, via the flexible coupling, 28 and enter the inlet orifice 30 of the reservoir 32 and would proceed to fill up reservoir 32. The water entering the reservoir causes the float mechanism 40 to move in an upwardly direction which in turn causes it to move lever 42, as shown in FIG. 3 or activate valve 52 as shown in FIG. 5, thereby cutting off the flow of water from the tank 14 into bowl 12 or, alternatively, cutting off the flow of water coming from the water source into the tank 14. Either one of these actions would prevent further water from entering the bowl and therefore overflowing and entering into the reservoir.
An individual attempting to activate the trip handle 20 a second time to try and use water dislodge the blockage in the bowl 12 would be unable to have any additional water flow, thus protecting the surface or floor area 56 surrounding the toilet from becoming water logged and damaged. A person being unable to use the flushing mechanism would view the window 36 in the reservoir 32 and determine the level of water therein. Upon observing that the water level exceeds the safe level, as indicated by the fact that no additional water is able to flow into the bowl would turn off valve 18 preventing any additional water inflow into the system and proceed to empty the reservoir 32 into another draim system. Once the reservoir has been completely emptied, it is returned to its regular position beside the bowl and connected to the spout as described hereinbefore and is ready for operation again. Valve 18 is then opened filling the tank 14 with water and the system is be ready for use again. If the blockage had not been removed from the bowl at the time the reservoir 32 was emptied the reservoir would again come into play if the trip handle were activated a second time, thus protecting the floor 56 again. Once elimination of the blockage has been accomplished, the reservoir emptied, the operation of the system as a safety and overflow protection apparatus for the bowl is accomplished.
Hereinbefore has been described an overflow apparatus for use with a toilet, which includes a bowl and water flushing source. It will be understood that the various changes in the details, materials, arrangement of parts and operating conditions which have been herein described and illustrated in order to explain the nature of the invention may be made by those skilled in the art within the principles and scope of the invention. | An overflow protection apparatus for use with a toilet includes a bowl having an outwardly extending spout coupled by a flexible hose to a reservoir adapted to receive any excess water flowing out of the toilet. Means are also provided for closing off the water flow from the flushing source and/or the input water source so that the toilet cannot be flushed again until the cause for the overflow therein is cleared. | 4 |
SUMMARY OF THE INVENTION
This invention relates to hypochloresterolemic and hypolipemic products from the cultivation of a microfungus of the genus Aspergillus. More specifically, it relates to compounds of formulae I and II in substantially pure form: ##STR2## as well as pharmaceutically acceptable salts and esters of compound II. The invention also relates to a process of cultivating the microfungus and isolating from the medium hypochloresterolemic compounds of the above structures. These new compounds have the property of inhibiting cholesterol biosynthesis and are useful against hypercholesterolemia and hyperlipemia.
BACKGROUND OF THE INVENTION
Because of the possible connection between high blood cholesterol and atherosclerosis, many efforts have been made to find ways and substances to reduce serum cholesterol in the mammalian body. One way is to inhibit in mammals the body's ability to synthesize cholesterol.
U.S. Pat. No. 4,231,938 and E.P. publication No. 0022478 describe the fermentative production of mevinolin and dihydromervinolin, with chemical structures closely related to the novel compounds of this invention, by cultivation of Aspergillus terreus in a nutrient medium. Those compounds are highly active antihypercholesterolemic agents.
DESCRIPTION OF THE INVENTION
It now has been found that the cultivation of the same microorganism, the microfungus Aspergillus terreus, produces an additional substance isolated from the fermentation broth as the compound of Structure I, that is also an inhibitor of the biosynthesis of cholesterol in mammals. The invention also relates to II and to pharmaceutically acceptable salts of II and to C 1-3 alkyl esters of II, and to substituted C 1-3 alkyl esters of II wherein the substitutent is phenyl, dimethylamino, or acetylamino.
The pharmaceutically acceptable salts of this invention include those formed from cations such as sodium, potassium, aluminum, calcium, lithium, magnesium, zinc, ammonia, ethylenediamine, N-methylglucamine, lysine, arginine, ornithine, choline, N,N'-dibenzylethylene-diamine, chloroprocaine, diethanolamine, procaine, N-benzylphenethylamine, 1-p-chlorobenzyl-2-pyrrolidine-1'-yl-methylbenzimidazole, diethylamine, piperazine, tris(hydroxymethyl)aminomethane, and tetramethylammonium.
The compounds of this invention are useful as antihypercholesterolemic agents for the treatment of artherosclerosis, hyperlipemia and like diseases in humans. They may be administered orally or parenterally in the form of a capsule, a tablet, an injectable preparation or the like. It is usually desirable to use the oral route. Doses may be varied, depending on the age, severity, body weight and other conditions of human patients but daily dosage for adults is within a range of from about 2 mg to 2000 mg (preferably 2 to 100 mg) which may be given in two to four divided doses. Higher doses may be favorably employed as required.
The compounds of this invention also have useful antifungal activities. For example, they may be used to control strains of Penicillium sp., Aspergillus niger, Cladosporium sp., Cochliobolus miyabeanus and Helminthosporium cynodnotis. For those utilities they are admixed with suitable formulating agents, powders, emulsifying agents or solvents such as aqueous ethanol and sprayed or dusted on the plants to be protected.
In another aspect of this invention, it relates to a process for producing the compounds of this invention which comprises cultivating a microorganism belonging to the genus Aspergillus and then recovering compound I of this invention from the cultured broth. As described in U.S. Pat. No. 4,231,938, the Aspergillus, isolated and indentified as a hitherto undescribed microorganism, was designated MF-4833 in the culture collection of Merck and Co., Inc., Rahway, N.J. and a culture thereof was placed on permanent deposit with the American Type Culture Collection, 12301 Parklawn Drive, Rockville, Md. 20852, and has been assigned accession number ATCC 20541. Another isolate, of the organism, designated MF-4845 in the Merck culture collection, has likewise been placed on deposit and has been given the accession number ATCC 20542. Although the use of these is described in connection with the process of this invention, other organisms of the genus Aspergillus including mutants of the above named are also capable of producing these novel compounds and their use is contemplated in carrying out the process of this invention.
The morphological characteristics of the microorganisms MF-4833 and MF-4845 have been found to be those of the genus Aspergillus. Using the criteria specified in the standard authority "Manual of the Aspergilli", Charles Thom and Kenneth B. Rasper, published by the Williams and Wilkins Company, Baltimore, Md., 1945, and by comparison with known species, it has been determined that both strains are Aspergillus terreus.
The culture of these organisms to produce the novel compounds is carried out in aqueous media such as those employed for the production of other fermentation products. Such media contain sources of carbon, nitrogen and inorganic salts assimilable by the microorganism.
In general, carbohydrates such as sugars, for example, glucose, fructose, maltose, sucrose, xylose, mannitol and the like and starches such as grains, for example, oats, ryes, cornstarch, corn meal and the like can be used either alone or in combination as sources of assimilable carbon in the nutrient medium. The exact quantity of the carbohydrate source or sources utilized in the medium depends in part upon the other ingredients of the medium but, in general, the amount of carbohydrates usually varies between about 1% and 6% by weight of the medium. These carbon sources can be used individually, or several such carbon sources may be combined in the medium. In general, many proteinaceous materials may be used as nitrogen sources in the fermentation process. Suitable nitrogen sources include for example, yeast hydrolysates, primary yeast, soybean meal, cottonseed flour, hydrolysates of casein, corn steep liquor, distiller's solubles or tomato paste and the like. The sources of nitrogen either alone or in combination, are used in amounts ranging from about 0.2% to 6% by weight of the aqueous medium.
Among the nutrient inorganic salts which can be incorporated in the culture media are the customary salts capable of yielding sodium, potassium, ammonium, calcium, phosphate, sulfate, chloride, carbonate, and like ions. Also included are trace metals such as cobalt, manganese, iron and magnesium.
It should be noted that the media described in the Examples are merely illustrative of the wide variety of media which may be employed, and are not intended to be limitative. Specifically, the carbon sources used in the culture media to produce the novel compounds of this invention included dextrose, dextrin, oat flour, oatmeal, molasses, citrate, soybean, oil, glycerol, malt extract, cod liver oil, starch, ethanol, figs, sodium ascorbate and lard oil. Included as nitrogen sources were peptonized milk, autolyzed yeast, yeast RNA, tomato paste, casein, primary yeast, peanut meal, distillers solubles, corn steep liquor, soybean meal, corn meal, NZ amine, beef extract, asparagine, cottonseed meal and ammonium sulfate. The major ionic components were CaCo 3 , KH 2 PO 4 , MgSO 4 .7H 2 O and NaCl and small amounts of CaCl 2 .6H 2 O and traces of Fe, Mn, Mo, B and Cu were also present.
The fermentation is carried out at temperatures ranging from about 20° to 37° C.; however, for optimum results it is preferable to conduct the fermentation at temperatures of from about 22° to 30° C. The pH of the nutrient media suitable for growing the Aspergillus culture and producing the novel compounds can vary from about 6.0 to 8.0.
Although the novel compounds are produced by both surface and submerged culture, it is preferred to carry out the fermentation in the submerged state. A small scale fermentation is conveniently carried out by inoculating a suitable nutrient medium with the Aspergillus culture and, after transfer to a production medium, permitting the fermentation to proceed at constant temperature of about 28° C. on a shaker for several days.
The fermentation is initiated in a sterilized flask of medium via one or more stages of seed development. The nutrient medium for the seed stage may be any suitable combination of carbon and nitrogen sources. The seed flask is shaken in a constant temperature chamber at about 28° C. for 2 days, or until growth is satisfactory, and some of the resulting growth is used to inoculate either a second stage seed or the production medium. Intermediate stage seed flasks, when used, are developed in essentially the same manner, that is, part of the contents of the flask from the last seed stage are used to inoculate the production medium. The inoculated flasks are shaken at a constant temperature for several days, and at the end of the incubation period the contents of the flasks are centrifuged or filtered.
For large scale work, it is preferable to conduct the fermentation in suitable tanks provided with an agitator and a means of aerating the fermentation medium. According to this method, the nutrient medium is made up in the tank and sterilized by heating at temperatures of up to about 120° C. Upon cooling, the sterilized medium is inoculated with a previously grown seed of the producing culture, and the fermentation is permitted to proceed for a period of time as, for example, from 3 to 5 days while agitating and/or aerating the nutrient medium and maintaining the temperature at about 28° C. This method of producing the novel compounds is particularly suited for the preparation of large quantities.
Compound I can be hydrolyzed with bases such as NaOH to yield the salts such as the sodium salt of Compound II. The use of bases with other pharmaceutically acceptable cations affords salts of these cations. Careful acidification of the salts affords the hydroxy acid II. The hydroxy acid II or its ammonium salt can be converted to Compound I by refluxing in toluene. Treating Compound I under acidic or basic catalysis with methanol, ethanol, propanol, or butanol or with phenyl, dimethylamino, or acetylamine alkanols yields the corresponding esters of Compound II which also form a part of this invention.
The physico-chemical properties of Compound I are summarized as follows:
1. Molecular Formula:
C.sub.24 H.sub.36 O.sub.6
2. Mass Spectrum:
The mass spectrum was recorded using the chemical ionization technique and displayed in FIG. 1. The peak m/z=421 corresponds to M+1.
3. 1 H NMR Spectrum:
The spectrum was recorded in CDCl 3 solution and chemical shifts are shown in FIG. 2 in ppm relative to internal tetramethylsilane at zero ppm. On the basis of these and other data, the structure of Compound I is believed, with a considerable degree of certainty, to have the chemical structure I: ##STR3##
The corresponding hydroxy acid, Compound II, then has the structure: ##STR4##
EXAMPLE 1
Preparation of Compound I
A. Fermentation
The medium used in each step of the fermentation comprised:
______________________________________Corn steep liquor 5 gTomato paste 40 gOat Flour 10 gGlucose 10 gTrace element solution 10 mlDistilled water 1000 ml______________________________________
adjusted to pH 6.8 with sodium hydroxide.
The trace element solution comprised:
______________________________________FeSO.sub.4.7H.sub.2 O 1 gMnSO.sub.4.4H.sub.2 O 1 gCuCl.sub.2.2H.sub.2 O 25 mgCaCl.sub.2 100 mgH.sub.3 BO.sub.4 56 mg(NH.sub.4).sub.6 Mo.sub.7 O.sub.24.4H.sub.2 O 19 mgZnSO.sub.4.7H.sub.2 O 200 mgdistilled water 1 liter______________________________________
All media were checked for sterility before inoculation with a microorganism.
To a 250 ml non-baffled Erlenmeyer flask was charged 40 ml of medium and the contents of one tube of lyophilized organism MF 4833. It was then shaken for 24 hours at 28° C. on a rotary shaker at 220 rpm. New flasks were then charged with 40 ml of medium and 1 ml of the first flask's contents and were shaken an additional 24 hours at 28° C. A 2 liter flask was then charged with 400 ml of medium and 10 ml of the second stage fermentation mixture and this too was shaken for 24 hours at 28° C.
A 200 gallon stainless steel fermentation vat was then charged with 501 liters of a medium comprising:
______________________________________lactose 2% wt/voldistiller solubles 1.5% wt/volautolyzed yeast 0.5% wt/volPolyglycol P2000 0.25% wt/vol______________________________________
whose pH was adjusted to 7.0. This was sterilized 15 minutes at 121° C. One liter of the third stage above was then charged and the mixture was incubated at 130 rpm at 28° C. for 96 hours with an air flow of 10 cfm.
B. Isolation
About 37.5 lbs. (3/4 bag) of a silicaceous filter aid was added to 110 gal. whole broth from the culture of MF-4833 described above and the mixture was filtered through an 18-inch filter press. The clarified filtrate, (pH 6.6) was adjusted to pH 4.0 by careful addition of 450 ml of concentrated hydrochloric acid, and extracted by agitation with about one-third volume (36 gal) of ethyl acetate. After separation, the upper solvent layer was removed, and the water phase again extracted with ethyl acetate (38 gal) in a similar fashion. After separation, the two extracts were combined and back-washed by agitation with about twelve gallons of water. After separation, the ethyl acetate solution was concentrated under vacuum at a temperature below 30° C., first in a stirred kettle, and finally in a rotary vacuum evaporator to a residual volume of slightly less than one gallon.
Approximately 1 gal. (3800 ml) of ethyl acetate concentrate from the preceding extraction was further concentrated in a rotary evaporator (ca 10 mm, 40° C. bath) to a syrup and was then concentrated twice more, after addition of about one liter of methylene chloride in two portions, to free the syrup of polar solvent. The final oil of about 300 ml which contained about 250 g of solids by dry weight determination, was made up to about 750 ml with ethyl acetate:methylene chloride (30/70; v/v) and 200 g of silica gel was added and mixed in to form a slurry. This was layered over the top of a 14 cm by 36 cm column bed holding 2.5 kg of the same silica gel, in about 7.5 L volume, which had been packed as a slurry in the same solvent mixture. Development with the same solvent was continued until 3 liters of effluent was taken off as forerun.
Development with ethyl acetate-methylene chloride (50/50; v/v) was begun, taking 800 ml effluent fractions. Twelve fractions were taken, then 100% ethyl acetate elution was begun, and after seven more fractions, 100% acetone elution was begun. Peak activity was found in fraction 8. It was concentrated to an oil for further purification; dry wt. by solids determination was 9.0 gm.
Fraction 8 from the silica gel column was triturated with 50 ml methylene chloride and filtered; the dried filter cake weighed 4.9 gm. The filtrate was charged to a 2-inch I.D. by 1-meter long column filled with Sephadex LH-20 dextran gel (Pharmacia) swollen and equilibrated in methylene chloride, and the column was eluted with methylene chloride at a rate of 15 ml/min. Compound I was eluted between 0.64 and 0.81 column volumes. Solvent was removed from this peak leaving a slightly brown residue weighing approximately 0.290 gm. This residue (213 mg) was taken up in 1.5 ml of CH 2 Cl 2 --CH 3 CN (65-35), charged to a prepacked and equilibrated silica gel column (EM LOBAR Size B) and eluted with CH 2 Cl 2 --CH 3 CN (65-35) at 5 ml/min. Evaporation of solvent from the peak eluting between 235 and 360 ml of eluant left 121 mg of crystalline material, m.p. 155°-160° C.
Eighty-two mg of this material was recrystallized from 0.6 ml of absolute ethanol. 2 L of ethanol mother liquors and wash (containing solids at 46 mg/ml, therefore 92 g solids) was evaporated to an oil under vacuum at 40° C. To remove the last trace of ethanol, the oil was taken up in 1.5 L of toluene and the solvent removed under vacuum. Trituration of the residue in cold toluene (1 L) overnight followed by centrifugation and flash evaporation of the centrifugate yielded an oil. This oil was then taken up in 450 ml of hexanes:toluene:methanol 4:1:1 (solvent A), allowed to stand overnight at room temperature, and then centrifuged. The supernatant (total solid 64.35 g) was then charged onto an 8 L Sephadex LH-20 column (10.2×100 cm) equilibrated in solvent A. Elution was done in the same solvent system. The fractions between elution volumes 10,000 ml-12,000 ml were pooled and solvents removed under vacuum. The residue from two such runs were combined (12.4 g) and redissolved in hexanes:toluene:methanol (solvent B) 3:1:1 and rechromatographed on an LH-20 column (bed vol. 930 ml) in the same solvent system. Eluates between elution volumes 1490 ml-2460 ml were pooled and the solvent removed under vacuum. A CH 2 Cl 2 solution of the residue (5.4 g) was then adsorbed onto a silica gel column (E. Merck, silica gel 60, 35-70 mesh, 272 g) and elution was done in a stepwise gradient of MeOH/EtOAc/CH 2 Cl 2 and the 200 ml fractions were analyzed by TLC. The fractions from 10% and 25% MeOH/EtOAc elutions were pooled and the solvent stripped. The residue was chromatographed on an ES-chromegabond MC-18 column (0.96×50 cm) using the mobile phase MeCN:H 2 O 50:50 at a flow rate of 5 ml/min. monitoring at 260 nm, with the fraction collector set at 0.5 min/tube. Fraction 27 (43 mg) from this HPLC step was further purified by E. Merck analytical 20×20 cm silica gel 60F plates with 2 passes in EtOAc. This procedure yielded two UV bands. The slower-moving one was then purified to homogeneity by HPLC using a similar procedure as before yielding I (1.6 mg).
EXAMPLE 2
Alkali and Alkaline Earth Salts of Compound II
To a solution of 42 mg of the product of Example 1 in 2 ml of ethanol is added 1 ml of aqueous NaOH (10 -4 moles; 1 equivalent). After one hour at room temperature, the mixture is taken to dryness in vacuo to yield the sodium salt of Compound II.
In like manner the potassium salt is prepared using one equivalent of potassium hydroxide, and the calcium salt using one equivalent of CaO.
EXAMPLE 3
Ammonium Salt of Compound II
The sodium salt from Example 2 is dissolved in 2 ml of water, cooled in ice and acidified slowly with 0.5 M HCl. The mixture is extracted with ethyl acetate, back-extracted with water, dried over MgSO 4 and filtered. The filtrate is treated with anhydrous ammonia with stirring and cooling to precipitate the ammonium salt.
EXAMPLE 4
Ethylenediamine Salt of Compound II
To a solution of 0.50 g of the ammonium salt of Compound II in 10 ml of methanol is added 75 μl of ethylenediamine. The methanol is stripped off under vacuum and the residue is triturated with acetone, stored in the cold, and filtered to obtain the ethylenediamine salt of Compound II.
EXAMPLE 5
Tris(hydroxymethyl)aminomethane Salt of Compound II
To a solution of 202 mg of the ammonium salt of Compound II in 5 ml of methanol is added a solution of 60.5 mg of tris(hydroxymethyl)aminomethane in 5 ml of methanol. The solvent is removed in vacuo and the residue triturated with a 1:1 mixture of acetonitrile:methanol. The desired tris(hydroxymethyl)aminomethane salt of Compound II is filtered off and dried.
EXAMPLE 6
L-Lysine Salt of Compound II
A solution of 0.001 mole of L-lysine and 0.0011 mole of the ammonium salt of Compound II in 15 ml of 85% ethanol is concentrated to dryness in vacuo. The residue is triturated with 10 ml of warm ethanol, cooled, and filtered to give the L-lysine salt of Compound II.
Similarly prepared are the L-arginine, L-ornithine, and N-methylglucamine salts of Compound II.
EXAMPLE 7
Tretramethylammonium Salt of Compound II
A mixture of 68 mg of Compound III in 2 ml of methylene chloride and 0.08 ml of 24% tetramethylammonium hydroxide in methanol is diluted with ether to cause precipation of the tetramethylammonium salt of Compound II.
EXAMPLE 8
Methyl Ester of Compound II
To a solution of 400 mg of the product, Compound I, in 100 ml of absolute methanol is added 10 ml 0.1 M sodium ethoxide in absolute ethanol. This solution is allowed to stand at room temperature for one hour, is then diluted with water and extracted twice with water, the ethyl acetate, dried over anhydrous sodium sulfate, is removed in vacuo to yield the methyl ester of Compound II.
In like manner, by the use of equivalent amounts of propanol, butanol, isobutanol, t-butanol, amylalcohol, isoamylalcohol, 2-dimethylaminoethanol, benzylalcohol, phenethanol, 2-acetamidoethanol, glycerol and the like, the corresponding esters are obtained. | Substances isolated after cultivation of a microorganism belonging to the genus Aspergillus in a culture medium include a compound with structural formula: ##STR1## compound I is a member of a class of hypocholesterolemic and hypolipemic medicaments. | 2 |
RELATED APPLICATION
[0001] This application is a continuation of and claims priority to U.S. patent application Ser. No. 11/346,451 filed on Feb. 2, 2006.
BACKGROUND
[0002] The present invention relates to data processing by digital computer, SmartPhones, personal data assistants, and so forth, and more particularly to RFID-based personnel tracking.
[0003] Significant resources and costs are invested by many businesses to keep track of the whereabouts and/or arrival and departure times of their field-based employees, e.g. nurses, field technicians, delivery and repair personnel or the like, at various work sites such as the homes of patients or the like. One computer-based system for reporting the arrival and departure times of employees requires manual intervention and is inherently prone to being abused. These systems do not provide reliable and instantaneously available reports on the work schedules of field employees, such as would enable businesses to complete the preparation of service bills and invoices much sooner.
[0004] Another computer-based system accepts telephone calls for inclusion in a report from telephone locations which are included in a valid Automatic Number Identification (ANI) database. ANI is a service that provides the receiver of a telephone call with the number of the calling phone. The method of providing this information is determined by the service provider (such as AT&T, MCI, Sprint, and so forth). The service is often provided by sending the digital tone multi frequency (DTMF) tones along with the call. Call centers can use the information to forward calls to different people for different geographic areas. ANI is commonly used by emergency center dispatchers to save the caller having to report the information and, when necessary, to help locate callers.
SUMMARY
[0005] The present invention provides methods and apparatus, including computer program products, for RFID-based personnel tracking.
[0006] In one aspect, the invention features a method of tracking employees including, in a first computer system, prompting a user for identification input, validating the identification input, receiving data from a first scan of a Radio Frequency Identification (RFID) tag upon initiation of a task, receiving data from a second scan of the RFID tag upon termination of the task, and uploading the identification input and the data of the first and second scan to a second computer system for storage and correlation.
[0007] In embodiments, the first computer system can be a portable computer having an RFID reader. The portable computer having an RFID reader can be a pocket personal computer (PC) with an RFID reader plug-in.
[0008] Data from the first and second scan can be time stamped by the first computer system, the time stamp including a date and time. Data from the first and second scan can include site identification.
[0009] The method can include generating a report from a correlation of the uploaded identification input and the data of the first and second scan.
[0010] The method can include transmitting the report to a report subscriber. The report subscriber can be an employer of the user.
[0011] In another aspect, the invention features a method of tracking including, in a local computer system, inputting a user identification from a field-based user, receiving data from a first scan of a Radio Frequency Identification (RFID) tag upon the field-based user's initiation of a task, receiving data from a second scan of the RFID tag upon the field-based field-based user's termination of the task, and storing the user identification and the data of the first and second scan.
[0012] In embodiments, the method can include periodically sending the stored user identification and the data of the first and second scan to a remote computer system for storage and manipulation.
[0013] The local computer system can be a portable computer having an RFID reader. The portable computer having an RFID reader can be a pocket personal computer (PC) with an RFID reader plug-in.
[0014] Data from the first and second scan can be time stamped by the local computer system, the time stamp including a date and time. Data from the first and second scan can include site identification.
[0015] In still another aspect, the invention features a employee tracking system including a Radio Frequency Identification (RFID) tag, a first computer system for prompting a user for identification input, validating the identification input, receiving data from a first scan of the RFID tag upon initiation of a task, and receiving data from a second scan of the RFID tag upon termination of the task, and a second computer system for receiving, storing and correlating an upload the identification input and the data of the first and second scan.
[0016] In embodiments, the first computer system can be a portable computer having an RFID reader. The portable computer having an RFID reader can be a pocket personal computer (PC) with an RFID reader plug-in.
[0017] Data from the first and second scan can be time stamped by the first computer system, the time stamp including a date and time. Data from the first and second scan can include site identification.
[0018] The invention can be implemented to realize one or more of the following advantages.
[0019] The system and method enable tracking the whereabouts and arrival and departures times of field-based employees at remote sites.
[0020] A trusted employee can place an RFID tag in a known location for subsequent use by one or more non-trusted employees. In one example, the trusted employee places the tag in the known location and the placed tag's serial number is recorded.
[0021] The system and method enable the generation of reports that reflect field-based employee identification along with start and end dates and times with respect to specific job sites visited by the field-based employee.
[0022] The system and method enable a field-based employee to communicate with a remote computer system.
[0023] The system and method enable accurate and non-counterfeitable verification of a field-based employee's job activities.
[0024] One implementation of the invention provides all of the above advantages.
[0025] Other features and advantages of the invention are apparent from the following description, and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] FIG. 1 is a block diagram of an exemplary Radio Frequency Identification (RFID)-based personnel tracking system.
[0027] FIG. 2 is a flow diagram.
[0028] FIG. 3 is a flow diagram.
[0029] Like reference numbers and designations in the various drawings indicate like elements.
DETAILED DESCRIPTION
[0030] As shown in FIG. 1 , an exemplary Radio Frequency Identification (RFID)-based personnel tracking system 10 includes a remote computer system 12 linked to a host computer system 14 . The link between the remote computer system 12 and the host computer system 14 can be a network link, such as the Internet, a wireless link or a telephone link between a modem residing in the remote computer system 12 and the host computer system 14 .
[0031] The remote computer system 12 can include a processor 15 and memory 16 . Memory 16 includes an operating system 18 , such as Linux or Microsoft Windows®, and a tracking/reporting process 100 , described below.
[0032] The host computer system 14 is linked to an RFID reader 20 (also referred to as a read/write device or interrogator). The system 10 also includes an RFID tag 22 (also referred to as a transponder). RFID incorporates the use of electromagnetic or electrostatic coupling in the radio frequency (RF) portion of the electromagnetic spectrum to uniquely identify an object, animal, or person. An advantage of RFID is that it does not require direct contact or line-of-sight scanning. Another advantage is RFID, unlike bar codes, is hard to counterfeit.
[0033] In this example, the RFID reader 20 includes a built-in antenna 24 that uses radio frequency waves to transmit a signal that activates the transponder 22 . When activated, the tag 22 transmits data back to the antenna 24 . The RFID tag 22 can hold many types of data, such as a serial number or identification number.
[0034] RFID tags, such as RFID tag 22 , are either passive, active or battery assisted. Passive RFID tags receive their power to exchange from the signal sent by the RFID reader 20 . Active RFID tags have a battery to power their own transmissions. Battery assisted RFID tags have a battery that powers chip electronics but does not transmit RF energy.
[0035] RFID tags, such as RFID tag 22 , can be read-only or read-write. Read-only RFID tags are programmed with an identification number or other data at the manufacturer's site and cannot be altered. Data on read/write RFID tags can be revised or erased thousands of times by the user.
[0036] In a preferred example, system 10 uses read-only passive RFID tags. In this preferred example, the host computer system 14 and reader 20 with antenna 24 are integrated into a single hand-held portable computing device, such as a smartphone or PDA with built-in RFID reader, a Pocket PC with plug-in RFID reader card, and other computing devices with RFID capabilities. A smartphone is any electronic handheld device that integrates the functionality of a mobile phone, personal digital assistant or other information appliance.
[0037] An example plug-in RFID reader card is the Socket™ RFID Reader Card Series 6 from Socket Communications, Inc., of Newark, Calif. A Pocket PC, also referred to as a P/PC or PPC, is a handheld-sized portable computer that runs, for example, Microsoft Corporation's Windows CE® operating system. A Pocket PC has many capabilities of modern desktop personal computers. Pocket PCs can be used with many add-ons (e.g., plug-ins), like Global Positioning System (GPS) receivers, barcode readers, RFID readers and cameras.
[0038] Pocket PC with plug-in RFID reader card includes a processor 26 and memory 28 . Memory 28 includes an operating system 30 , such as Windows CE®, and a remote tracking process 200 , described below.
[0039] The RFID-based personnel tracking system 10 is used to keep track of the whereabouts and/or arrival and departure times of field-based employees, e.g. nurses, field technicians, delivery and repair personnel or the like, at various work sites, such as the homes of patients or the like. In such cases, a passive read-only RFID tag 22 is placed in each work site of interest. In one particular example, a trusted employee places the RFID tag in a known location for subsequent use by one or more non-trusted employees. For example, an RFID tag 22 can be affixed to a refrigerator door in a patient's home. Each field-based employee is assigned a user identification (ID) and a Pocket PC with plug-in RFID reader card. When a field-based employee is dispatched, upon arriving at the site the employee initiates the remote tracking process 200 on the employee's pocket PC with plug-in RFID reader. The remote tracking process 200 prompts the employee to scan the RFID tag 22 located at the site at initiation of the visit. After the employee scans the RFID tag, the remote tracking process 200 waits until the employee inputs an indication of a termination of the visit. Upon receiving the termination input from the employee, the remote tracking process 200 prompts the field-based employee to scan the RFID tag 22 . Once the RFID tag 22 is scanned, the remote tracking process 200 waits for the initiation of another remote visit by the field-based employee at another site or a signal indicating that all scheduled visits for the time period have been completed.
[0040] At periodic times, such as after each scan, once a day, once a week, or once a month, the field-based employee connects the pocket PC with RFID reader plug-in to a network access point, such as a telephone line. Remote tracking process 200 initiates communication with tracking/reporting process 100 in remote computer system 12 . Data stored in the pocket PC with respect to each RFID scanned during the period is transferred over the network access point, e.g., modem line, for processing by the tracking/reporting process 100 .
[0041] The tracking/reporting process 100 stores the data. The data can include (and be indexed by) a field-based employee identification (ID), site ID, start time of visit, end time of visit, date of visit, and so forth. The tracking/reporting process 100 can correlate dates and times against scheduled visits. The data is stored in remote computer system 12 for later use in developing reports and to insure that the field-based employee has been to the remote site where he or she has been prescheduled to appear. Alternatively, information that a certain field-based employee has appeared at other than the pre-designated location can be relayed immediately to an employer to whom receipt of such information might be valuable.
[0042] Once all data has been transferred from the particular pocket PC with RFID reader plug-in, the data can be used to generate one or more reports. For example, at a conclusion of each day and/or any other desired or predefined reporting period, tracking/reporting process 100 generates various reports for the employees of one or several companies, indicating and/or providing a list of dates, the arrival and departure times of each employee and the place where services have been performed. These reports can be stored in a database, for example. The information in the database can then forwarded to subscribers or users as hard copy output, electronically (e.g., email), and/or through a direct computer connection to remote computer system 12 (e.g., secure web site). The reports can be sent, for example, asynchronously, synchronously or through Wide Area Networks (WANs).
[0043] As shown in FIG. 2 , process 100 includes receiving ( 102 ) data from a computer system of a field-based employee. Data can be received, for example, over a modem/telephone line, a public network or a private network. Process 100 determines ( 104 ) a user identification associated with the received data and indexes ( 106 ) the received data by user identification for storage.
[0044] Process 100 correlates ( 108 ) date and time data against scheduled visits. The data is stored for later use in developing reports and to insure that the field-based employee associated with the user ID has been to the remote site where he or she has been prescheduled to appear. The reports can be viewed by a subscriber or emailed to a designated user address. Alternatively, information that a certain field-based employee has appeared at other than the pre-designated location can be relayed via email, for example, to an employer to whom receipt of such information might be valuable.
[0045] As shown in FIG. 3 , process 200 includes prompting ( 202 ) a user to enter a user identification (ID). The user ID identifies a unique field-based employee. Process 200 determines ( 204 ) whether the received user ID is valid. If the received user ID is invalid, process 200 signals ( 206 ) an error and prompts ( 202 ) the user to enter a user ID. If the received user ID is valid, process 200 prompts ( 208 ) the field-based employee to enter an option. If the inputted option represents initiation of a site visit, process 200 prompts ( 210 ) the user to scan an RFID tag located at the visited site.
[0046] After the field-based employee scans the RFID tag, process 200 stores ( 212 ), for example, a current date and time of the site visit initiation, as provided by the operating system of the field-based employee's handheld computer/RFID reader, a site identification from the RFID tag, and additional information, if needed.
[0047] If the inputted option represents a termination of the site visit, process 200 prompts ( 214 ) the user to scan an RFID tag located at the visited site. After the field-based employee scans the RFID tag, process 200 stores ( 216 ), for example, a current date and time of the site visit termination, as provided by the operating system of the field-based employee's handheld computer/RFID reader, a site identification from the RFID tag, and additional information, if needed.
[0048] If the inputted option represents reporting, process 200 connects ( 218 ) to a network and begins upload of the stored data to a remote computer system. Connecting ( 218 ) can be, for example, dialing a modem or linking over a public or private network.
[0049] Embodiments of the invention can be implemented in digital electronic circuitry, or in computer hardware, firmware, software, or in combinations of them. Embodiments of the invention can be implemented as a computer program product, i.e., a computer program tangibly embodied in an information carrier, e.g., in a machine readable storage device or in a propagated signal, for execution by, or to control the operation of, data processing apparatus, e.g., a programmable processor, a computer, or multiple computers. A computer program can be written in any form of programming language, including compiled or interpreted languages, and it can be deployed in any form, including as a stand alone program or as a module, component, subroutine, or other unit suitable for use in a computing environment. A computer program can be deployed to be executed on one computer or on multiple computers at one site or distributed across multiple sites and interconnected by a communication network.
[0050] Method steps of embodiments of the invention can be performed by one or more programmable processors executing a computer program to perform functions of the invention by operating on input data and generating output. Method steps can also be performed by, and apparatus of the invention can be implemented as, special purpose logic circuitry, e.g., an FPGA (field programmable gate array) or an ASIC (application specific integrated circuit).
[0051] Processors suitable for the execution of a computer program include, by way of example, both general and special purpose microprocessors, and any one or more processors of any kind of digital computer. Generally, a processor will receive instructions and data from a read only memory or a random access memory or both. The essential elements of a computer are a processor for executing instructions and one or more memory devices for storing instructions and data. Generally, a computer will also include, or be operatively coupled to receive data from or transfer data to, or both, one or more mass storage devices for storing data, e.g., magnetic, magneto optical disks, or optical disks. Information carriers suitable for embodying computer program instructions and data include all forms of non volatile memory, including by way of example semiconductor memory devices, e.g., EPROM, EEPROM, and flash memory devices; magnetic disks, e.g., internal hard disks or removable disks; magneto optical disks; and CD ROM and DVD-ROM disks. The processor and the memory can be supplemented by, or incorporated in special purpose logic circuitry.
[0052] It is to be understood that the foregoing description is intended to illustrate and not to limit the scope of the invention, which is defined by the scope of the appended claims. Other embodiments are within the scope of the following claims. | Methods and apparatus, including computer program products, for RFID-based personnel tracking. A method of tracking employees includes, in a first computer system, prompting a user for identification input, validating the identification input, receiving data from a first scan of a Radio Frequency Identification (RFID) tag upon initiation of a task, receiving data from a second scan of the RFID tag upon termination of the task, and uploading the identification input and the data of the first and second scans to a second computer system for storage and correlation. | 6 |
TECHNICAL FIELD
[0001] The application relates generally to casement windows and, more particularly, to a motorized window latching system.
BACKGROUND OF THE ART
[0002] Casement windows are well known. Such windows typically have one or more window sash pivotable about a vertical axis between an open and a closed position. A latch bar is commonly employed to lock the window sash in its closed position in tight sealing engagement against the window frame. Such latch bars generally include a flat steel strip having various latch points therealong for engagement with corresponding keepers provided along an edge of the associated window sash. The latch bar is typically manually actuated by a pivotable lever or lock handle.
[0003] Heretofore, the motorization of casement window latch mechanisms has been challenging. In most instances, access to the window latch bar is difficult and there is very little room to position the motorized operator. Also the motorized latch operator must not adversely affect the aesthetic of the window in order for the product to gain commercial acceptance.
[0004] There is thus a need for a compact motorized latch operator that can be integrated into a casement window without adversely affecting the appearance thereof.
SUMMARY
[0005] It is therefore an object to provide a compact motorized latch operator that can be integrated to a casement window.
[0006] In one aspect, there is provided a motorized latch operator adapted to be retrofitted to a normally manually operated latching assembly of a casement window mounted in a building wall, the casement window having at least one window sash hingedly mounted in a casement for pivotal movement about a vertical axis between open and closed positions, keepers being provided along one side of the window sash for engagement with corresponding latches mounted on a vertical side frame member of the casement, the latches being operatively interconnected by a vertical latch bar mounted for longitudinal movement in a gap defined between the side frame member and a moulding member; the motorized operator comprising a reversible rotary motor mounted in one of an internal cavity of the casement and a cavity in the building wall next to the casement, a vertically supported lead screw drivingly connected to the reversible rotary motor, a slider threadably engaged on the lead screw and constrained to up and down linear movement in response to rotation of the lead screw by the reversible rotary motor, the slider being connectable to the lock bar to transmit the linear movement imparted to the slider by the lead screw to the lock bar in order to actuate the latches of the casement window.
[0007] In a second aspect, there is provided a power-operated latch assembly for a casement window mounted in a building wall, the casement window having at least one window sash hingedly mounted in a window frame for pivotal movement about a vertical axis between open and closed positions; the power-operated latch assembly comprising at least two keepers mounted to the window sash for locking engagement with corresponding latches operated by a latch bar mounted for vertical movement along one vertical member of the window frame, a reversible operator mountable in one of a cavity defined in the building wall and an internal cavity defined in the window frame, a vertical push and pull rod disposed axially next to the latch bar, the push and pull rod being drivingly connected to the reversible operator, and a link between the push and pull rod and the latch bar, the link transferring the movement communicated to the push and pull rod to the latch bar.
[0008] In a third aspect, there is provided a casement window comprising at least one window sash hingedly mounted in a window frame for pivotal movement about a vertical axis between open and closed positions, a power-operated latch mechanism for releasably locking the at least one window sash in the closed position, the power-operated latch mechanism comprising at least two keepers mounted to the window sash for locking engagement with corresponding latches operated by a latch bar mounted for vertical movement along one vertical member of the window frame, a reversible rotary motor mounted in one of a cavity defined in the building wall and an internal cavity defined in the window frame, a vertically supported lead screw drivingly connected to the reversible rotary motor, a vertically displaceable slider threadably engaged on the lead screw for linear movement therealong, and a link between the slider and the latch bar, the link transferring the movement communicated to the slider to the latch bar.
[0009] Further details of these and other aspects of the present invention will be apparent from the detailed description and figures included below.
DESCRIPTION OF THE DRAWINGS
[0010] Reference is now made to the accompanying figures, in which:
[0011] FIG. 1 is a perspective view of a double hung casement type window as seen from inside a room and having a motorized unlatching system mounted inside the central profiled post of the window casement, the front vertical moulding normally covering the central profiled post being omitted to reveal the normally hidden motorized unlatching system;
[0012] FIG. 2 is a perspective view of the motorized unlatching system together with the window original latching hardware shown in isolation;
[0013] FIG. 3 is a cross-sectional view taken along line 3 - 3 in FIG. 1 ;
[0014] FIG. 4 is a longitudinal cross-sectional view illustrating the motorized unlatching system in position in the central profiled post of the window casement;
[0015] FIG. 5 is a perspective view of another model of double hung casement type window, the vertical moulding along one side of the central post of the window being broken away to show part of a motorized latching system;
[0016] FIG. 6 is a vertical cross-sectional view illustrating the details of the motorized latching system of FIG. 5 ;
[0017] FIG. 7 is a perspective view of a single hung casement window, the vertical moulding along one side of the window frame being omitted to reveal details of a motorized latching system connected to the original manual latching system of the window; and
[0018] FIG. 8 is vertical cross-sectional view illustrating the details of the motorized latching system shown in FIG. 7 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0019] FIG. 1 illustrates a first example of a conventional casement window 10 to which a motorized latching system or operator 12 can be integrated or retrofitted to provide for motorized latching and unlatching of the window. The illustrated exemplary casement window 10 is of conventional double hung casement type comprising a pair of window sashes 14 hingedly mounted in a casement 16 for pivotal movement between open and closed positions about mobile vertical axes at opposite sides of the casement 16 .
[0020] The casement window 10 is provided with latching hardware to releasably secure the window sashes 14 in their closed position. The latching hardware can comprise a plurality of keepers 18 (two in the illustrated example) on each window sash 14 for engagement with corresponding attachment points or latches 20 mounted on opposed longitudinal exterior sides of the central profiled post 22 of the casement 16 . The latches 20 capture the keepers 18 and operation of the latches 20 draw the corresponding window sash 14 into its closed position where it is locked. In the closed position, the window sash 14 is seated in the frame and compresses weather stripping (not shown) to seal the window assembly. In the illustrated example, the latches of each set of latches 20 are interconnected by a latch bar 24 adapted to transmit the movement from one latch to another, thereby allowing for joint operation of the latches 20 of a same set. The latch bars 24 are typically made from flat steel strips mounted for linear sliding movement against the exterior longitudinal sides of the central profiled post 22 of the casement 16 .
[0021] Instead of manually actuating the interconnected latches 20 via a conventional lever or handle provided at one of the latching points on each side of the central profiled post 22 , it is herein proposed to nest a power-operated or motorized latch actuator system 12 in an existing frontal opening defined in the central profiled post 22 and to connect the system 12 directly to the existing latch bars 24 on each side of the central profiled post 22 . Once installed, the motorized system 12 is hidden behind the front moulding (not shown) normally covering the post 22 when viewed from inside the room in which the window is mounted. By taking advantage of the existing free internal space offered by the central profiled post 22 , it is possible to completely conceal the system 12 within the window casement 16 , thereby preserving the overall appearance of the window.
[0022] As best shown in FIG. 2 , the system 12 generally comprises at least one reversible actuator, such as electrical reversible rotary motor 26 , a push and pull rod which can take the form of a lead screw 28 drivingly connected to the motor 26 , a slider 30 threadably engaged on the lead screw 28 for linear movement within the profiled post 22 ( FIG. 1 ) in the upward and the downward directions, and a pair of link plates 32 mounted to opposed sides of the slider 30 in order to rigidly connect the slider 30 to the lock bars 24 of the window 10 . An example of a suitable actuator is the 12 DVC E Type Inline DC Gearmotor Model No. 8501 manufactured by Merkle-Korff Industries. The dimensions of the selected actuator must allow the same to be fully contained within the central profiled post 22 . The motor 26 is connected to a source of power (not shown), such as a battery. The lead screw 28 can consist of a stainless steel screw with ACME threads. The slider 30 can be manufactured in a block of polytetrafluoroethylene or from another solid block of low friction material in order to minimize the friction between the lead screw 28 and the slider 30 .
[0023] The system 12 further comprises a support 36 for supporting the motor 26 and the lead screw 28 and facilitating mounting of the system 12 within the central profiled post 22 of the casement window. The support 36 comprises an elongated back 38 and top and bottom L-shaped plates 40 and 42 mounted at opposed ends of the elongated back 38 . The elongated back 38 provides a mounting surface for fixedly mounting the system 12 into central profiled post 22 of the casement 16 . Holes can be defined through the back of the support 36 for receiving mounting screws or the like. The motor 26 is mounted to the undersurface of the bottom L-shaped plate 42 . A support block 44 having a screw receiving hole depends from the top L-shaped plate 40 for receiving a tip end portion of the lead screw 28 . Limit switches 46 a, 46 b and 46 c are mounted to the front face of the support back 38 above and below the slider 30 . Projections 48 a, 48 b, 48 c, such as screws, are provided on the top and bottom surfaces of the slider 30 to trigger the limit switches 46 a, 46 b and 46 c when the slider 30 reaches its top and bottom travel limits. The limit switches 46 a, 46 c are operatively connected to the motor 26 to shut down the same and reverse the direction of movement once triggered by a corresponding one of the triggering projections 48 a, 48 c, thereby defining the range of motion or stroke of the slider 30 on the lead screw 28 . The third limit switch 46 b is used as an interlock. The limit switch 46 b is provided to prevent the motor (not shown) used to displace the window sashes 14 between their open and closed positions from being operated when the latches 20 are engaged with the keepers 18 . It is provided to “sense” the lock state of the window sashes. It can also be used to prevent the motor 26 of the power operated latching system from being operated when the window sashes are opened.
[0024] The motor 26 , the lead screw 28 , the slider 30 , the support block 44 and the limit switches 46 a, 46 b, 46 c are pre-assembled on the support 36 and this sub-assembly is mounted within the central profiled post 22 , such as by screwing the support back 38 to a corresponding back surface of the casement window central profiled post 22 . As shown in FIG. 4 , the central post 22 is provided in the form of an extrusion having a generally C-shaped profile with a front open face. The central post 22 has a frontal recess defined by sidewall surfaces 50 and inwardly projecting frontal wall surfaces 52 . The slider 30 has a generally T-shaped body including a rearwardly projecting shank portion 54 and lateral shoulders 56 . The shank portion 54 is received between the frontal wall surfaces 52 of the profiled post 22 with the lateral shoulders 56 resting against a front side of the frontal wall surfaces 52 between said sidewall surfaces 50 . This arrangement prevents the slider 30 from rotating together with the lead screw 28 . The slider 30 is thus constrained to move linearly in the upward or the downward direction depending whether the motor 26 is rotatably driving the lead screw 28 in the clockwise or the counter-clockwise direction.
[0025] Still referring to FIG. 4 , it can be appreciated that the lock bars 24 interconnecting the latches 20 ( FIG. 1 ) are guided in vertical tracks defined at the outer sides of the central profiled post 22 . The link plates 32 are positioned laterally outwardly from the sidewall surfaces 50 of the post 22 and are fixedly attached to the lock bars 24 by fasteners such as screws or the like. Vertically elongated slots 58 had to be machined (also see FIG. 3 ) in the post sidewall surfaces 50 for allowing the link plates 32 to be rigidly connected to the slider 30 by means of shoulder screws 57 . In this way, the linear movement of the slider 30 inside the post 22 can be simultaneously transmitted to both latch bars 24 on the opposed sides of the central profiled post 22 . The length of the elongated slots 58 is selected to accept the full stroke of the slider 30 as set by the position of the limit switches 46 .
[0026] In use, a remote control can be used to operate the system 12 . A wireless control receiver (not shown) can be mounted in the building wall underneath the window frame for receiving control commands and transmitting same to the electric motor 26 . The rotational movement of the lead screw 28 causes the linear displacement of the slider 30 which in turn push or pull on the lock bars 24 (depending in which direction the screw is rotated) to actuate the latches 20 in order to lock or unlock the window.
[0027] If more torque is required to operate the latches, a second motor and a second lead screw could be added to the above described latch operator assembly. The second motor could be mounted to the top L-shaped plate 40 of the support with the second lead screw laterally offset with respect to the first lead screw 28 . The motors would be synchronized but operated to drive the first and second lead screws in opposed directions.
[0028] FIGS. 5 and 6 illustrate another example of the integration of a motorized latch actuation system 12 ′ to a double hung type casement window 10 ′ but this time for a model of window having a solid central post 22 ′ having no internal cavity in which the above described components of the motorized latching system could potentially be mounted. The only space available to access the lock bars 24 ′ is the ¾ inch to 1 inch gap existing between the central post 22 ′ and the vertical moulding 23 on each side of the post 22 ′. This does not leave enough room to accommodate the motor.
[0029] The motor 26 ′ had thus to be disposed in a rectangular wooden box or casing 27 mounted to the casement 16 ′ underneath sill 29 . The casing 27 forms a hollow window frame extension for receiving window operator equipment and the like. The motor 26 ′ is thus concealed in the building wall below the original window frame. The dimensions of the casing 27 , notably the height thereof, are greatly limited by the presence of the structural or skeleton members of the building wall in which the window is mounted. In view of the small space available underneath the casement window 10 ′, the motor 26 ′ is horizontally disposed in the casing 27 and a universal joint 31 is used to connect the motor 26 ′ to the lead screw 28 ′ extending vertically along the side of the central post 22 ′ in the gap defined between the side moulding 23 and the central window post 22 ′.
[0030] The lead screw 28 ′ extends through a hole 33 defined in the window sill 29 and is vertically supported by a bottom support block 37 mounted to the central post 22 ′ underneath the sill of the window 10 ′. As shown in FIG. 6 , the lead screw 28 ′ has a shoulder resting on top of the bottom block 37 to prevent the screw 28 ′ from sliding downwardly under gravity into the lead screw passage defined in the bottom block 37 . The upper end or tip of the lead screw 28 ′ is received in a hole defined in a top support 44 ′ screwed or otherwise secured to the side of the central post 22 ′. The top support 44 ′ is also contained in the gap between the post 22 ′ and the moulding 23 .
[0031] The limit switches 46 a ′, 46 b ′ and 46 c ′ are also directly mounted to the side of the post 22 ′ below the internally threaded slider 30 ′ mounted on the lead screw 28 ′ in the gap between the post 22 ′ and the moulding 23 . A L-shaped triggering finger 39 extends downwardly from the slider 30 ′ for triggering the limit switches 46 a ′, 46 b ′ and 46 c ′ when the slider 30 ′ reaches the end of its stroke.
[0032] The mounting of the slider 30 ′ against the side wall of the central post 22 ′ locks the slider 30 ′ against rotation and constrains the slider 30 ′ to move linearly along the side wall of the post 22 ′ in response to the rotation of the lead screw 28 ′. An elongated strip or rod 41 extends upwardly from a post facing side of the slider 30 ′ in order to rigidly connect the same to the existing lock bar 24 ′ interconnecting the latches 20 ′ of the window 10 ′. The linear movement of the slider 30 ′ on the lead screw 28 ′ can thus be transferred to the existing lock bar 24 ′ in order to latch and unlatch the window.
[0033] It is understood that a similar motorized latch operator is provided on the other side of the central post to operate the lock bar interconnecting the latches associated to the second window sash (not shown).
[0034] FIGS. 7 and 8 illustrate another example of the integration of a motorized latch actuation system 12 ″ to an originally manually actuated latching system of a single hung type casement window 10 ″. In this example, the window lock bar 24 ″ interconnecting the latches 20 ″ on one side of the window frame is disposed further towards the outside of the room in which the window is mounted. The casing 27 ″ secured underneath the window frame in the building wall and holding the motor 26 ′ is not aligned with the lock bar 24 ″. The casing 27 ″ is located further towards the inside of the room relative to the lock bar 24 ″. As will be seen herein after, this misalignment problem is overcome by connecting the motorized system 12 ″ to an existing link 70 originally joined to the lever/handle (not shown) of the lower manual latch 20 ″.
[0035] As shown in FIG. 8 , the motor 26 ′ is horizontally mounted in casing 27 ″ which is disposed in the building wall underneath the window frame. The motor 26 ″ is drivingly connected to a vertically disposed lead screw 28 ″ via universal joint 31 ″. The lead screw 28 ″ extends through a hole defined in the window sill and has a top head 71 retained captive between a base 72 and a cover 74 . The base 72 and the cover 74 are made of a low friction material and are used to support the lead screw 28 ″ in position. The base 72 is mounted on a top surface of the window sill and has a through bore defined therein for allowing the lead screw 28 ″ to pass therethrough. A recess is defined in a top surface of the base 72 for receiving a split washer 76 . The washer 76 is mounted about the lead screw 28 ″ underneath head 71 . The cover 74 has a recess defined in an undersurface thereof for accommodating the screw head 71 and is screwed or otherwise suitably secured to the base 72 . A horizontal moulding (not shown) covers the sill of the window to conceal the base 72 and the cover 74 .
[0036] A low frictional material rectangular sleeve 78 is installed in the hole defined in the window sill to provide for smoothly guided movement of slider 30 ″ on the lead screw 28 ″. The sleeve 78 is configured to lock the slider 30 ″ against rotation while providing for smooth linear gliding movement therein. An elongated flattened rod or strip 80 is attached to the slider 30 ″ and extends vertically upwardly through aligned slotted holes defined in the base 72 and cover 74 . The upper end of the strip 80 is pivotally connected to existing link 70 which is, in turn, connected to the lock bar 24 ″ joining all the latches 20 ″ of the window. The pull and push strip 80 can be guided at the upper end thereof by a guide 82 mounted to the side member of the window frame on which the latches 20 ″ are mounted. The vertical moulding (not shown) of the side member of the window frame conceal all the mechanism disposed therealong.
[0037] As shown in FIG. 7 , the limit switches 46 a ″, 46 b ″, 46 c ″ are mounted on the side of the frame next to the upper latch 20 ″ so as to be triggered by the components thereof.
[0038] The above description is meant to be exemplary only, and one skilled in the art will recognize that changes may be made to the embodiments described without departing from the scope of the invention disclosed. Modifications which fall within the scope of the present invention will be apparent to those skilled in the art, in light of a review of this disclosure, and such modifications are intended to fall within the appended claims. | A power-operated latch is integrated to a casement window for selectively locking and unlocking a vertically hinged window sash. The power-operated latch is adapted to be concealed in the window frame and is directly connectable to the existing window latch hardware. A reversible rotary motor drives a vertically supported lead screw on which a slider is threadably engaged for selectively raising and lowering a longitudinally movable latch bar. | 4 |
This is a divisional of application Ser. No. 08/042,302, filed on Apr. 2, 1993, now U.S. Pat. No. 5,371,076.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to novel [4S-(4α,4aα,5 α,5aα,6α,12aα)]-4-(dimethylamino)-6-(substituted)-9-[[(substituted amino)substituted]amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-1,11-dioxo-2-naphthacenecarboxamides herein after called 9-[(substituted glycyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracyclines, which exhibit antibiotic activity against a wide spectrum of organisms including organisms which are resistant to tetracyclines and are useful as antibiotic agents.
The invention also relates to novel 9-[(haloacyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracycline and novel 9-[(protected aminoacyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracycline intermediates useful for making the novel compounds of the present invention and to novel methods for producing the novel compounds and intermediate compounds.
SUMMARY OF THE INVENTION
This invention is concerned with novel 9-[(substituted glycyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracyclines, represented by formula I, which have antibacterial activity; with methods of treating infectious diseases in warm blooded animals employing these new compounds; with pharmaceutical preparations containing these compounds; with novel intermediate compounds and processes for the production of these compounds. More particularly, this invention is concerned with compounds of formula I which have antibacterial activity against tetracycline resistant strains as well as a high level of activity against strains which are normally susceptible to tetracyclines. ##STR2##
In formula I,
R is selected from methylene, α-CH 3 and β-CH 3 ;
R 1 is selected from hydrogen; straight or branched (C 1 -C 8 )alkyl group selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, hexyl, heptyl and octyl; straight or branched (C 1 -C 8 )alkyl group optionally substituted with α-mercapto, α-(methylthio), α-hydroxy, carboxyl, carboxamido, amino, guanidino or amidino; (C 6 -C 10 )aryl group selected from phenyl, α-naphthyl and β-naphthyl; substituted (C 6 -C 10 )aryl group substitution selected from hydroxy, halogen, (C 1 -C 4 )alkoxy, trihalo(C 1 -C 3 ) alkyl, nitro, amino, cyano, (C 1 -C 4 )alkoxycarbonyl, (C 1 -C 3 )alkylamino and carboxy; (C 7 -C 9 )aralkyl group selected from benzyl, 1-phenylethyl, 2-phenylethyl and phenylpropyl; substituted(C 7 -C 9 )aralkyl group substitution selected from halo, (C 1 -C 4 )alkyl, nitro, hydroxy, amino, mono- or di-substituted (C 1 -C 4 )alkylamino, (C 1 -C 4 )alkoxy, (C 1 -C 4 )alkylsulfonyl, cyano and carboxy; (heterocycle)methyl group said heterocycle selected from 4-(or 3-)imidazolyl, 4-(3-)oxazolyl, 3-(or 2-)indolyl, 2-(or 3-) furanyl, 2-(or 3-)thienyl, 2-(or 3-)pyrrolyl, 2-(or 3-)pyrazolyl, 4-(1,2,3-triazolyl) and benzimidazolyl; (C 3 -C 6 )cycloalkylmethyl group selected from (cyclopropyl)methyl, (cyclobutyl)methyl, (cyclopentyl)methyl and (cyclohexyl)methyl;
R 2 is selected from hydrogen and (C 1 -C 6 )alkyl selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl and hexyl;
W is selected from amino; hydroxylamino; (C 1 -C 12 ) straight or branched alkyl monosubstituted amino group substitution selected from methyl, ethyl, n-propyl, 1-methylethyl, n-butyl, 1-methylpropyl, 2-methylpropyl, 1,1-dimethylethyl, n-pentyl, 2-methylbutyl, 1,1-dimethylpropyl, 2,2-dimethylpropyl, 3-methylbutyl, n-hexyl, 1-methylpentyl, 1,1-dimethylbutyl, 2,2-dimethylbutyl, 3-methylpentyl, 1,2-dimethylbutyl, 1,3-dimethylbutyl, 1-methyl-1-ethylpropyl, heptyl, octyl, nonyl, decyl, undecyl and dodecyl and the diastereomers and enantiomers of said branched alkyl monosubstituted amino group; (C 3 -C 8 )cycloalkyl monosubstituted amino group substitution selected from cyclopropyl, trans-1,2-dimethylcyclopropyl, cis-1,2-dimethylcyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl, cyclooctyl, bicyclo[2.2.1]hept-2-yl, and bicyclo[2.2.2]oct-2-yl and the diastereomers and enantiomers of said (C 3 -C 8 )cycloalkyl monosubstituted amino group; [(C 4 -C 10 )cycloalkyl](C 1 -C 3 )alkyl monosubstituted amino group substitution selected from (cyclopropyl)methyl, (cyclopropyl)ethyl, (cyclobutyl)methyl, (trans-2-methylcyclopropyl)methyl, and (cis-2-methylcyclobutyl)methyl; (C 3 -C 10 )alkenyl monosubstituted amino group substitution selected from allyl, 3-butenyl, 2-butenyl (cis or trans), 2-pentenyl, 4-octenyl, 2,3-dimethyl-2-butenyl, 3-methyl-2-butenyl, 2-cyclopentenyl and 2-cyclohexenyl; (C 6 -C 10 )aryl monosubstituted amino group substitution selected from phenyl and naphthyl; (C 7 -C 10 )aralkylamino group selected from benzyl, 2-phenylethyl, 1-phenylethyl, 2-(naphthyl)methyl, 1-(naphthyl)methyl and phenylpropyl; substituted phenyl amino group substitution selected from (C 1 -C 5 )acyl, (C 1 -C 5 )acylamino, (C 1 -C 4 )alkyl, mono or disubstituted (C 1 -C 8 )alkylamino, (C 1 -C 4 )alkoxy, (C 1 -C 4 )alkoxycarbonyl, (C 1 -C 4 )alkylsulfonyl, amino, carboxy, cyano, halogen, hydroxy, nitro and trihalo(C 1 -C 3 )alkyl; straight or branched symmetrical disubstituted (C 2 -C 8 )alkylamino group substitution selected from dimethyl, diethyl, diisopropyl, di-n-propyl, di-n-butyl and diisobutyl; symmetrical disubstituted (C 3 -C 14 )cycloalkylamino group substitution selected from dicyclopropyl, dicyclobutyl, dicyclopentyl, dicylohexyl and dicycloheptyl; straight or branched unsymmetrical disubstituted (C 3 -C 14 )alkylamino group wherein the total number of carbons in the substitution is not more than 14; unsymmetrical disubstituted (C 4 -C 14 )cycloalkylamino group wherein the total number of carbons in the substitution is not more than 14; (C 2 -C 8 )azacycloalkyl and substituted (C 2 -C 8 )azacycloalkyl group selected from aziridinyl, azetidinyl, pyrrolidinyl, piperidinyl, 4-methylpiperidinyl, 2-methylpyrrolidinyl, cis-3,4-dimethylpyrrolidinyl, trans-3,4-dimethylpyrrolidinyl, 2-azabicyclo[2.1.1]hex-2-yl, 5-azabicyclo[2.1.1]hex-5-yl, 2-azabicyclo[2.2.1]hept-2-yl, 7-azabicyclo[2.2.1]hept-7-yl, and 2-azabicyclo[2.2.2]oct-2-yl and the diastereomers and enantiomers of said (C 2 -C 8 )azacycloalkyl and substituted (C 2 -C 8 )azacycloalkyl group; 1-azaoxacycloalkyl group selected from morpholinyl and 1-aza-5-oxocycloheptane; substituted 1-azaoxacycloalkyl group substitution selected from 2-(C 1 -C 3 )alkylmorpholinyl, 2-(C 3 -C 6 )cycloalkylmorpholinyl, 3-(C 1 -C 3 )alkylisooxazolidinyl, tetrahydrooxazinyl and 3,4-dihydrooxazinyl; [1,n]-diazacycloalkyl and substituted [1,n]-diazacycloalkyl group selected from piperazinyl, 2-(C 1 -C 3 )alkylpiperazinyl, 2-(C 3 -C 6 )cycloalkylpiperazinyl, 4-(C 1 -C 3 )alkylpiperazinyl, 2,4-dimethylpiperazinyl, 4-(C 1 -C 4 )alkoxypiperazinyl, 4-(C 6 -C 10 )aryloxypiperazinyl, 4-hydroxypiperazinyl, 2,5-diazabicyclo[2.2.1]hept-2-yl, 2,5-diaza-5-methylbicyclo[2.2.1]hept-2-yl, 2,3-diaza-3-methylbicyclo[2.2.2]oct-2-yl, and 2,5-diaza-5,7-dimethylbicyclo[2.2.2]oct-2-yl and the diastereomers or enantiomers of said [1,n]-diazacycloalkyl and substituted [1,n]-diazacycloalkyl group; 1-azathiacycloalkyl and substituted 1-azathiacycloalkyl group selected from thiomorpholinyl, 2-(C 1 -C 3 )alkylthiomorpholinyl and 3-(C 3 -C 6 )cycloalkylthiomorpholinyl; N-azolyl and substituted N-azolyl group selected from 1-imidazolyl, 2-(C 1 -C 3 )alkyl-1-imidazolyl, 3-(C 1 -C 3 )alkyl-1-imidazolyl, 1-pyrrolyl, 2-(C 1 -C 3 )alkyl-1-pyrrolyl, 3-(C 1 -C 3 )alkyl-1-pyrrolyl, 1-pyrazolyl, 3-(C 1 -C 3 )-alkyl-1-pyrazolyl, indolyl, 1-(1,2,3-triazolyl), 4-(C 1 -C 3 )alkyl-1-(1,2,3-triazolyl), 5-(C 1 -C 3 )alkyl-1-(1,2,3-triazolyl), 4-(1,2,4-triazolyl, 1-tetrazolyl, 2-tetrazolyl and benzimidazolyl; (heterocycle) amino group said heterocycle selected from 2- or 3-furanyl, 2- or 3-thienyl, 2-, 3- or 4-pyridyl, 2- or 5-pyridazinyl, 2-pyrazinyl, 2-(imidazolyl), (benzimidazolyl), and (benzothiazolyl) and substituted (heterocycle)amino group (substitution selected from straight or branched (C 1 -C 6 )alkyl); (heterocycle)methylamino group selected from 2- or 3-furylmethylamino, 2- or 3-thienylmethylamino, 2-, 3- or 4-pyridylmethylamino, 2- or 5-pyridazinylmethylamino, 2-pyrazinylmethylamino, 2- (imidazolyl)methylamino, (benzimidazolyl)methylamino, and (benzothiazolyl)methylamino and substituted (heterocycle)methylamino group (substitution selected from straight or branched (C 1 -C 6 )alkyl); carboxy(C 2 -C 4 )alkylamino group selected from aminoacetic acid, α-aminopropionic acid, β-aminopropionic acid, α-butyric acid, and β-aminobutyric acid and the enantiomers of said carboxy (C 2 -C 4 )alkylamino group; (C 1 -C 4 )alkoxycarbonylamino group selected from methoxycarbonylamino, ethoxycarbonylamino, allyloxycarbonylamino, propoxycarbonylamino, isoproproxycarbonylamino, 1, 1-dimethylethoxycarbonylamino, n-butoxycarbonylamino, and 2-methylpropoxycarbonylamino; (C 1 -C 4 )alkoxyamino group selected from methoxyamino, ethoxyamino, n-propoxyamino, 1-methylethoxyamino, n-butoxyamino, 2-methylpropoxyamino, and 1,1-dimethylethoxyamino; (C 3 -C 8 )cycloalkoxyamino group selected from cyclopropoxy, trans-1, 2-dimethylcyclopropoxy, cis-1,2-dimethylcyclopropoxy, cyclobutoxy, cyclopentoxy, cyclohexoxy, cycloheptoxy, cyclooctoxy, bicyclo[2.2.1]hept-2-yloxy, and bicyclo[2.2.2]oct-2-yloxy and the diastereomers and enantiomers of said (C 3 -C 8 )cycloalkoxyamino group; (C 6 -C 10 )aryloxyamino group selected from phenoxyamino, 1-naphthyloxyamino and 2-naphthyloxyamino; (C 7 -C 11 )arylalkoxyamino group substitution selected from benzyloxy, 2-phenylethoxy, 1-phenylethoxy, 2-(naphthyl)methoxy, 1-(naphthyl)methoxy, and phenylpropoxy; or R 1 and W taken together are --CH 2 (CH 2 ) n CH 2 NH--, wherein n=1-3;
and the pharmacologically acceptable organic and inorganic salts or metal complexes. It will be appreciated that when R 1 does not equal R 2 the stereochemistry of the asymmetric carbon (i.e. the carbon bearing the W substituent) maybe be either the racemate (DL) or the individual enantiomers (L or D).
Preferred compounds are compounds according to the above formula I, wherein:
R is selected from methylene, α-CH 3 and β-CH 3 ;
R 1 is selected from hydrogen; straight or branched (C 1 -C 8 )alkyl group selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, hexyl, heptyl and octyl; straight or branched (C 1 -C 8 )alkyl group optionally substituted with α-mercapto, α-(methylthio), α-hydroxy, carboxyl, carboxamido, amino, guanidino or amidino; (C 6 -C 10 )aryl group selected from phenyl, α-naphthyl and β-naphthyl; (C 7 -C 9 )aralkyl group selected from benzyl, 1-phenylethyl, 2-phenylethyl and phenylpropyl; substituted(C 7 -C 9 )aralkyl group substitution selected from halo, (C 1 -C 4 )alkyl, nitro, hydroxy, amino, mono- or di-substituted (C 1 -C 4 )alkylamino, (C 1 -C 4 )alkoxy, (C 1 -C 4 )alkylsulfonyl, cyano and carboxy; (heterocycle)methyl group said heterocycle selected from 4-(or 3-)imidazolyl, 4-(or 3-)oxazolyl, 3-(or 2-)indolyl, 2-(or 3-)furanyl, 2-(or 3-)thienyl, 2-(or 3-)pyrrolyl and 2-(or 3-)pyrazolyl; (C 3 -C 6 )cycloalkylmethyl group selected from (cyclopropyl)methyl, (cyclobutyl)methyl, (cyclopentyl)methyl and (cyclohexyl)methyl;
R 2 is selected from hydrogen and (C 1 -C 6 )alkyl selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl and hexyl;
W is selected from amino; hydroxylamino; (C 1 -C 12 ) straight or branched alkyl monosubstituted amino group substitution selected from methyl, ethyl, n-propyl, 1-methylethyl, n-butyl, 1-methylpropyl, 2-methylpropyl, 1,1-dimethylethyl, n-pentyl, 2-methylbutyl, 1,1-dimethylpropyl, 2,2-dimethylpropyl, 3-methylbutyl, n-hexyl, 1-methylpentyl, 1,1-dimethylbutyl, 2,2-dimethylbutyl, 3-methylpentyl, 1,2-dimethylbutyl, 1,3-dimethylbutyl, 1-methyl-1-ethylpropyl, heptyl, octyl, nonyl, decyl, undecyl and dodecyl and the diastereomers and enantiomers of said branched alkyl monosubstituted amino group; (C 3 -C 8 )cycloalkyl monosubstituted amino group substitution selected from cyclopropyl, trans-1,2-dimethylcyclopropyl, cis-1,2-dicyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl, cyclooctyl, bicyclo[2.2.1]hept-2-yl, and bicyclo[2.2.2]oct-2-yl and the diastereomers and enantiomers of said (C 3 -C 8 )cycloalkyl monosubstituted amino group; [(C 4 -C 10 )cycloalkyl] (C 1 -C 3 )alkyl monosubstituted amino group substitution selected from (cyclopropyl)-methyl, (cyclopropyl)ethyl, (cyclobutyl)methyl, (trans-2-methylcyclopropyl)methyl, and (cis-2-methylcyclobutyl)methyl; (C 3 -C 10 )alkenyl monosubstituted amino group substitution selected from allyl, 3-butenyl, 2-butenyl (cis or trans), 2-pentenyl, 4-octenyl, 2,3-dimethyl-2-butenyl, 3-methyl-2-butenyl 2-cyclopentenyl and 2-cyclohexenyl; (C 6 -C 10 )aryl monosubstituted amino group substitution selected from phenyl and naphthyl; (C 7 -C 11 )aralkylamino group selected from benzyl, 2-phenylethyl, 1-phenylethyl, 2-(naphthyl)methyl, 1-(naphthyl)methyl and phenylpropyl; straight or branched symmetrical disubstituted (C 2 -C 8 )alkylamino group substitution selected from dimethyl, diethyl, diisopropyl and di-n-propyl; symmetrical disubstituted (C 3 -C 14 )cycloalkylamino group substitution selected from dicyclopropyl, dicyclobutyl, dicyclopentyl, dicylohexyl and dicycloheptyl; straight or branched unsymmetrical disubstituted (C 3 -C 14 )alkylamino group wherein the total number of carbons in the substitution is not more than 14; unsymmetrical disubstituted (C 4 -C 14 )cycloalkylamino group wherein the total number of carbons in the substitution is not more than 14; (C 2 -C 8 )azacycloalkyl and substituted (C 2 -C 8 )azacycloalkyl group selected from aziridinyl, azetidinyl, pyrrolidinyl, piperidinyl, 4-methylpiperidinyl, 2-methylpyrrolidinyl, cis-3,4-dimethylpyrrolidinyl, trans-3,4-dimethylpyrrolidinyl, 2-azabicyclo[2.1.1]hex-2-yl, 5-azabicyclo[2.1.1]hex-5-yl, 2-azabicyclo[2.2.1]hept-2-yl, 7-azabicyclo[2.2.1]hept-7-yl, and 2-azabicyclo[2.2.2]oct-2-yl and the diastereomers and enantiomers of said (C 2 -C 8 )azacycloalkyl and substituted (C 2 -C 8 )azacycloalkyl group; 1-azaoxacycloalkyl group selected from morpholinyl and 1-aza-5-oxacycloheptane; substituted 1-azaoxacycloalkyl group selected from 2-(C 1 -C 3 )alkylmorpholinyl, 2-(C 3 -C 6 )cycloalkylmorpholinyl, 3-(C 1 -C 3 )alkylisoxazolidinyl, tetrahydrooxazinyl and 3,4-dihydrooxazinyl; [1,n]-diazacycloalkyl and substituted [1,n]-diazacycloalkyl group selected from piperazinyl, 2-(C 1 -C 4 )alkylpiperazinyl, 2-(C 3 -C 6 )cycloalkylpiperazinyl, 4-(C 1 -C 3 )alkylpiperazinyl, 2,4-dimethylpiperazinyl, 4-(C 1 -C 3 )alkoxypiperazinyl, 4-(C 6 -C 10 )-aryloxypiperazinyl, 4-hydroxypiperazinyl, 2,5-diaza-bicyclo[2.2.1]hept-2-yl, 2,5-diaza-5-methylbicyclo-[2.2.1]hept-2-yl, 2,3-diaza-3-methylbicyclo[2.2.2]-oct-2-yl, and 2,5-diaza-5,7-dimethylbicyclo[2.2.2]oct- 2-yl and the diastereomers or enantiomers of said [1,n]-diazacycloalkyl and substituted [1,n]-diazacycloalkyl group; 1-azathiacycloalkyl and substituted 1-azathiacycloalkyl group selected from thiomorpholinyl, 2-(C 1 -C 3 )alkylthiomorpholinyl and 3-(C 3 -C 6 )cycloalkylthiomorpholinyl; N-azolyl and substituted N-azolyl group selected from 1-imidazolyl, 2-(C 1 -C 3 )alkyl-1-imidazolyl, 3-(C 1 -C 3 )alkyl-1-imidazolyl, 1-pyrrolyl, 2-(C 1 -C 3 )alkyl-1-pyrrolyl, 3-(C 1 -C 3 )alkyl-1-pyrazolyl, 1-pyrazolyl, 3-(C 1 -C 3 )alkyl-1-pyrazolyl, indolyl, 1-(1,2,3-triazolyl), 4-alkyl-1-(1,2,3-triazolyl), 5-(C 1 -C 3 )alkyl-1-(1,2,3-triazolyl), 4-(1,2,4-triazolyl, 1-tetrazolyl, 2-tetrazolyl and benzimidazolyl; (heterocycle)amino group said heterocycle selected from 2- or 3-furanyl, 2- or 3-thienyl, 2-, 3- or 4-pyridyl, 2- or 5-pyridazinyl, 2-pyrazinyl, 2-(imidazolyl), (benzimidazolyl), and (benzothiazolyl) and substituted (heterocycle) amino group (substitution selected from straight or branched (C 1 -C 6 )alkyl); (heterocycle)methylamino group selected from 2- or 3-furylmethylamino, 2- or 3-thienylmethylamino, 2 -, 3 - or 4-pyridylmethylamino, 2 - or 5-pyridazinylmethylamino, 2-pyrazinylmethylamino, 2-(imidazolyl)methylamino, (benzimidazolyl) methylamino, and (benzothiazolyl)methylamino and substituted (heterocycle) methylamino group (substitution selected from straight or branched (C 1 -C 6 )alkyl); carboxy(C 2 -C 4 )alkylamino group selected from aminoacetic acid, α-aminopropionic acid, β-aminopropionic acid, α-butyric acid, and β-aminobutyric acid and the enantiomers of said carboxy(C 2 -C 4 )alkylamino group; (C 1 -C 4 )alkoxycarbonylamino group selected from methoxycarbonylamino, ethoxycarbonylamino, allyloxycarbonylamino, propoxycarbonylamino, isoproproxycarbonylamino, 1,1-dimethylethoxycarbonylamino, n-butoxycarbonylamino, and 2-methylpropoxycarbonylamino; (C 1 -C 4 )alkoxyamino group selected from methoxyamino, ethoxyamino, n-propoxyamino, 1-methylethoxyamino, n-butoxyamino, 2 -methylpropoxyamino, and 1,1-dimethylethoxyamino; (C 3 -C 8 )cycloalkoxyamino group substitution selected from cyclopropoxy, trans-1,2-dimethylcyclo-propoxy, cis-1,2-dimethylcyclopropoxy, cyclobutoxy, cyclopentoxy, cyclohexoxy, cycloheptoxy, cyclooctoxy, bicyclo[2.2.1]hept-2-yloxy, and bicyclo[2.2.2]oct-2-yloxy and the diastereomers and enantiomers of said (C 3 -C 8 )cycloalkoxyamino group; (C 6 -C 10 )aryloxyamino group selected from phenoxyamino, 1-naphthyloxyamino and 2-naphthyloxyamino; (C 7 -C 11 )arylalkoxyamino group substitution selected from benzyloxy, 2-phenylethoxy, 1-phenylethoxy, 2-(naphthyl)methoxy, 1-(naphthyl)methoxy and phenylpropoxy; or R 1 and W taken together are --CH 2 (CH 2 ) n CH 2 N--, wherein n=1-3;
and the pharmacologically acceptable organic and inorganic salts or metal complexes.
Particularly preferred compounds are compounds according to the above formula I, wherein:
R is selected from methylene, α-CH 3 and β-CH 3 ;
R 1 is selected from hydrogen; straight or branched (C 1 -C 8 )alkyl group selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, hexyl, heptyl and octyl; straight or branched (C 1 -C 8 )alkyl group optionally substituted with α-mercapto, α-hydroxy, carboxyl, carboxamido, or amino; (C 6 -C 10 )aryl group selected from phenyl, α-naphthyl and β-naphthyl; (C 7 -C 9 )aralkyl group selected from benzyl, 1-phenylethyl, 2-phenylethyl and phenylpropyl; (heterocycle)methyl group said hetrocycle selected from 4-(or 3-)imidazolyl, 4-(or 3-)oxazolyl, 3-(or 2-)indolyl, 2-(or 3-)furanyl and 2-(or 3-)thienyl; (C 3 -C 6 )cycloalkylmethyl group selected from (cyclopropyl)methyl, (cyclobutyl)methyl, (cyclopentyl)methyl and (cyclohexyl)methyl;
R 2 is selected from hydrogen and (C 1 -C 6 )alkyl selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl and hexyl;
W is selected from amino; (C 1 -C 12 ) straight or branched alkyl monosubstituted amino group substitution selected from methyl, ethyl, n-propyl, 1-methylethyl, n-butyl, 1-methylpropyl, 2-methylpropyl, 1,1-dimethylethyl, n-pentyl, 2-methylbutyl, 1,1-dimethylpropyl, 2,2-dimethylpropyl, 3-methylbutyl, n-hexyl, 1-methylpentyl, 1,1-dimethylbutyl, 2,2-dimethylbutyl, 3-methylpentyl, 1,2-dimethylbutyl, 1,3-dimethylbutyl, 1-methyl-1-ethylpropyl, heptyl, octyl, nonyl and decyl and the diastereomers and enantiomers of said branched alkyl monosubstituted amino group; (C 3 -C 8 )cycloalkyl monosubstituted amino group substitution selected from cyclopropyl, trans-1,2-dimethylcyclopropyl, cis-1,2-dimethylcyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl and cyclooctyl and the diastereomers and enantiomers of said (C 3 -C 8 )cycloalkyl monosubstituted amino group; [(C 4 -C 10 )cycloalkyl] (C 1 -C 2 )alkyl monosubstituted amino group substitution selected from (cyclopropyl)methyl, (cyclopropyl)ethyl and (cyclobutyl)methyl; (C 3 -C 10 )alkenyl monosubstituted amino group substitution selected from allyl, 3-butenyl, 2-butenyl (cis or trans), 2-pentenyl, 4-octenyl, 2,3-dimethyl-2-butenyl, 3-methyl-2-butenyl 2-cyclopentenyl and 2-cyclohexenyl; (C 7 -C 10 )aralkylamino group selected from benzyl, 2-phenylethyl, 1-phenylethyl, 2-(naphthyl)methyl, 1-(naphthyl)methyl and phenylpropyl; straight or branched symmetrical disubstituted (C 2 -C 8 )alkylamino group substitution selected from dimethyl, diethyl, diisopropyl and di-n-propyl; straight or branched unsymmetrical disubstituted (C 3 -C 14 )alkylamino group wherein the total number of carbons in the substitution is not more than 14; unsymmetrical disubstituted (C 4 -C 14 )cycloalkylamino group wherein the total number of carbons in the substitution is not more than 14; (C 2 -C 8 )azacycloalkyl and substituted (C 2 -C 8 )azacycloalkyl group selected from aziridinyl, azetidinyl, pyrrolidinyl, piperidinyl, 4-methylpiperidinyl, 2-methylpyrrolidinyl, cis-3,4-dimethylpyrrolidinyl, and trans-3,4-dimethylpyrrolidinyl and the diastereomers and enantiomers of said (C 2 -C 8 )azacycloalkyl and substituted (C 2 -C 8 )azacycloalkyl group; 1-azaoxacycloalkyl group selected from morpholinyl and 1-aza-5-oxacycloheptane; substituted 1-azaoxacycloalkyl group selected from 2-(C 1 -C 3 )alkylmorpholinyl, 3-(C 1 -C 3 )alkylisooxazolidinyl and tetrahydrooxazinyl; [1,n]-diazacycloalkyl and substituted [1,n]-diazacycloalkyl group selected from piperazinyl, 2-(C 1 -C 3 )alkylpiperazinyl, 4-(C 1 -C 3 )alkylpiperazinyl, 2,4-dimethylpiperazinyl, 4-hydroxypiperazinyl, 2,5-diazabicyclo[2.2.1]hept-2-yl, 2,5-diaza-5-methylbicyclo[2.2.1]hept-2-yl, and 2,3-diaza-3-methylbicyclo[2.2.2]oct-2-yl, the diastereomers or enantiomers of said [1,n]-diazacycloalkyl and substituted [1,n]-diazacycloalkyl group; 1-azathiacycloalkyl and substituted 1-azathiacycloalkyl group selected from thiomorpholinyl and 2-(C 1 -C 3 )alkylthiomorpholinyl; N-azolyl and substituted N-azolyl group selected from 1-imidazolyl, 2-(C 1 -C 3 )alkyl-1-imidazolyl, 3-(C 1 -C 3 )alkyl-1-imidazolyl, 1-pyrrolyl, 2-(C 1 -C 3 )alkyl-1-pyrrolyl, 3-(C 1 -C 3 )alkyl-1-pyrrolyl, 1-pyrazolyl, 3-(C 1 -C 3 )alkyl-1-pyrazolyl, indolyl, 1-(1,2,3-triazolyl), 4-(C 1 -C 3 )alkyl-1-(1,2,3-triazolyl), 5-(C 1 -C 3 )alkyl-1-(1,2,3-triazolyl) and 4-(1,2,4-triazolyl; (heterocycle)methylamino group selected from 2- or 3-furylmethylamino, 2- or 3-thienylmethylamino, 2-, 3- or 4-pyridylmethylamino, 2- or 5-pyridazinylmethylamino, 2-pyrazinylmethylamino, 2-(imidazolyl)methylamino, (benzimidazolyl)methylamino, and (benzothiazolyl)methylamino and substituted (heterocycle)methylamino group (substitution selected from straight or branched (C 1 -C 6 )alkyl); carboxy(C 2 -C 4 )alkylamino group selected from aminoacetic acid, α-aminopropionic acid, β-aminopropionic acid, α-butyric acid, and β-aminobutyric acid and the enantiomers of said carboxy(C 2 -C 4 )alkylamino group; (C 1 -C 4 )alkoxycarbonylamino group selected from methoxycarbonylamino, ethoxycarbonylamino, allyloxycarbonylamino, propoxycarbonylamino, isoproproxycarbonylamino, 1,1-dimethylethoxycarbonylamino, n-butoxycarbonylamino, and 2-methylpropoxycarbonylamino, (C 1 -C 4 )alkoxyamino group substitution selected from methoxy, ethoxy, n-propoxy, 1-methylethoxy, n-butoxy, 2-methylpropoxy, and 1,1-dimethylethoxy; (C 7 -C 11 )arylalkoxyamino group substitution selected from benzyoxy, 2-phenylethoxy, 1-phenylethoxy, 2-(naphthyl)methoxy, 1-(naphthyl)methoxy and phenylpropoxy; or R 1 and W taken together are --CH 2 (CH 2 ) n CH 2 NH--, wherein n=1-3;
and the pharmacologically acceptable organic and inorganic salts or metal complexes.
Compounds of special interest are compounds according to the above formula I and II wherein:
R is selected from α-CH 3 ;
R 1 is selected from hydrogen; straight or branched (C 1 -C 4 )alkyl group selected from methyl, ethyl, propyl and butyl; straight or branched (C 1 -C 4 )alkyl group optionally substituted with amino; (heterocyclo)methyl group said heterocycle selected from imidazolyl and 3-indolyl; (C 5 -C 6 )cycloalkylmethyl group selected from (cyclopentyl)methyl and (cyclohexyl) methyl; (C 2 -C 4 )carboxamidoalkyl group selected from carboxamidomethyl and carboxamidoethyl;
R 2 is selected from hydrogen and (C 1 -C 2 )alkyl selected from methyl and ethyl;
W is selected from amino; (C 1 -C 8 ) straight or branched alkyl monosubstituted amino group substitution selected from methyl, ethyl, n-propyl, 1-methylethyl, n-butyl, 1-methylpropyl, 2-methylpropyl, n-hexyl and n-octyl; (C 3 -C 6 )cycloalkyl monosubstituted amino group substitution selected from cyclopropyl, cyclopentyl and cyclohexyl; [(C 4 -C 5 )cycloalkyl] (C 1 -C 2 )alkyl monosubstituted amino group substitution selected from (cyclopropyl)methyl and (cyclopropyl)ethyl; (C 3 -C 4 )alkenyl monosubstituted amino group substitution selected from allyl and 3-butenyl; (C 7 -C 10 )aralkylamino group selected from benzyl, 2-phenylethyl and 1-phenylethyl; straight or branched symmetrical disubstituted (C 2 -C 4 )alkylamino group substitution selected from dimethyl and diethyl; straight or branched unsymmetrical disubstituted (C 3 )alkylamino group substitution selected from methyl(ethyl); (C 2 -C 5 )azacycloalkyl group selected from pyrrolidinyl and piperidinyl; 1-azaoxacycloalkyl group selected from morpholinyl; substituted-1-azaoxacycloalkyl group selected from 2-(C 1 -C 3 )alkylmorpholinyl; [1,n]-diazacycloalkyl and substituted [1,n]-diazacycloalkyl group selected from piperazinyl, 2-(C 1 -C 3 )alkylpiperazinyl, 4-(C 1 -C 3 )alkylpiperazinyl, and 2,5-diaza-5-methylbicyclo[2.2.1]hept-2-yl and the diastereomers and enantiomers of said [1,n]-diazacycloalkyl and substituted [1,n]-diazacycloalkyl group; 1-azathiacycloalkyl and substituted 1-azathiacycloalkyl group selected from thiomorpholinyl and 2-(C 1 -C 3 )alkylthiomorpholinyl; N-azolyl group selected from 1-imidazolyl; (heterocycle)methylamino group selected from 2- or 3-thienylmethylamino and 2-, 3- or 4-pyridylmethylamino; (C 1 -C 4 )alkoxycarbonylamino group substitution selected from methoxycarbonylamino, ethoxycarbonylamino, and 1,1-dimethylethoxycarbonylamino; or R 1 and W taken together are --CH 2 CH 2 CH 2 NH--;
and the pharmacologically acceptable organic and inorganic salts or metal complexes.
Also included in the present invention are compounds useful as intermediates for producing the above compounds of formula I. Such intermediate include those having the formula II: ##STR3## wherein: Y is selected from (CH 2 ) n X, n=0-5, X is halogen selected from bromine, chlorine, fluorine and iodine; alternatively, X is a protected amino selected from trifluoroacetylamino, (C 1 -C 4 )alkoxycarbonylamino selected from t-butoxycarbonylamino, methoxycarbonylamino, ethoxycarbonylamino, allyloxycarbonylamino and 1,1,1-trichloroethoxycarbonylamino, (C 7 -C 14 )arylalkoxycarbonylamino selected from benzyloxycarbonylamino, naphthylmethoxycarbonylamino, 9-fluorenylmethoxycarbonylamino, p-methoxybenzyloxycarbonylamino, and p-nitrobenzyloxycarbonylamino, (C 7 -C 23 ) arylalkylamino selected from benzylamine, p-methoxybenzylamine, p-nitrobenzylamine, tritylamine and 4-methoxytritylamine;
R is selected from methylene, α-CH 3 and β-CH 3 ;
R 1 is selected from hydrogen; straight or branched (C 1 -C 8 )alkyl group selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, hexyl, heptyl and octyl; straight or branched (C 1 -C 8 )alkyl group optionally substituted with α-mercapto, α-hydroxy, carboxyl, carboxamido, amino, guanidino or amidino; (C 6 -C 10 )aryl group selected from phenyl, α-naphthyl and β-naphthyl; substituted (C 6 -C 10 )aryl group substitution selected from hydroxy, halogen, (C 1 -C 4 )alkoxy, trihalo(C 1 -C 3 )alkyl, nitro, amino, cyano, (C 1 -C 4 )alkoxycarbonyl, (C 1 -C 3 )alkylamino and carboxy; (C 7 -C 9 )aralkyl group selected from benzyl, 1-phenylethyl, 2-phenylethyl and phenylpropyl; substituted (C 7 -C 9 )aralkyl group substitution selected from halo, (C 1 -C 4 )alkyl, nitro, hydroxy, amino, mono- or di-substituted (C 1 -C 4 )alkylamino, (C 1 -C 4 )alkoxy, (C 1 -C 4 )alkylsulfonyl, cyano and carboxy; (heterocycle)methyl group said heterocycle selected from 4-(or 3-)imidazolyl, 4-(or 3-)oxazolyl, 3-(or 2-)indolyl, 2-(or 3-)furanyl, 2-(or 3-)thienyl, 2-(or 3-) pyrrolyl, 2-(or 3-) pyrazolyl, 4-(1,2,3-triazolyl) and benzimidazolyl; (C 3 -C 6 )cycloalkylmethyl group selected from (cyclopropyl)methyl, (cyclobutyl)methyl, (cyclopentyl)methyl and (cyclohexyl)methyl;
R 2 is selected from hydrogen and (C 1 -C 6 )alkyl selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl and hexyl. It will be appreciated that when R 1 does not equal R 2 the stereochemistry of the asymmetric carbon (i.e. the carbon bearing the W substituent) maybe be either the racemate (DL) or the individual enantiomers (n or D); and the pharmacologically acceptable organic and inorganic salts and metal complexes.
Preferred compounds are compounds according to the above formula II wherein:
Y is selected from (CH 2 ) n X, n=0-5, X is halogen selected from bromine, chlorine, fluorine and iodine; alternatively, X is a protected amino selected from trifluoroacetylamino, (C 1 -C 4 )alkoxycarbonylamino selected from t-butoxycarbonylamino, methoxycarbonylamino, ethoxycarbonylamino, allyloxycarbonylamino and 1,1,1-trichloroethoxycarbonylamino, (C 7 -C 14 )arylalkoxycarbonylamino selected from benzyloxycarbonylamino, naphthylmethoxycarbonylamino, 9-fluorenylmethoxycarbonylamino, p-methoxybenzyloxycarbonylamino, and p-nitrobenzyloxycarbonylamino, (C 7 -C 23 ) arylalkylamino selected from benzylamine, p-methoxybenzylamine, p-nitrobenzylamine, tritylamine and 4-methoxytritylamine;
R is selected from methylene, α-CH 3 and β-CH 3 ;
R 1 is selected from hydrogen; straight or branched (C 1 -C 8 )alkyl group selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, hexyl, heptyl and octyl; straight or branched (C 1 -C 8 )alkyl group optionally substituted with α-mercapto, α-hydroxy, carboxyl, carboxamido; (C 6 -C 10 )aryl group selected from phenyl, α-naphthyl and β-naphthyl; (C 7 -C 9 )aralkyl group selected from benzyl, 1-phenylethyl, 2-phenylethyl and phenylpropyl; substituted(C 7 -C 9 )aralkyl group substitution selected from halo, (C 1 -C 4 )alkyl, nitro, hydroxy, amino, mono- or di-substituted (C 1 -C 4 )alkylamino, (C 1 -C 4 )alkoxy, (C 1 -C 4 )alkylsulfonyl, cyano and carboxy;
R 2 is selected from hydrogen and (C 1 -C 6 )alkyl selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl and hexyl; and the pharmacologically acceptable organic and inorganic salts and metal complexes.
Particularly preferred compounds are compounds according to the above formula II wherein:
Y is selected from (CH 2 ) n X, n=0-5, X is halogen selected from bromine, chlorine, fluorine and iodine; alternatively, X is a protected amino selected from trifluoroacetylamino, (C 3 -C 4 ) alkoxycarbonylamino selected from t-butoxycarbonylamino, allyloxycarbonylamino and 1,1,1-trichloroethoxycarbonylamino, (C 7 -C 14 )arylalkoxycarbonylamino selected from benzyloxycarbonylamino, and 9-fluorenylmethoxycarbonylamino], (C 7 -C 23 )arylalkylamino selected from benzylamine, and tritylamine;
R is selected from methylene, α-CH 3 and β-CH 3 ;
R 1 is selected from hydrogen; straight or branched (C 1 -C 8 )alkyl group selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, hexyl, heptyl and octyl; straight or branched (C 1 -C 8 )alkyl group optionally substituted with α-mercapto, α-hydroxy, carboxyl, carboxamido; (C 6 -C 10 )aryl group selected from phenyl, α-naphthyl and β-naphthyl; (C 7 -C 9 )aralkyl group selected from benzyl, 1-phenylethyl, 2-phenylethyl and phenylpropyl;
R 2 is selected from hydrogen and (C 1 -C 6 )alkyl selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl and hexyl; and the pharmacologically acceptable organic and inorganic salts and metal complexes.
Compounds of special interest are compounds according to the above formula II wherein:
Y is selected from (CH 2 ) n X, n=0-5, X is halogen selected from bromine, chlorine, fluorine and iodine; alternatively, X is a protected amino selected from triluoroacetylamino, (C 3 -C 4 )alkoxycarbonylamino selected from t-butoxycarbonylamino and allyloxycarbonylamino], (C 7 -C 14 )arylalkoxycarbonylamino selected from benzyloxycarbonylamino, and 9-fluorenylmethoxycarbonylamino], (C 7 -C 23 )arylalkylamino [selected from benzylamine and tritylamine];
R is selected from α-CH 3 ;
R 1 is selected from hydrogen; straight or branched (C 1 -C 4 )alkyl group selected from methyl, ethyl, propyl and butyl; straight or branched (C 1 -C 4 )alkyl group optionally substituted with amino; (heterocyclo)methyl group said heterocycle selected from imidazolyl and 3-indolyl; (C 5 -C 6 )cycloalkylmethyl group selected from (cyclopentyl)methyl and (cyclohexyl)methyl; (C 2 -C 4 )carboxamidoalkyl group selected from carboxamidomethyl and carboxamidoethyl;
R 2 is selected from hydrogen and (C 1 -C 2 )alkyl selected from methyl and ethyl; and the pharmacologically acceptable organic and inorganic salts and metal complexes.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The novel compounds of the present invention may be readily prepared in accordance with the following schemes. ##STR4##
The 9-[(substituted glycyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracyclines, or mineral acid salts, can be made by the procedure described in scheme I. In accordance with scheme I, 9-amino-6-(substituted)-5-hydroxy-6-deoxytetracycline or its mineral acid salt, 1, is dissolved in a mixture of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)pyrimidone and acetonitrile or equivalent solvents. Sodium carbonate is added and the mixture is stirred for 5 minutes. An acid chloride, acid anhydride or suitably activated acylation reagent of the formula: ##STR5## wherein X=suitable leaving group and R 1 , R 2 , and W have been described hereinabove, is added and the reaction is stirred at room temperature for from 0.5-2 hours to give the corresponding 9-[(substituted glycyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracycline, or its mineral acid salt 3. ##STR6##
The second method for producing 9-[(substituted glycyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracyclines or its mineral acid salt 3, is shown in scheme II. This method uses common intermediates which are easily prepared by reacting commercially available haloacyl halides, anhydrides or suitably activated haloacylating agents of the formula: ##STR7## wherein Y, R 1 and R 2 are as defined hereinabove and Q is halogen selected from bromine, chlorine, iodine, fluorine or suitable leaving group; with 9-amino-6-(substituted)-5-hydroxy-6-deoxytetracyclines, or its mineral acid salt 1, to give straight or branched 9-[(haloacyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracyclines or its mineral acid salt, 2, in almost quantitative yield. The above intermediates, straight or branched 9-[(haloacyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracyclines or its mineral acid salt 2, react with a wide variety of nucleophiles, especially amines, having the formula WH, wherein W is as defined hereinabove to give the new 9-[(substituted glycyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracyclines or mineral acid salt 3 of the present invention.
In accordance with Scheme II, 9-amino-6-(substituted)-5-hydroxy-6-deoxytetracycline or its mineral acid salt, 1, is mixed with
a) a polar-aprotic or protic (low temp.) solvent such as 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidone, herein after called DMPU, hexamethylphosphoramide herein after called HMPA, dimethylformamide, dimethylacetamide, N-methylpyrrolidone, 1,2-dimethoxyethane, water or equivalent thereof;
b) an inert solvent such as acetonitrile, methylene chloride, tetrahydrofuran chloroform, carbon tetrachloride, 1,2-dichloroethane, tetrachloroethane, diethyl ether, t-butyl methyl ether, isopropyl ether or equivalent thereof;
c) a base such as sodium carbonate, sodium bicarbonate, sodium acetate, potassium carbonate, potassium bicarbonate, triethylamine, cesium carbonate, lithium carbonate or bicarbonate equivalents; and
d) a straight or branched haloacyl halide, anhydride or suitably activated haloacylating agent of the formula: ##STR8## wherein Y, R 1 , R 2 and Q are as defined hereinabove such as bromoacetyl bromide, (bromoacetic anhydride, chloroacetyl chloride (chloroacetic anhydride) or 2-bromopropionyl bromide or equivalent thereof; the halo, Y, and halide, Q, in the haloacyl halide can be the same or different halogen and is selected from bromine, chlorine, iodine and fluorine; Y is (CH 2 ) n X, n=0-5, X is halogen;
e) for 0.5 to 5 hours at room temperature to the reflux temperature of the reaction; to form the corresponding 9-[(haloacyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracycline, 2, or its mineral acid salt.
The intermediate, 9-[(haloacyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracycline or mineral acid salt 2, is treated, under an inert atmosphere of helium, argon or nitrogen, with
a) a nucleophile WH such as an amine or substituted amine or equivalent for example methylamine, dimethylamine, ethylamine, n-butylamine, propylamine or n-hexylamine;
b) a polar-aprotic or protic solvent such as DMPU, HMPA, dimethylformamide, dimethylacetamide, N-methylpyrrolidone, 1,2-dimethoxyethane, water or equivalent;
c) for from 0.5-2 hours at room temperature or under reflux temperature to produce the desired 9-[(substituted glycyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracycline, 3, or its mineral acid salt.
Alternatively, the intermediate, 9-[(protected aminoacyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracycline (Y=protected amino group), is treated under an inert atmosphere of helium, argon or nitrogen with an appropriate nitrogen deprotection reagent using methods known to those skilled in the art [(a) Richard C. Larock, Comprehensive Organic Transformations, VCH Publishers, 1989; (b) Theodora Greene, Protecting Groups in Organic Synthesis, Academic Press, 1991]. It is well known to one skilled in the art that the appropriate nitrogen protection and deprotection scheme is chosen based on chemical and physical stability. ##STR9##
In accordance with Scheme III, compounds of formula 3 are N-alkylated in the presence of formaldehyde and either a primary amine such as methylamine, ethylamine, benzylamine, methyl glycinate, (L or D)alanine, (L or D)lysine or their substituted congeners; or a secondary amine such as morpholine, pyrrolidine, piperidine or their substituted congeners to give the corresponding Mannich base adduct, 4.
The 9-[(substituted glycyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracyclines may be obtained as metal complexes such as aluminum, calcium, iron, magnesium, manganese and complex salts; inorganic and organic salts and corresponding Mannich base adducts using methods known to those skilled in the art (Richard C. Larock, Comprehensive Organic Transformations, VCH Publishers, 411-415, 1989). It is well known to one skilled in the art that an appropriate salt form is chosen based on physical and chemical stability, flowability, hygroscopicity and solubility. Preferably, the 9-[(substituted glycyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracyclines are obtained as inorganic salt such as hydrochloric, hydrobromic, hydroiodic, phosphoric, nitric or sulfate; or organic salt such as acetate, benzoate, citrate, cysteine or other amino acids, fumarate, glycolate, maleate, succinate, tartrate, alkylsulfonate or arylsulfonate. Depending on the stoichiometry of the acids used, the salt formation occurs with the C(4)-dimethylamino group (1 equivalent of acid) or with both the C(4)-dimethylamino group and the W group (2 equivalents of acid). The salts are preferred for oral and parenteral administration.
Some of the compounds of the hereinbefore described Schemes have centers of asymmetry at the carbon bearing the W substituent. The compounds may, therefore, exist in at least two (2) stereoisomeric forms. The present invention encompasses the racemic mixture of stereo isomers as well as all stereoisomers of the compounds whether free from other stereoisomers or admixed with stereoisomers in any proportion of enantiomers. The absolute configuration of any compound may be determined by conventional X-ray crystallography.
The stereochemistry centers on the tetracycline unit (i.e. C-4, C-4a, C-5, C-5a, C-6 and C-12a) remain intact throughout the reaction sequences.
BIOLOGICAL ACTIVITY
Method for in Vitro Antibacterial Evaluation
(Table 1)
The minimum inhibitory concentration (MIC), the lowest concentration of the antibiotic which inhibits growth to the test organism, is determined by the agar dilution method using Muller-Hinton II agar (Baltimore Biological Laboratories). An inoculum density of 1-5×10 5 CFU/ml and a range of antibiotic concentrations (32-0.004 μg/ml) is used. The plates are incubated for 18 hours at 35° C. in a forced air incubator. The test organisms comprise strains that are sensitive to tetracycline and genetically defined strains that are resistant to tetracycline, due to inability to bind to bacterial ribosomes (tetM) or by a tetK encoded membrane protein which confers tetracycline resistance by energy-dependent efflux of the antibiotic from the cell.
Testing Results
The claimed compounds exhibited good in vitro activity against a spectrum of doxycycline-sensitive and doxycycline-resistant Gram-positive and Gram-negative bacteria (Table 1). Notably, compounds A-D, compared to deoxycycline, exhibited excellent in vitro activity against strains containing the two major resistance determinants: efflux, as represented by tetB and tetD (E. coli UBMS 88-1, E. coli MC4100 and E. coli J3272) and ribosomal protection, as represented by S. aureus UBMS 90-1 and UBMS 90-2 and E. coli UMBS 89-1 and 90-4. These compounds showed improved activity against Enterococcus and comparable activity to doxycycline against sensitive strains. Compounds E-F exhibited similar activity against deoxycycline-resistant, both efflux and ribosomal protection mechanisms, and deoxycycline-susceptible strains. Compounds G-H showed similar activity against doxycycline susceptible S. aureus strains and doxycycline-resistant (both efflux and ribosomal resistant) strains. Compounds I-J had similar activity against doxycycline-sensitive strains and strains resistant to doxycycline due to ribosomal protection, but were less effective against strains carrying the efflux (tetK) resistance mechanism.
As can be seen from Table 1, compounds of the invention can be used to prevent or control important mammalian and veterinary diseases such as diarrhea, urinary tract infections, infections of skin and skin structure, ear, nose and throat infections, wound infections, mastitis and the like.
Thus, the improved efficacy of 9-[(N,N-dimethylglycyl)amido]-6-(substituted)-5-hydroxy-6-deoxytetracycline is demonstrated by the in vitro activity against isogenic strains into which the resistance determinants, such as tetM, are cloned (Table 1).
______________________________________LEGEND FOR COMPOUNDSCompound Name______________________________________Doxycycline [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12, 12a-pentahydroxy-6-methyl-1,11-dioxo-2- naphthacenecarboxamideA [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[[(dimethylamino)acetyl]amino]-1,4,4a, 5,5a,6,11,12a-octahydro-3,5,10,12,12a- pentahydroxy-6-methyl-1,11-dioxo-2- naphthacenecarboxamideB [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(L-leucyl)amino]-1,4,4a,5,5a,6,11,12a- octahydro-3,5,10,12,12a-pentahydroxy-6- methyl-1,11-dioxo-2-naphthacenecarboxamideC [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(L-phenylalanyl)amino]-1,4,4a,5,5a,6, 11,12a-octahydro-3,5,10,12,12a-penta- hydroxy-6-methyl-1,11-dioxo-2-naphtha- cenecarboxamideD [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(D-phenylalanyl)amino]-1,4,4a,5,5a,6, 11,12a-octahydro-3,5,10,12,12a-penta- hydroxy-6-methyl-1,11-dioxo-2-naphtha- cenecarboxamideE [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[[L-β-(cyclohexyl)alanyl]amino]-l,4,4a, 5,5a,6,11,12a-octahydro-3,5,10,12,12a- pentahydroxy-6-methyl-1,11-dioxo-2- naphthacenecarboxamideF [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(L-prolyl)amino]-1,4,4a,5,5a,6,11, 12a-octahydro-3,5,10,12,12a-pentahydroxy- 6-methyl-1,11-dioxo-2-naphthacenecar- boxamideG [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(L-N,N-dimethylphenylalanyl)amino]- 1,4,4a,5,5a,6,11,12a-octahydro-3,5,10, 12,12a-pentahydroxy-6-methyl-1,11-dioxo- 2-naphthacenecarboxamideH [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(L-N-methylleucyl)amino]-1,4,4a,5,5a,6, 11,12a-octahydro-3,5,10,12,12a-penta- hydroxy-6-methyl-1,11-dioxo-2-naphthacene- carboxamideI [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(L-tryptophanyl)amino]-1,4,4a,5,5a,6, 11,12a-octahydro-3,5,10,12,12a-penta- hydroxy-6-methyl-1,11-dioxo-2-naphthacene- carboxamideJ [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[L-tyrosyl)amino]-1,4,4a,5,5a,6, 11,12a-octahydro-3,5,10,12,12a-penta- hydroxy-6-methyl-1,11-dioxo-2-naphthacene- carboxamideK [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(L-glutaminyl)amino]-1,4,4a,5,5a,6, 11,12,a-octahydro-3,5,10,12,12a-penta- hydroxy-6-methyl-1,11-dioxo-2-naphthacene- carboxamideL [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(L-glycyl)amino]-1,4,4a,5,5a,6,11,12a- octahydro-3,5,10,12,12a-pentahydroxy-6- methyl-1,11-dioxo-2-naphthacenecarboxamideM [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(bromoacetyl)amino]-1,4,4a,5,5a,6,11, 12a-octahydro-3,5,10,12,12a-pentahydroxy- 6-methyl-1,11-dioxo-2-naphthacenecarbox- amideN [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 9-[(L-lysyl)amino]-1,4,4a,5,5a,6,11,12a- octahydro-3,5,10,12,12a-pentahydroxy-6- methyl-1,11-dioxo-2-naphthacenecarbox- amide______________________________________
TABLE 1__________________________________________________________________________Antimicrobial Activity of 9-(α-Aminoacyl)-6-(substituted)-5-hydroxy-6-deoxytetracyclinesORGANISM Doxycycline A B C D E F G__________________________________________________________________________E. coli UBMS 88-1 (tetB) 32.00 1.00 2.00 4.00 4.00 8.00 4.00 32.00E. coli MC4100 (tet-sensitive) 0.25 0.25 0.50 0.50 1.00 2.00 1.00 8.00E. coli PRP1 (tetA) 8.00 4.00 16.00 16.00 8.00 8.00 16.00 16.00E. coli MC4100 (TN10WT) >32.00 1.00 2.00 4.00 4.00 4.00 4.00 >32.00E. coli J3272 (tetC) 8.00 8.00 4.00 8.00 4.00 8.00 8.00 32.00E. coli UBMS 89-1 (tetM) 16.00 0.50 1.00 2.00 4.00 2.00 2.00 8.00E. coli UBMS 89-2 (tet-sensitive) 2.00 0.50 1.00 4.00 4.00 8.00 2.00 32.00E. coli J2175 (par J2445) 2.00 0.50 2.00 4.00 4.00 4.00 2.00 32.00E. coli J2445 (IMP mut) 0.25 0.12 0.50 0.50 0.50 1.00 1.00 2.00E. coli UBMS 90-4 (tetM) 32.00 0.25 1.00 2.00 2.00 4.00 2.00 16.00E. coli UBMS 90-5 K-12 1.00 0.50 1.00 4.00 4.00 4.00 2.00 32.00E. coli #311 MP (Mino-sensitive) 1.00 0.50 1.00 2.00 4.00 4.00 2.00 16.00E. coli ATCC 25922 1.00 0.50 1.00 2.00 4.00 4.00 2.00 16.00E. coli J3272 (tetD) 32.00 0.25 1.00 1.00 1.00 2.00 1.00 16.00Serr. marc. FPOR 87-33 16.00 8.00 32.00 >32.00 >32.00 >32.00 16.00 >32.00X. maltophilia NEMC 87-2 1.00 4.00 16.00 32.00 >32.00 >32.00 32.00 32.00Ps. aeruginosa ATCC 2785 32.00 16.00 32.00 >32.00 >32.00 >32.00 >32.00 >32.00S aureus NEMC 89-4 (MRSA) 0.12 0.25 1.00 0.50 2.00 2.00 2.00 2.00S. aureus UBMS 88-4 (par 88-5, tetM) 0.06 0.25 1.00 0.50 1.00 2.00 2.00 1.00S. aureus UBMS 88-5 (tetM) 8.00 0.50 1.00 1.00 4.00 4.00 4.00 2.00S. aureus UBMS 88-7 (tetK) 4.00 4.00 2.00 4.00 16.00 2.00 4.00 2.00S. aureus UBMS 90-1 (tetM) 8.00 0.50 1.00 2.00 8.00 8.00 4.00 2.00S. aureus UBMS 90-3 0.06 0.12 0.50 0.50 1.00 0.50 1.00 1.00S. aureus UBMS 90-2 (tetM) 8.00 0.50 0.50 0.50 2.00 2.00 2.00 2.00S. aureus IVES 2943 (tet-resist) 16.00 8.00 4.00 16.00 32.00 4.00 32.00 2.00S. aureus ROSE MP (tet-resist) 8.00 8.00 8.00 32.00 >32.00 8.00 >32.00 8.00S. aureus SMITH MP (mino-sens) 0.12 0.25 0.50 0.50 0.50 1.00 2.00 4.00S. aureus IVES 1983 MP 16.00 8.00 2.00 8.00 32.00 8.00 32.00 2.00S. aureus ATCC 29213 0.06 0.25 1.00 1.00 1.00 2.00 2.00 2.00S. hemolyticus AVAH 88-3 0.25 0.50 2.00 8.00 8.00 8.00 4.00 4.00Enterococcus 12201 (vanc-resist.) 8.00 0.50 0.50 1.00 4.00 2.00 4.00 1.00E. faecalis ATCC 29212 4.00 0.25 0.25 0.50 0.50 0.50 2.00 1.00__________________________________________________________________________ORGANISM Doxycycline H I J K L M N__________________________________________________________________________E. coli UBMS 88-1 (tetB) 32.00 8.00 8.00 16.00 >32.00 16.00 >32.00 >32.00E. coli MC4100 (tet-sensitive) 0.25 1.00 2.00 2.00 4.00 4.00 >32.00 >32.00E. coli PRP1 (tetA) 8.00 16.00 16.00 32.00 >32.00 >32.00 >32.00 >32.00E. coli MC4100 (TN10WT) >32.00 4.00 8.00 16.00 >32.00 32.00 >32.00 >32.00E. coli J3272 (tetC) 8.00 8.00 8.00 16.00 >32.00 >32.00 >32.00 >32.00E. coli UBMS 89-1 (tetM) 16.00 4.00 8.00 16.00 >32.00 8.00 >32.00 >32.00E. coil UBMS 89-2 (tet-sensitive) 2.00 8.00 8.00 16.00 16.00 8.00 >32.00 >32.00E. coli J2175 (par J2445) 2.00 4.00 8.00 16.00 16.00 8.00 >32.00 >32.00E. coli J2445 (IMP mut) 0.25 1.00 1.00 1.00 4.00 4.00 >32.00 >32.00E. coli UBMS 90-4 (tetM) 32.00 4.00 4.00 8.00 >32.00 8.00 >32.00 >32.00E. coli UBMS 90-5 K-12 1.00 4.00 8.00 8.00 16.00 8.00 >32.00 >32.00E. coli #311 MP (Mino-sensitive) 1.00 4.00 8.00 16.00 16.00 8.00 >32.00 >32.00E. coli ATCC 25922 1.00 4.00 8.00 16.00 16.00 8.00 >32.00 >32.00E. coli J3272 (tetD) 32.00 2.00 4.00 8.00 >32.00 8.00 >32.00 >32.00Sar. marc. FPOR 87-33 16.00 >32.00 >32.00 >32.00 >32.00 32.00 >32.00 >32.00X. maltophilia NEMC 87-2 1.00 >32.00 >32.00 >32.00 16.00 >32.00 >32.00 >32.00Ps. aeruginosa ATCC 2785 32.00 >32.00 >32.00 >32.00 >32.00 >32.00 >32.00 >32.00S. aureus NEMC 89-4 (MRSA) 0.12 2.00 4.00 2.00 2.00 8.00 16.00 >32.00S. aureus UBMS 88-4 (par 88-5, tetM) 0.06 2.00 4.00 2.00 2.00 8.00 16.00 >32.00S. aureus UBMS 88-5 (tetM) 8.00 2.00 4.00 2.00 >32.00 16.00 >32.00 >32.00S. aureus UBMS 88-7 (tetK) 4.00 2.00 16.00 32.00 32.00 >32.00 16.00 16.00S. aureus UBMS 90-1 (tetM) 8.00 2.00 4.00 4.00 >32.00 16.00 >32.00 >32.00S. aureus UBMS 90-3 0.06 1.00 2.00 0.50 1.00 4.00 8.00 >32.00S. aureus UBMS 90-2 (tetM) 8.00 1.00 4.00 1.00 >32.00 8.00 >32.00 >32.00S. aureus IVES 2943 (tet-resist) 16.00 2.00 32.00 >32.00 >32.00 >32.00 >32.00 >32.00S. aureus ROSE MP (tet-resist) 8.00 16.00 32.00 >32.00 >32.00 >32.00 >32.00 >32.00S. aureus SMITH MP (mino-sens) 0.12 2.00 1.00 1.00 4.00 8.00 8.00 >32.00S. aureus IVES 1983 MP 16.00 4.00 16.00 >32.00 >32.00 >32.00 >32.00 >32.00S. aureus ATCC 29213 0.06 4.00 4.00 2.00 2.00 8.00 16.00 >32.00S. hemolyticus AVAH 88-3 0.25 16.00 16.00 16.00 4.00 16.00 >32.00 >32.00Enterococcus 12201 (vanc-resist.) 8.00 2.00 2.00 1.00 >32.00 16.00 >32.00 >32.00E. faecalis ATCC 29212 4.00 1.00 1.00 0,50 >32.00 4.00 >32.00 >32.00__________________________________________________________________________
When the compounds are employed an antibacterials, they can be combined with one or more pharmaceutically acceptable carriers, for example, solvents, diluents and the like, and may be administered orally in such forms as tablets, capsules, dispersible powders, granules, or suspensions containing, for example, from about 0.05 to 5% of suspending agent, syrups containing, for example, from about 10 to 50% of sugar, and elixirs containing for example, from about 20 to 50% ethanol and the like, or parenterally in the form of sterile injectable solutions or suspensions containing from about 0.05 to 5% suspending agent in an isotonic medium. Such pharmaceutical preparations may contain, for example, from about 25 to about 90% of the active ingredient in combination with the carrier, more usually between about 5% and 60% by weight.
An effective amount of compound from 2.0 mg/kg of body weight to 100.0 mg/kg of body weight should be administered one to five times per day via any typical route of administration including but not limited to oral, parenteral (including subcutaneous, intravenous, intramuscular, intrasternal injection or infusion techniques), topical or rectal, in dosage unit formulations containing conventional non-toxic pharmaceutically acceptable carriers, adjuvants and vehicles. It will be understood, however, that the specific dose level and frequency of dosage for any particular patient may be varied and will depend upon a variety of factors including the activity of the specific compound employed, the metabolic stability and length of action of that compound, the age, body weight, general health, sex, diet, mode and time of administration, rate of excretion, drug combination, the severity of the particular condition, and the host undergoing therapy.
These active compounds may be administered orally as well as by intravenous, intramuscular, or subcutaneous routes. Solid carriers include starch, lactose, dicalcium phosphate, microcrystalline cellulose, sucrose and kaolin, while liquid carriers include sterile water, polyethylene glycols, non-ionic surfactants and edible oils such as corn, peanut and sesame oils, as are appropriate to the nature of the active ingredient and the particular form of administration desired. Adjuvants customarily employed in the preparation of pharmaceutical compositions may be advantageously included, such as flavoring agents, coloring agents, preserving agents, and antioxidants, for example, vitamin E, ascorbic acid, BHT and BHA.
The preferred pharmaceutical compositions from the standpoint of ease of preparation and administration are solid compositions, particularly tablets and hard-filled or liquid-filled capsules. Oral administration of the compounds is preferred.
These active compounds may also be administered parenterally or intraperitoneally. Solutions or suspensions of these active compounds as a free base or pharmacologically acceptable salt can be prepared in glycerol, liquid, polyethylene glycols and mixtures thereof in oils. Under ordinary conditions of storage and use, these preparations contain a preservative to prevent the growth of microorganisms.
The pharmaceutical forms suitable for injectable use include sterile aqueous solutions or dispersions and sterile powders for the extemporaneous preparation of sterile injectable solutions or dispersions. In all cases, the form must be sterile and must be fluid to the extent that easy syringability exists. It must be stable under the conditions of manufacture and storage and must be preserve against the contaminating action of micoorganisms such as bacterial and fungi. The carrier can be a solvent or dispersion medium containing, for example, water, ethanol, polyol (e.g., glycerol, propylene glycol and liquid polyethylene glycol), suitable mixtures thereof, and vegetable oil.
The invention will be more fully described in conjunction with the following specific examples which are not be construed as limiting the scope of the invention.
EXAMPLE 1
[4S-(4alpha,12aalpha)]-9-[(Bromoacetyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
A stirred mixture of 0.030 g of 9-amino-5-hydroxy-6-deoxytetracycline, 0.10 g of sodium bicarbonate and 1 ml of N-methylpyrrolidinone at ambient temperature, is treated with 0.010 ml of bromoacetyl bromide. After 20 minutes, the suspension is filtered into stirred diethyl ether and the crude product is filtered. The crude product is purified by preparative HPLC to give 0.015 g of the desired product as a yellow glass.
MS(FAB): m/z 579 (M+H) and 581 (M+H).
1 H NMR (CD 3 OH): δ 8.20(d,1H,J=8.3 Hz,H-8); 6.90(d,1H, J=8.3 Hz,H-7); 4.37(bs,1H,H-4); 4.08(s,2H,CH 2 Br); 3.52(dd,1H,J=8.25;11.40 Hz,H-5); 2.92(bs,6H,NMe 2 ); 2.70-2.90(m,2H,H-4a and H-6); 2.51(dd,J=8.25;12.36 Hz, H-5a) and 1.50(d,3H,J=6.7 Hz,C-CH 3 ).
EXAMPLE 2
[4S-(4alpha,12aalpha)]-9-[(Bromoacetyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide monohydrobromide
To a room temperature solution of 1.75 g of 9-amino-5-hydroxy-6-deoxytetracycline monosulfate, 20 ml of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidone, hereinafter called DMPU, and 4 ml of acetonitrile is added 0.60 g of sodium carbonate. The mixture is stirred for 5 minutes followed by addition of 1.100 g of bromoacetyl bromide. The reaction is stirred one hour, filtered, and the filtrate added dropwise to a mixture of 50 ml of isopropanol and 500 ml of diethyl ether. The resulting yellow solid is collected, washed first with the mixed solvent (isopropanol and diethyl ether), followed by diethyl ether and dried to give 1.40 g of product.
MS(FAB): m/z 579 (M+H) and 581 (M+H).
EXAMPLE 3
[4S-(4alpha,12aalpha)]-9-[(Chloroacetyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide monohydrochloride
To a room temperature solution of 0.05 g of 9-amino-5-hydroxy-6-deoxytetracycline hydrochloride, 1.5 ml of DMPU and 0.5 ml of acetonitrile is added 0.023 g of chloroacetyl chloride. The mixture is stirred for 30 minutes, then poured into a mixture of 0.5 ml of methyl alcohol, 2 ml of isopropyl alcohol and 20 ml of diethyl ether. The resulting solid is collected, washed with diethyl ether and dried to give 0.040 g of the desired product.
MS (FAB): m/z 535 (M+H) and 537 (M+H).
EXAMPLE 4
[4S-(4alpha,12aalpha)]-9-[(2-Bromo-1-oxopropyl)amino](dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide monohydrobromide
The title compound is prepared by the procedure of Example 2, using 2.0 g of 9-amino-5-hydroxy-6-deoxytetracycline hydrochloride, 0.7 g of sodium carbonate, 20 ml of DMPU, 8 ml of acetonitrile and 1.73 g of 2-bromopropionyl bromide. The reaction is stirred for 1 hour to give 1.55 g of the desired product. This reaction works equally well without sodium carbonate.
MS(FAB): m/z 593 (M+H) and 595 (M+H).
EXAMPLE 5
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-1-piperidineacetamide
A solution of 0.108 g of product from Example 1, 1 ml of piperidine and 2 ml of N-methylpyrrolidone, under argon, is stirred at room temperature for 30 minutes. The reaction is concentrated in vacuo and the residue diluted with 1 ml of methanol. The solution is added dropwise to 100 ml of diethyl ether and the precipitate collected, washed with diethyl ether and dried to give a yellow product. The yellow solid is purified by preparative HPLC to give 0.045 g of the desired product as a yellow glass.
MS (FAB): m/z 585 (M+H).
1 H NMR (CD 3 OH): δ 8.23(d,1H,J=8.3 Hz,H-8); 6.95(d,1H, J=8.3 Hz,H-7); 4.37(bs,1H,H-4); 4.13(s,2H,COCH 2 N); 3.52(dd,1H,J=8.25;11.40 Hz,H-5); 2.92(bs,6H,NMe 2 ); 2.70-2.90(m,2H,H-4a and H-6); 2.51(dd,J=8.25;12.36 Hz, H-5a); 2.3-2.55(m,4H); 1.70-1.99(m,6H) and 1.51(d,3H, J=6.7 Hz, C-CH 3 ).
EXAMPLE 6
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-1-piperidineacetamide dihydrochloride
A solution of 0.215 g of product from Example 1, 4 ml of piperidine and 4 ml of N-methylpyrrolidone, under argon, is stirred at room temperature for 30 minutes. The reaction is concentrated in vacuo and the residue diluted with 2 ml of methanol and added dropwise to 150 ml of diethyl ether. 2M hydrochloric acid in diethyl ether is added to give a yellow solid. The resulting solid is collected, washed with diethyl ether and dried to give 0.20 g of product.
MS (FAB): m/z 585 (M+H).
Substantially following the methods described in detail hereinabove, in Examples 5 or 6, the compounds of this invention listed below in Examples 7-22 are prepared.
__________________________________________________________________________Example Starting Material MS(FAB):# Name Prod. of Exp. Reactant Rx Time m/z__________________________________________________________________________ 7 [4S-(4alpha,12aalpha)]-4-(dimethyl- 1 Methylamine 2.5 hrs. 531(M + H)amino)-1,4,4a,5,5a,6,11,12a-octahydro- (40% in water)3,5,10,12,12a-pentahydroxy-6-methyl-9-[[(methylamino)acetyl]amino]-1,11-dioxo-2-naphthacenecarboxamide dihydrochloride 8 [4S-(4alpha,12aalpha)]-4-(Dimethyl- 1 Ethylamine 2.0 hr. 545(M + H)amino)-9-[[(ethylamino)acetyl]amino]- (70% in water)1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,-12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide dihydrochloride 9 [7S-(7alpha,10aalpha)]-N-[9-(Amino- 1 Pyrrolidine 2.0 hr. 571(M + H)carbonyl)-7-(dimethylamino)-5,5a,6,6a,-7,10,10a,12-octahydro-1,6,8,10a,11-penta-hydroxy-5-methyl-10,12-dioxo-2-naphtha-cenyl]-1-pyrrolidineacetamide10 [7S-(7alpha,10aalpha)]-N-[9-(Aminocar- 2 4-Methyl- 1.0 hr. 599(M + H)bonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,- piperidine10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-4-methyl-1-piperidineacetamide11 [4S-(4alpha,12aalpha)]-4-(Dimethylamino)- 2 Propylamine 1 hr. 559(M + H)1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-9-[[(propylamino)acetyl]amino]-2-naphtha-cenecarboxamide dihydrochloride12 [4S-(4alpha,12aalpha)]-9-[[(Butyl- 2 n-Butylamine 2 hr. 573 (M + H)amino)acetyl]amino]-4-(dimethyl-amino)-1,4,4a,5,5a,6,11,12a-octa-hydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecar-boxamide13 [4S-(4alpha,12aalpha)]-4-(Dimethyl- 4 Dimethylamine 2 hr. 559 (M + H)amino)-9-[[2-(dimethylamino)-1-oxo-propyl]amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacene-carboxamide dihydrochloride14 [4S-(4alpha,12aalpha)]-4-(Dimethyl- 1 Amylamine 2 hr. 587(M + H)amino)-1,4,4a,5,5a,6,11,12a-octa-hydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-9-[[(pentylamino)-acetyl]amino]-2-naphthacenecarbox-amide monohydrochloride15 [4S-(4alpha,12aalpha)]-4-(Dimethyl- 1 Dimethylamine 2 hr. 545 (M + H)amino)-9-[[(dimethylamino)acetyl]-amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide16 [4S-(4alpha,12aalpha)]-4-(Dimethyl- 1 Benzylamine 2 hr. 607(M + H)amino)-1,4,4a,5,5a,6,11,12a-octa-hydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-9-[[[(phenylmethyl)-amino]acetyl]amino]-2-naphthacenecar-boxamide dihydrochioride17 [4S-(4alpha,12aalpha)]-4-(Dimethyl- 1 2-Thiophene- 11/2 hr. 613(M + H)amino)-1,4,4a,5,5a,6,11,12a-octa- methylaminehydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-9-[[[(2-thienyl-methyl)amino]acetyl]amino]-2-naphtha-cenecarboxamide dihydrochloride18 [4S-(4alpha,12aalpha)]-4-(Dimethyl- 3 Isobutylamine 2 hr. 573(M + H)amino)-1,4,4a,5,5a,6,11,12a-octa-hydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[[(2-methylpropyl)amino]-acetyl]amino]-1,11-dioxo-2-naphtha-cenecarboxamide dihydrochloride19 [4S-(4alpha,12aalpha)]-4-(Dimethyl- 3 2-(Aminomethyl) 11/2 hr. 608 (M + H)amino)-1,4,4a,5,5a,6,11,12a-octa- pyridinehydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-9-[[[(2-pyridinyl-methyl)amino]acetyl]amino]-2-naphtha-cenecarboxamide dihydrochloride20 [4S-(4alpha,12aalpha)]-9-[[(Diethyl- 1 Diethylamine 11/2 hr. 573 (M + H)amino)acetyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,-12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide21 [7S-(7alpha,l0aalpha)]-N-9-(Aminocar- 3 2-Methyl- 1 hr. 583 (M + H)bonyl)-7-(dimethylamino)-5,5a,6,6a,7,- pyrrolidine10,10a,12-octahydro-1,6,8,10a,11-penta-hydroxy-5-methyl-10,12-dioxo-2-naphtha-cenyl]-alpha-methyl-l-pyrrolidinecar-boxamide22 [4S-(4alpha,12aalpha)]-9-[[[(Cyclo- 3 (Aminomethyl) 1 hr. 571 (M + H)propylmethyl)amino]acetyl]amino]-4- cyclopropane(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacene-carboxamide dihydrochloride23 [4S-(4alpha,12aalpha)]-4-(Dimethyl- 1 t-Butylamine 2 hr. 573 (M + H)amino)-9-[[(t-butylamino)acetyl]-amino]-1,4,4a,5,5a,6,11,12a-octa-hydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecar-boxamide__________________________________________________________________________
EXAMPLE 24
General Procedure for the preparation of Mannich Bases
A mixture of 0.5 mm of product from Example 23 (free base), 3 ml of t-butyl alcohol, 0.55 mm of 37% formaldehyde, and 0.55 mm of pyrrolidine, morpholine or piperidine is stirred at room temperature for 30 minutes followed by heating at 100° C. for 15 minutes. The reaction mixture is cooled to room temperature and triturated with diethyl ether and hexane. The solid is collected, washed with diethyl ether and hexane, and dried to give the desired product. In this manner the following compound is made:
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-9-[[(t-butylamino)acetyl]amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-N-(1-pyrrolidinylmethyl)-2-naphthacenecarboxamide
Substantially following the method described in Example 5, the compounds of this invention listed below in Examples 25-48 are prepared using the product from Examples 1, 2 or 3.
EXAMPLE 25
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[(methoxyamino)acetyl]amino]-1,11-dioxo-2-naphthacenecarboxamide
EXAMPLE 26
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-9-[[[(phenylmethoxy) amino]acetyl]amino]-2-naphthacenecarboxamide
EXAMPLE 27
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-4-ethyl-1H-pyrazole-1-acetamide
EXAMPLE 28
[4S-(4alpha,12aalpha)]-9-[[(Cyclobutylmethylamino)acetyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
EXAMPLE 29
[4S-(4alpha,12aalpha)]-9-[[(2-Butenylamino)acetyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxonaphthacenecarboxamide
EXAMPLE 30
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[(hydroxyamino)acetyl]amino]-1,11-dioxo-2-naphthacenecarboxamide
EXAMPLE 31
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-9-[[[methyl(phenylmethyl)amino]acetyl]amino]-2-naphthacenecarboxamide
EXAMPLE 32
[7S-(7alpha,10aalpha)]-N[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-5-methyl-2,5-diazabicyclo[2.2.1]heptane-2-acetamide
EXAMPLE 33
[7S-[7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-3-methyl-4-morpholineacetamide
EXAMPLE 34
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-2-azabicyclo[2.2.1]heptane-2-acetamide
EXAMPLE 35
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5.a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-6-methyl-2-azabicyclo[2.2.2]octane-2-acetamide
EXAMPLE 36
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-4-methyl-1-piperazinecarboxamide
EXAMPLE 37
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-4-hydroxy-1-piperazineacetamide
EXAMPLE 38
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-3-methyl-1-piperazinecarboxamide
EXAMPLE 39
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-3-cyclopropyltetrahydro-4H-thiazine-4-acetamide
EXAMPLE 40
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-3-ethyl-1H-pyrrole-1-acetamide
EXAMPLE 41
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[(1H-imidazol-2-ylmethylamino)acetyl]amino]-1,11-dioxo-2-naphthacenecarboxamide
EXAMPLE 42
[7S-(7alpha,10aalpha)]-N-[2-[[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]amino]-2-oxoethyl]alanine
EXAMPLE 43
[7S-(7alpha,10aalpha)]-N-[2-[[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]amino]-2-oxoethyl]carbamic acid 1,1-dimethyl ester
EXAMPLE 44
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[[[(2-methylcyclopropyl)oxy]amino]acetyl]amino]-1,11-dioxo-2-naphthacenecarboxamide
EXAMPLE 45
[4S-(4alpha-12aalpha)]-9-[[[(Bicyclo[2.2.2]oct-2-yloxy)amino]acetyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
EXAMPLE 46
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[[(3-methyl-2-butenyl)amino]acetyl]amino]-1,11-dioxo-2-naphthacenecarboxamide
EXAMPLE 47
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[[[4-[(2-methyl-1-oxopropyl)amino]phenyl]amino]acetyl]amino]-1,11-dioxo-2-naphthacenecarboxamide
EXAMPLE 48
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-3-ethyl-1-pyrrolidineacetamide
Substantially following the method described in Example 5, the compounds of this invention listed below in Examples 49-55 are prepared using the product from Example 4.
EXAMPLE 49
[4S-[4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[2-[[(1-methyl-1H-imidazol-2-yl)methyl]amino]-1-oxopropyl]amino]-1,11-dioxo-2-naphthacenecarboxamide
EXAMPLE 50
[4S-(4alpha,12aalpha)]-9-[[2-(Dicyclopropylamino)-1-oxopropyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
EXAMPLE 51
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-10,12-dioxo-2-naphthacenyl]-4-methoxy-α-methyl-1-piperazinecarboxamide
EXAMPLE 52
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]tetrahydro-α,2-dimethyl-4H-1,4-thiazine-4-acetamide
EXAMPLE 53
[7S-(7alpha,10aalpha)]-[2-[[9-(Aminocarbonyl)-7-(dimethylamino]-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]amino]-2-oxo-1-methylethyl]carbamic acid 2-propenyl ester
EXAMPLE 54
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-4-(aminomethyl)-α-methyl-1-piperidineacetamide
EXAMPLE 55
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[2-[[3-(methylsulfonyl)phenyl]amino]-1-oxopropyl]amino]-1,11-dioxo-2-naphthacenecarboxamide
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 56 is prepared.
EXAMPLE 56
[4S-(4alpha,12aalpha)]-9-[(2-Bromo-2-methyl-1-oxopropyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
EXAMPLE 57
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[2-methyl-2-(methylamino)-1-oxopropyl]amino]-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 56 and methylamine.
EXAMPLE 58
[4S(4alpha,12aalpha)]-4-(Dimethylamino)-9-[[2-(dimethylamino)-2-methyl-1-oxopropyl]amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 56 and dimethylamine.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 59 is prepared.
EXAMPLE 59
[4S-(4alpha,12aalpha)]-9-[2-Bromo-1-oxobutyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
EXAMPLE 60
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-9-[[(3-methylcyclobutyl)oxy]amino]-1-oxobutyl]amino]-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 59 and 3-methylcyclobutyloxyamine.
EXAMPLE 61
[4S-(4alpha,12aalpha)]-9-[[2-[(1,1-dimethylethyl)methylamino]-1-oxobutyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 59 and N-methyl-t-butylamine.
EXAMPLE 62
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-α-ethyl-4-methyl-2-isoxazolidineacetamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 59 and 4-methyl-2-isoxazolidine,
EXAMPLE 63
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-α-ethyl-3-methyl-4H-1,2,4-triazole-4-acetamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 59 and 3-methyl-1,2,4-triazole.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 64 is prepared.
EXAMPLE 64
[4S-(4alpha,12aalpha)]-9-[(2-Bromo-1-oxopentyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
EXAMPLE 65
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-9-[[2-(dimethylamino)-1-oxopentyl]amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 64 and dimethylamine.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 66 is prepared.
EXAMPLE 66
[4S,(4alpha,12aalpha)]-9-[(2-Bromo-2-methyl-1-oxobutyl)amino]-4-dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
EXAMPLE 67
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-9-[[2-(ethylamino)-1-methyl-1-oxobutyl]amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 66 and ethylamine.
Substantially following the method, described in detail hereinabove in Example 2, the compound of invention Example 68 is prepared.
EXAMPLE 68
[4S-(4alpha,12aalpha)]-9-[(2-Bromo-3-hydroxy-1-oxopropyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-2 -naphthacenecarboxamide hydrobromide
EXAMPLE 69
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-9-[[2-(dimethylamino)-3-hydroxy-1-oxopropyl]amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 68 and dimethylamine.
EXAMPLE 70
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]-α-(hydroxymethyl)-4-methyl-1H-imidazole-1-acetamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 68 and 4-methylimidazole.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 71 is prepared.
EXAMPLE 71
[4S-(4alpha,12aalpha)]-9-[[2-Bromo-3-mercapto-1-oxopropyl)amino]-4-(dimethylamino)1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
EXAMPLE 72
[4S-(4alpha,12aalpha)]-9-[[2-(Diethylamino)-3-mercapto-1-oxopropyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 71 and diethylamine.
EXAMPLE 73
[7S-(7alpha,10aalpha)]-N-[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10-12-dioxo-2-naphthacenyl]-α-(mercaptomethyl)-1-piperazineacetamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 71 and piperazine.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 74 is prepared.
EXAMPLE 74
[7S-(7alpha,10aalpha)]-4-[[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10-12-dioxo-2-naphthacenyl]amino]-3-bromo-4-oxobutanoic acid hydrobromide
EXAMPLE 75
[7S-(7alpha,10aalpha]-4-[[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,11-dioxo-2-naphthacenyl]amino]-3-(hexylamino)-4-oxobutanoic acid
The titled compound is prepared by the procedure by Example 5. The reactants are the product from Example 74 and n-hexylamine.
EXAMPLE 76
[7S-(7alpha,10aalpha)]-4-[[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a-6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5=-methyl-10,12-dioxo-2-naphthacenyl]amino]tetrahydro-6-(hydroxymethyl]-2H-1,2-isoxazine-2-propanoic acid
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 74 and 6-(hydroxymethyl)-1,2-isoxazine.
EXAMPLE 77
[7S-(7alpha,10aalpha)]-4-[[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]amino]-3-[ethyl(phenylmethyl)amino]-4-oxobutanoic acid
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 74 and N-ethylbenzylamine.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 78 is prepared.
EXAMPLE 78
[7S-(7alpha,10aalpha)]-5-[[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a-11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]amino]-4-bromo-5-oxopentanoic acid hydrobromide
EXAMPLE 79
[7S-(7alpha,10aalpha)]-5-[[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]amino]-4-(cyclopropylamino)-5-oxopentanoic acid
The titled compound is prepared by procedure of Example 5. The reactants are the product from Example 78 and cyclopropylamine.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 80 is prepared.
EXAMPLE 80
[4S-(4alpha,12aalpha)]-9[(α-Bromophenylacetyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
EXAMPLE 81
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-9-[[2-(dimethylamino)-2-phenylacetyl]amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1-11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 80 and dimethylamine.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 82 is prepared.
EXAMPLE 82
[4S-(4alpha,12aalpha)]-9-[[Bromo(4-hydroxyphenyl)acetyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
EXAMPLE 83
[4S-(4alpha,12aalpha)]-9-[[(Butylamino)(4-hydroxyphenyl)acetyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 82 and n-butylamine.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 84 is prepared.
EXAMPLE 84
[4S-(4alpha,12aalpha)]-9-[[Bromo(4-methoxyphenyl)acetyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
EXAMPLE 85
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-9-[2-(dimethylamino)-2-(4-methoxyphenyl)acetyl]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1-11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 84 and dimethylamine.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 86 is prepared.
EXAMPLE 86
[4S-(4alpha,12aalpha)]-9-[[Bromo[4-(trifluoromethyl)phenyl]acetyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
EXAMPLE 87
[4S-(4alpha,12aalpha)]-4-(Dimethylamino)-9-[[2-(ethylmethylamino)-3-[4-(trifluoromethyl)phenyl]acetyl]amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 86 and N-ethylmethylamine.
Substantially following the method, described in detail herein above in Example 2, the compound of invention Example 88 is prepared.
EXAMPLE 88
[4S-(4alpha,12aalpha)]-9-[[Bromo[4-(dimethylamimo)phenyl]acetyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide hydrobromide
EXAMPLE 89
[4S-(4alpha12aalpha)]-4-(Dimethylamino)-9-[[[4-(dimethylamino)phenyl](2-propenylamino)acetyl]amino]-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by the procedure of Example 5. The reactants are the product from Example 88 and N-allylamine.
EXAMPLE 90
[7S-(7alpha,10aalpha)]-N-[2-[[9-(Aminocarbonyl)-7-(dimethylamino)-5,5a,6,6a,7,10,10a,12-octahydro-1,6,8,10a,11-pentahydroxy-5-methyl-10,12-dioxo-2-naphthacenyl]amino]-2-oxoethyl]carbamic acid 1,1-dimethylethyl ester
To a room temperature solution of 0.175 g of N-(tert-butoxycarbonyl)glycine in 5 ml of methylene chloride is added 0.91 g of dicyclohexylcarbodiimide. The reaction mixture is stirred for 30 minutes, filtered and concentrated in vacuo. The residue is dissolved in 2 ml of N-methylpyrrolidone and added to a solution of 0.142 g of 9-amino-5-hydroxy-6-deoxytetracycline in 2 ml of N-methylpyrrolidinone. After 2 hours, the solvent is concentrated in vacuo and the residue is purified by reverse phase chromatography to give 0.160 g of the desired product.
MS(FAB): m/z 617 (M+H)
1 H NMR (CD 3 OH): δ 8.30(d,1H,J=8.1 Hz,H-8); 6.87(d,1H,H-7); 4.37(bs,1H,H-4), 4.18(s,2H,CH 2 CON--); 3.53(dd,1H,J=8.25 and 11.40 Hz,H-5); 2.93(bs,6H,N(CH 3 ) 2 ); 2.70-2.90(m, 2H,H-4a and H-6); 2.51(dd,1H,J=8.25 and 12.36 Hz,H-5a); 1.96(s,9H,t-butyl); 1.50(d,3H,C(6)-CH 3 ).
EXAMPLE 91
[4S-(4alpha,12aalpha)]-9-[(Aminoacetyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The product from Example 90 is dissolved in 4 ml of trifluoroacetic acid/anisole (9:1), stirred for 45 minutes and slowly poured into 150 ml of diethyl ether. The precipitate is collected and purified by reverse phase chromatography to give 0.10 g of the desired product as a gold glass.
MS (FAB): m/z 517 (M+H).
1 H NMR (CD 3 OH): δ 8.24(d,1H,J=8.2 Hz,H-8); 6.92(d,1H,H-7); 4.35(bs,1H,H-4); 3.91(s,2H,CH 2 CON--); 3.52(dd,1H,J=8.24 and 11.40 Hz,H-5); 2.92(bs,6H,N(CH 3 ) 2 ); 2.70-2.90(m,2H,H-4a and H-6); 2.52(dd,1H,J=8.24 and 12.36 Hz,H-5a); 1.50(d,3H,C(6)-CH 2 ).
EXAMPLE 92
[4S-(4alpha,12aalpha)]-9-[L-(N-Methylleucyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The title compound is prepared by the tandem procedure of Examples 90 and 91. N-(tert-butoxycarbonyl)-N-methyl-L-leucine is coupled with 9-amino-5-hydroxy-6-deoxytetracycline to give the protected intermediate which is then deprotected and purified to give the desired compound.
MS(FAB): m/z 587 (M+H).
1 H NMR (CD 3 OH): δ 8.11(d,1H,J=8.2 Hz,H-8); 6.97(d,1H,H-7); 4.37(bs,1H,H-4); 4.08(dd,1H,CHCONH); 3.53(dd,1H,J=8.25 and 11.40 Hz,H-5); 2.94(bs,6H,NMe 2 ); 2.70-2.90(m,2H,H-4a and H-6); 2.71(s,3H,NCH 3 ); 2.51(dd,1H,J=8.25 and 12.36 Hz,H-5a); 1.52(d,3H, J=7.1 Hz, C(6)-CH 3 ); 1.5-1.6(m,3H,CH--CH 2 C); 0.90(d,6H,Me 2 CH).
EXAMPLE 93
[4S-(4alpha,12aalpha)-9-[(L-Glutamyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The title compound is prepared by the tandem procedure of Example 90 and 91. tert-Butyl N-(tert-butoxycarbonyl)-γ-L-glutamate is coupled with 9-amino-5-hydroxy-6-deoxytetracycline to give the protected intermediate which is then deprotected and purified to give the desired compound.
MS(FAB): m/z 589 (M+H).
EXAMPLE 94
[4S-(4alpha,12aalpha)-9-[(L-Aspartyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The title compound is prepared by the tandem procedure of Example 90 and 91. tert-Butyl N-(tert-butoxycarbonyl)-β-L-aspartate is coupled with 9-amino-5-hydroxy-6-deoxytetracycline to give the protected intermediate which is then deprotected and purified to give the desired compound.
MS(FAB): m/z 575 (M+H).
EXAMPLE 95
[4S-(4alpha,12aalpha)]-9[(D-Phenylalanyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
To a room temperature solution of 0.40 g of N-(9-fluorenylmethoxycarbonyl)-D-phenylalanine in 20 ml of methylene chloride/tetrahydrofuran (1:1) is added 0.095 g of dicyclohexylcarbodiimide. The reaction mixture is stirred for 1 hour, filtered and concentrated in vacuo. The residue is added to a solution of 0.151 g 9-amino-5-hydroxy-6-deoxytetracycline in 3 ml of N-methylpyrrolidone and the mixture is stirred for 4 hours. One ml of piperidine is added and the mixture stirred for an additional 20 minutes. The reaction mixture is slowly poured into 150 ml of stirring diethyl ether and the resulting precipitate is collected. The light yellow powder is purified by preparative chromatography to give 0.049 g of the desired product as a dark yellow glass.
MS(FAB): m/z 607 (M+H).
1 H NMR (CD 3 OH): δ 8.11(d,1H,J=6.9 Hz,H-8); 7.31(bs,5H,C 6 H 5 ); 6.92(d,1H,H-7); 4.40(t,1H,J=8.9 Hz, CHCO); 4.37(bs,1H,H-4); 3.53(dd,J=8.25 and 11.40 Hz, H-5); 3.15(d,2H,J=8.9 Hz,CH 2 CHO); 2.92(bs,6H,NMe 2 ); 2.70-2.90(m,2H,H-4a and H-6); 2.51(dd,1H,J=8.25 and 12.35 Hz,H-5a); and 1.50(d,3H,J=7.1 Hz,-C(6)-CH 3 ).
EXAMPLE 96
[4S-(4alpha,12aalpha)]-9-[(L-Phenylalanyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The title compound is prepared by the procedure of Example 92 using N-(9-fluorenylmethoxycarbonyl)-L-phenylalanine as the α-aminoacyl component.
MS(FAB): m/z 607 (M+H).
1 H NMR (CD 3 OH): δ 8.11(d,1H,J=6.9 Hz,H-8); 7.31(bs,5H, C 6 H 5 ); 6.92(d,1H,H-7); 4.40(t,1H,J=8.9 Hz; CHCO); 4.37(bs,1H,H-4); 3.53(dd,J=8.25 and 11.40 Hz, H-5); 3.15(d,2H,J=8.9 Hz, CH 2 CHO); 2.92(bs,6H,NMe 2 ), 2.70-2.90(m,2H,H-4a and H-6); 2.51(dd,1H,J=8.25 and 12.35 Hz,H-5a); and 1.50(d,3H,J=7.1 Hz, C(6)-CH 3 ).
EXAMPLE 97
[4S-(4alpha,12aalpha)]-9-[[L-β-(Cyclohexyl)alanyl]amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The tile compound is prepared by the procedure of Example 92 using N-(9-fluorenylmethoxycarbonyl)-β-cyclohexyl-L-alanine as the α-aminoacyl component.
MS(FAB): m/z 613 (M+H).
EXAMPLE 98
[4S-(4alpha,12aalpha)]-9-[(L-Leucyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The tile compound is prepared by the procedure of Example 92 using N-(9-fluorenylmethoxycarbonyl)-L-leucine as the α-aminoacyl component.
MS (FAB): m/z 573 (M+H).
EXAMPLE 99
[4S-(4alpha,12aalpha)-9-[(L-Glutaminyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The tile compound is prepared by the procedure of Example 92 using N-(9-fluorenylmethoxycarbonyl)-L-glutamine as the α-aminoacyl component.
MS(FAB): m/z 588 (M+H).
EXAMPLE 100
[4S-(4alpha,12aalpha)-9-[(L-Prolyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The title compound is prepared by the procedure of Example 90 coupling L-proline with 9-amino-5-hydroxy-6-deoxytetracycline.
MS (FAB): m/z 557 (M+H).
EXAMPLE 101
[4S-(4alpha,12aalpha)-9-[(L-(N,N-Dimethylphenylalanyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The title compound is prepared by the procedure of Example 90 coupling L-(N,N-dimethyl)phenylalanine with 9-amino-5-hydroxy-6-deoxytetracycline.
MS(FAB): m/z 635 (M+H).
EXAMPLE 102
[4S-(4alpha,12aalpha)-9-[(n-Tyrosinyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
To a room temperature solution of 4.60 g of N-(9-fluorenylmethoxycarbonyl)-O-(tert-butyl)-L-tyrosine in 50 ml of methylene chloride/tetrahydrofuran (1:1) is added 1.04 g of dicyclohexylcarbodiimide. The reaction mixture is stirred for 1 hour, filtered and concentrated in vacuo. The residue is added to a solution of 2.30 g 9-amino-5-hydroxy-6-deoxytetracycline in 30 ml of N-methylpyrrolidone and the mixture is stirred for 4 hours. Five ml of piperidine is added, the mixture stirred for an additional 30 minutes and concentrated in vacuo. The residue is dissolved in 30 ml of trifluoroacetic acid/anisole (9:1), stirred for 45 minutes and slowly poured into 1000 ml of diethyl ether. The resulting precipitate is collected and purified by reverse phase chromatography to give 1.3 g of the desired product as a gold glass.
MS(FAB): m/z 623 (M+H).
EXAMPLE 103
[4S-(4alpha,12aalpha)-9-[(L-Lysyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The title compound is prepared by procedure of Example 102 using N.sup.α -(9-fluorenylmethoxycarbonyl)-N.sup.γ -(tert-butoxycarbonyl)-L-lysine and 9-amino-5-hydroxy-6-deoxytetracycline.
MS(FAB): m/z 588 (M+H).
EXAMPLE 104
[4S-(4alpha,12aalpha)-9-[(L-Tryptophanyl)amino]-4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,5,10,12,12a-pentahydroxy-6-methyl-1,11-dioxo-2-naphthacenecarboxamide
The titled compound is prepared by procedure of Example 102 using N.sup.α -(9-fluorenylmethoxycarbonyl)-N-trityl-L-tryptophan and 9-amino-5-hydroxy-6-deoxytetracycline.
MS(FAB): m/z 646 (M+H). | The invention provides compounds of the formula: ##STR1## wherein R, R 1 , R 2 and W are defined in the specification. These compounds are useful as antibiotic agents. | 2 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a divisional of U.S. patent application Ser. No. 09/910,245 filed on Jul. 20, 2001 which application claims priority of U.S. provisional patent application 60/265,444 filed Jan. 31, 2001.
BACKGROUND OF INVENTION
[0002] Drilling rigs use blowout preventers (BOPs) to shut in a well during emergencies and for other purposes. The BOP operating system needs to be reliable in order to protect lives, the environment, and property. This invention relates to an improved BOP operating system and a quick dump valve. The quick dump valve includes a shuttle that has some structural similarity to shuttle valves used for control functions in prior art BOP operating systems. Specifically, the quick dump valve has some structural similarities to the Low Interflow Hydraulic Shuttle Valve which is the subject of a pending U.S. patent application Ser. No. 09/452,594 filed on Dec. 1, 1999 and a pending U.S. patent application Ser. No. 09/653,415 for a Pressure Biased Shuttle Valve filed on Sep. 1, 2000, both of which are incorporated herein by reference. Gilmore Valve Co. is the owner of these two pending U.S. Patent Applications, the present patent application for BOP Operating System with Quick Dump Valve and other U.S. patents for shuttle valves including U.S. Pat. Nos. 3,533,431 and 4,253,481. However, the present invention is structurally distinct from these prior art shuttle valves and it performs a different function as discussed below.
DESCRIPTION OF THE PRIOR ART
[0003] Subsea wellhead systems are often relied upon during deep-water exploration for oil and natural gas. The subsea wellhead system includes a stack of BOPs. Annular BOPs are actuated on a routine basis to snub or otherwise control pressure during normal drilling operations. Other blowout preventers, such as blind rams, pipe rams, and shear rams will also be included in the stack on the subsea wellhead. When these types of rams are actuated, operations in the well cease in order to control pressure or some other anomaly. Blind rams, pipe rams, shear rams and annular preventers are periodically functioned and tested to make sure that they are operational.
[0004] BOPs are tested periodically to ensure that they will function in emergencies and in other situations. Prior art subsea BOP operating systems include a control podcontrol pods, the lower marine riser package (LMRP), the BOP stack and interconnecting hoses and pipes. From time to time it may be necessary to perform an emergency disconnect of the LMRP from the BOP stack, for example, if a drill ship drifts off station or if a storm approaches. If it is necessary to make an emergency disconnect of the LMRP from the BOP stack, it will be necessary to close the shear rams. During the closing sequence, hydraulic fluid is forced through pipes or hose, a shuttle valve and additional segments of pipes or hose before it finally reaches the directional control valve vent port on the control pod where it is vented to the ocean. This circuitous hydraulic vent path results in a high differential pressure, which decreases flow of control fluid through the close side of the operating system. The decreased flow consumes valuable seconds, and as such, increases the time required to close the shear rams and disconnect the LMRP from the BOP stack. In prior art BOP operating systems, pilot operated check valves or conventional sub-plate mounted (SPM) poppet valves were used to vent this fluid during the closing sequence. These prior art vent devices rely upon springs or pilot pressure to operate properly.
[0005] The present dump valve for use in the improved BOP operating system utilizes a ported shuttle that automatically shifts with the direction of hydraulic pressure to either expose or seal the vent port in the valve. The present dump valve has two positions vent and open. It has several advantages over the prior art due to its location in the BOP operating system and its design. These advantages occur when the valve is in both the vent and the open positions as discussed below. The present dump valve is a much simpler design than the prior art pilot operated check valves and conventional SPM valves.
[0006] The present dump valve and improved BOP operating system are designed to reduce hydraulic shock and vibration, to reduce the incidence of hose collapse on both the close side and the open side of the system, to facilitate installation and maintenance, and to shorten the emergency disconnect sequence of the LMRP from the BOP stack. In some prior art systems, hydraulic shock and vibration would sometimes accompany the closing function.
[0007] In the improved BOP operating system the dump valve of the present invention is located at or near the open port of the BOP. During the closing sequence in the improved BOP operating system, the present dump valve is shifted to the vent position. In this position fluid is vented from the BOP operating system. When it is time to open the shear rams, fluid flow reverses through the dump valve and it moves to the open position. In the open position, the vent is closed allowing fluid to move through the open port into the BOP to open the rams.
[0008] Some BOP hoses may collapse in deep water when subjected to high velocity flows of hydraulic fluid resulting from functioning of the BOPs with large capacity operators. Hose collapse is, of course, undesirable. The present dump valve and the improved BOP operating system are designed to reduce flow velocities in the control system, and thereby reduce the incidence of BOP control hose collapse. In the improved BOP operating system, the dump valve is positioned at or near the open port on the BOP to vent fluid from the system during the closing sequence. Because the dump valve is located at or near the open port on the Ram's BOP, this high velocity fluid is vented and does not pass through the open side hose. The control hoses on the open side of the BOP will, therefore, be less prone to collapse because they are no longer exposed to the hydraulic shock and negative pressure waves caused by high velocity flow of fluid when the BOP rams are being closed.
[0009] When the rams are being opened, the dump valve also acts as a dampener to reduce the incidence of hose collapse on the close side of the operating system. In a preferred embodiment, when the rams are functioned open, fluid passing through the dump valve is restricted because the orifice through the dump valve is smaller than the inside diameter of the hose leading to and exiting from the dump valve. This flow restrictor will effectively slow down the velocity of the fluid entering the BOP rams. In turn, the velocity of the exhausting fluid from the close side will be reduced to a rate that reduces hydraulic shock and therefore reduces the incidence of hose collapse. In some prior art BOP operating systems, it may take as much as 20 seconds to close and open the rams. The improved BOP operating system with quick dump valve should allow the rams to close in approximately 5 to 15 seconds; however, it may take more than 30 seconds for the rams to open.
[0010] Maintenance on prior art BOP operating systems is sometimes lengthy and expensive. The present dump valve is smaller and lighter than conventional SPM valves or pilot operated check valves, which will facilitate valve installation reliability and maintenance.
[0011] The improved BOP operating system with quick dump valve should reduce the amount of time it takes to make an emergency disconnect of the LMRP from the BOP stack. In prior art BOP operating systems when it was necessary to close the rams, fluid was forced through a length of hydraulic hose, a shuttle valve and additional segments of tubing or hose before it finally reached the directional control valve vent port on the control pod. This circuitous hydraulic vent path on the close side of prior art operating systems results in a high differential pressure, which decreases flow of control fluid when the rams are being closed. The decreased flow consumes valuable seconds and, as such, increases the time required to close the rams and disconnect the LMRP from the BOP stack. Positioning the quick dump valve at or near the BOP Ram's open port will substantially shorten the hydraulic vent path and reduce the differential pressure. All of these features will reduce the amount of time required to close the BOP rams during an emergency and thus speed up the disconnect of the LMRP from the BOP stack.
SUMMARY OF INVENTION
[0012] The quick dump valve uses a ported shuttle design that shifts to either expose or seal off the vent port in the valve. When the BOP is being closed, the shuttle moves to the vent position allowing fluid to be vented from the improved operating system. This vent function which is located at or near the BOP prevents high velocity fluid from passing through the open side hose thus reducing the incidence of hydraulic shock, vibration and hose collapse.
[0013] When the BOP is being opened, the shuttle in the dump valve moves to the open position allowing fluid to pass through the dump valve and into the BOP. A flow restrictor is positioned in the shuttle, which acts as a dampener to reduce hydraulic shock, vibration and the incidence of hose collapse on the close side of the BOP rams. While the BOP is being opened, it is important that the shuttle achieve a good seal to prevent fluid from escaping to vent. The diameter on the supply side of the shuttle is larger than the diameter on the BOP side which results in more force being applied to the seals to prevent unwanted fluid from escaping to vent while the BOP is being opened.
[0014] In some situations, it is desirable to prevent fluid from flowing to supply when fluid is escaping to vent while the BOP is being opened. In the first alternative embodiment, a ball check valve, is positioned in the shuttle to block fluid flow from the BOP to supply when the dump valve is in the vent position. In the first alternative embodiment, the diameter on the supply side of the shuttle is larger than the diameter on the BOP side, which results in more force being applied to the seals to prevent unwanted fluid from escaping to vent while the BOP is being opened.
[0015] In the second alternative embodiment, a ball check valve is positioned in the shuttle to block fluid flow from the BOP to supply when the dump valve is in the vent position. In the second alternative embodiment, the diameter on the supply side of the shuttle is the same diameter as in the BOP side. The cracking pressure of the check valve results in the differential pressure and force required to energize the metal to metal face seal. Differential area was utilized to accomplish this in the alternative and first alternative embodiment.
[0016] In the third alternative embodiment, there is no internal check valve and the diameter on the supply side of the shuttle is the same diameter as on the BOP side. In the third alternative embodiment soft seals are used on both sides of the shuttle to achieve a seal. These seals may be located in either the shuttle or adapters.
BRIEF DESCRIPTION OF DRAWINGS
[0017] In order to more fully understand the aforementioned features, advantages and objects of the present invention, a more detailed description of the invention is provided in the appended drawings. It is noted, however, that the appended drawings illustrate only a typical embodiment of this invention and are therefore not to be considered limiting of its scope, for the invention may admit to other equally effective embodiments. Reference the appended drawings, wherein:
[0018] [0018]FIG. 1 is a hydraulic circuit showing the BOP rams in the closed position and the quick dump valve of the present invention in the vent position.
[0019] [0019]FIG. 2 is a hydraulic circuit showing the BOP rams in the open position and the dump valve of the present invention in the open position.
[0020] [0020]FIG. 3 is a perspective view of a preferred embodiment of the quick dump valve of the present invention.
[0021] [0021]FIG. 4 is a section view of the quick dump valve of FIG. 3 in the vent position with flow arrows showing the direction of fluid flow from the BOP through the dump valve and out the vent.
[0022] [0022]FIG. 5 is a section view of the dump valve of FIG. 3 in the open position with flow arrows showing the flow of fluid from supply through the dump valve through the BOP.
[0023] [0023]FIG. 6 is an enlargement of the metal to metal seal 6 shown in FIG. 5.
[0024] [0024]FIG. 7 is an alternative embodiment of the dump valve of the present invention including a ball check valve. This ball check valve eliminates all return flow through the supply side hydraulics during venting. The supply side of the shuttle has a larger diameter than the BOP side.
[0025] [0025]FIG. 8 is a second alternative embodiment of the dump valve of the present invention including a ball check valve. Both sides of the shuttle are the same diameter. The spring in the ball check valve creates a differential pressure across the shuttle and the force necessary to energize the metal seal.
[0026] [0026]FIG. 9 is a third alternative embodiment of the dump valve of the present invention having soft seals. Both sides of the shuttle have approximately the same diameter. Axial force is not required to energize these seals as in the previously described embodiment.
DETAILED DESCRIPTION
[0027] The quick dump valve uses a ported shuttle design that shifts to either expose or seal off the vent port in the valve. When the BOP is being closed, the shuttle moves to the vent position, allowing fluid to be vented from the improved operating system. This vent function which is located at or near the BOP prevents high velocity fluid from passing through the open side hose, thus reducing the incidence of hydraulic shock, vibration and hose collapse.
[0028] Control pods, attached to the LMRP, direct hydraulic operating fluid to all the functions on the BOP and LMRP. The LMRP is positioned on the BOP stack. BOP control systems have two (2) redundant hydraulic systems commonly referred to in the industry as blue and yellow pods.
[0029] [0029]FIG. 1 is a hydraulic circuit diagram of a portion of the improved BOP operating system with the quick dump valve 10 positioned at or near the open port on the BOP. In FIG. 1, fluid flows from the yellow pod hydraulic supply through valves on the control pod through the shuttle valve generally identified by the numeral 12 through hoses 14 as identified by the flow arrow to the close port 16 in the BOP assembly 18 . This side of the operating system is referred to as the close side of the system because fluid flows into this side when the rams are functioned close. A piston 20 divides the BOP assembly 18 into a close chamber 22 and an open chamber 24 . A rod 26 extends from the piston 20 to the BOP rams.
[0030] The open chamber 24 connects to an open port 28 , which connects to a short conduit 30 , which connects to the quick dump valve 10 . Alternatively, the dump valve 10 can be directly connected to the open port 28 . Additional hoses 32 connect the dump valve 10 to one of three ports on the shuttle valve generally identified by the numeral 35 . The other two ports on the shuttle valve 35 connect to the blue pod and the yellow pod hydraulic supply as well known to those skilled in the art. When either the blue pod accumulators or the yellow pod accumulators are energizedWhen hydraulic fluid is directed from either the blue or yellow pods, the shuttle valve 35 seals off the path of the non-energized hydraulic system and routes the fluid to the BOP.
[0031] In order to open the rams as shown in FIG. 1, high pressure fluid exits from a pod, in this case the yellow pod, and moves through the shuttle valve 12 , the conduit 14 , the close port 16 and enters the close chamber 22 thus moving the piston 20 to the left-hand side of the BOP assembly 18 as shown in FIG. 1. As high-pressure fluid enters the close chamber 22 , fluid must exit the open chamber 24 . As the piston 20 moves to the closed position, the fluid in the open chamber 24 moves into the dump valve 10 , shifting it to the vent position (FIG. 4) thus venting the fluid to sea. During the closing process fluid is being vented through the dump valve 10 . After the BOP is closed, the pressure in the close chamber 24 equalizes and no further fluid is vented. However, the shuttle 36 in the dump valve 10 remains in the vent position until the BOP is opened. During vent flow the majority of the fluid exhausts through the vent port 44 of the dump valve 10 . A small portion of fluid, between 10 to 20%, flows through the flow restrictor passage 82 in the shuttle, and back through the shuttle valves 35 where it exhausts to the ocean (via components not shown in FIG. 1). Because the flow rate back through the shuttle valves is greatly reduced, energy which can trigger vibration or oscillation is also low. As an alternative configuration a check valve can be employed in the inside of the dump valve 10 to totally eliminate this flow.
[0032] The BOP assembly 18 operates with fluids that are flowing as fast as 320 gpm at pressures of 1500 to 3000 psi. These high pressures and high flow rates sometimes create hydraulic shock and vibration in the BOP operating system generally shown in FIG. 1. Prior art SPM's and pilot operated check valves are sometimes installed in “Tee” connections located near the BOP on both the opening and closing sides. These valves are actuated by external means to vent return flow to the ocean. This is similar to the function performed by the dump valve 10 , however, the dump valve 10 is a much simpler device containing fewer moving parts, and therefore improved reliability. Also due to the greater size of the prior art SPM's and pilot operated check valves, they must be mounted in the BOP frame or other structure which is a greater distance away than the location of the present dump valve 10 , increasing the resistance to vent flow. In the improved operating system of FIG. 1, the dump valve 10 is installed at the open port 28 or in close proximity thereto by conduit 30 . When the BOP is closed as shown in FIG. 1, the dump valve 10 is in the vent position allowing fluid from the close chamber 24 to vent from the operating system. This reduces hydraulic shock and vibration and the incident of hose collapse on the open side of the operating system. The improved BOP operating system of FIG. 1 with the quick dump valve 10 allows the BOP rams to be closed more quickly than most prior art systems because the fluid from the open chamber 24 is vented from the system at or near the open port 28 . Some prior art systems took up to 20 seconds to close. The present invention should be able to close in 5-15 seconds.
[0033] The dump valve 10 is smaller and lighter than conventional SPM or pilot operated check valves which should facilitate installation and maintenance on the improved BOP operating system. The dump valve 10 is a simpler more reliable design than prior art SPM and pilot operated check valves.
[0034] [0034]FIG. 2 is a partial hydraulic circuit diagram portion of the improved BOP operating system. In order to open the BOP rams, high pressure fluid flows from the blue pod hydraulic supply through the shuttle valve 35 through the piping and/or hose 32 and enters the dump valve 10 . The velocity of this fluid causes the dump valve to move from the vent position of FIG. 4 to the open position of FIG. 5. In the open position, fluid passes through a flow restrictor in the dump valve 10 to the open port 28 and into the open chamber 24 . This causes the piston 20 to move towards the right-hand side of the drawing, which retracts the rod 26 thus opening the BOP. As the piston 20 moves from the full closed position of FIG. 1 to the full open position, fluid in the closed chamber 22 moves through the close port 16 and the hose 14 on the close side of the BOP operating system. In order to dampen hydraulic shock, the present invention will take more than 30 seconds to open, but this is acceptable because the open function does not occur under emergency conditions.
[0035] [0035]FIG. 3 is a perspective view of the dump valve 10 , which is supported by brackets 38 and 40 . The dump valve 10 has a supply port 34 , which connects to the hose 32 on the open side of the operating system. A BOP port 42 connects to the hose 30 or directly to the open port 28 . A vent port 44 is connected to conduits, which are vented to sea.
[0036] [0036]FIG. 4 is a section view of the dump valve 10 in the vent position. In this position, fluid moves from the open chamber 24 , through the valve 10 and is vented to sea. When the shuttle 36 is in the vent position fluid flows through the dump valve 10 as shown by the flow arrows in the drawing. Fluid enters the dump valve 10 through the BOP port 42 and exits through the vent port 44 as shown by the flow arrows. The body 46 has a longitudinal bore that is threaded to receive the supply adapter 48 and the BOP adapter 50 . An O-ring 52 is positioned in channel 51 and between the body 46 and the BOP adapter 50 thus creating a seal between these two components. Another O-ring 54 is positioned between the supply adapter 48 and the body 46 to create a seal between these two components. The body also has a transverse bore which forms the vent port 44 and which connects to the longitudinal bore.
[0037] The shuttle 36 has a central radial collar 56 and opposing end portions 58 and 60 . The diameter, identified by the arrow A, of the end portion 58 , is larger than the diameter, identified by the arrow B, of the end portion 60 . This step in diameter produces greater area on the supply end 58 . When the shuttle 36 is in the open position shown in FIG. 5, and the BOP piston 20 has reached full travel stopping flow and equalizing the pressure across the shuttle, a difference in force is created by this greater area on the supply end holding the shuttle in the open position and effecting a metal to metal seal as shown in FIGS. 5 and 6. The area of the end portion 58 should be larger than the area of the end portion 60 to ensure a good seal. Applicants have determined that a good seal can be achieved if the area of end portion 58 is approximately 1.5 times greater than the area of the end portion 60 ; however other area ratios may be suitable, provided that a good seal is achieved when the valve 10 is in the open position as shown in FIGS. 5 and 6.
[0038] The end portion 58 has an O-ring groove 61 formed therein. An O-ring 62 and a first backup ring 64 and a second backup ring 66 are positioned in the O-ring groove 61 . The O-ring can be formed from conventional materials such as nitrile rubber provided that they will meet operational temperatures in the subsea environment. The backup rings are typically produced from polymers such as Delrin® or Teflon®.
[0039] The end portion 60 includes a plurality of apertures 68 , 70 , 72 , 74 and others not shown. These transverse apertures connect with a bore 76 to allow fluids to flow through the dump valve 10 to the vent port 44 as shown by the flow arrows in FIG. 4. Fluids flow from the open chamber 24 to the open port 28 , through the conduit 30 to the BOP port 42 through the bore 76 , and the plurality of apertures 68 , 70 , 72 and 74 to the vent port 44 and hence to sea.
[0040] A bore 80 is formed in the longitudinal axis of the end portion 58 of the shuttle 36 . A flow restrictor 82 allows fluid communication between the bore 80 and the bore 76 better seen in the next figure FIG. 5.
[0041] [0041]FIG. 5 is a section view of the dump valve 10 in the open position allowing fluid to flow through the dump valve 10 to the open chamber 24 of the BOP assembly 18 as shown by the flow arrows. Fluid enters the supply port 34 , passes through the bore 80 , the flow restrictor 82 , the bore 76 , the BOP port 42 and thereafter flows into the open chamber 24 in the BOP assembly 18 as better seen in FIG. 1. For a one inch dump valve, applicants have determined that a flow restrictor with an I.D. of from 0.156 to 0.375 inches is suitable. The 0.156 inch I.D. flow restrictor allows a flow rate of 20 gpm at 1500 psi differential pressure.
[0042] The shuttle 36 is typically located in one of two positions. The vent position is shown in FIG. 4 and the open position is shown in FIG. 5. When the shuttle is in the vent position of FIG. 4 the shoulder 55 abuts the supply adapter 48 . When the shuttle 36 is in the open position of FIG. 5, the end portion 58 of shuttle 36 is in sealing engagement with the supply adapter 48 and the end portion 60 of shuttle 36 is in sealing engagement with the BOP adapter 50 . Various types of seals could be used to accomplish a seal between the end portion 58 and the adapter 48 and the end portion 60 and the adapter 50 , including metal to metal seals or soft seals. It is important that the seals utilized withstand the high pressures and flow velocities encountered in this application. It is important that the shuttle 36 achieve a seal with the adapter 48 and adapter 50 when the shuttle is in the open position as shown in FIG. 5. Otherwise hydraulic fluid will bleed out the vent and slow down or thwart efforts to open the BOP rams. Likewise a good seal between the shuttle 36 and the adapter 48 and adapter 50 is important when the valve 10 is in the vent position.
[0043] [0043]FIG. 6 is an enlarged section view of the end portion 60 of the shuttle 36 and a portion of the BOP adapter 50 using metal to metal seals. Again, other types of seals may be suitable for this valve and the selection of metal to metal seals is a manufacturing choice. The shuttle 36 includes a circumfrential flange 56 with a shoulder 57 which is a part of end portion 60 . An outwardly tapered metal sealing surface 100 is formed on the shoulder 57 . Applicants believe that a taper of approximately 8° is optimum for this application. However, other tapers in the range of 5-15° may also be effective so long as they create a coining effect on the metal valve seat 102 of the supply adapter 50 . The only requirement for the angle of taper is to achieve coining and therefore sealing between the sealing surface 100 and the metal valve seat 102 . FIG. 6 shows the sealing surfaces after the dump valve 10 has been manufactured but before any coining has occurred.
[0044] The adapter 50 includes a chamfer 104 recessed behind the metal valve seat 102 to thereby create an obtuse metal point 106 that will contact the tapered metal sealing surface 100 on the flange 56 of the shuttle 36 . Coining occurs when the shuttle moves back and forth from the vent to the open positions. As the shuttle moves back and forth, the tapered metal sealing surface 100 impacts the point 106 and metal it displaced from the point 106 to the chamfer 104 . This displacement of metal is referred to as coining.
[0045] [0045]FIG. 6 shows the metal valve seat 102 and the metal sealing surface 100 on the end portion 60 of shuttle 36 before any coining has occurred. Applicant uses a chamfer with a 15° angle and a 0.015 inch radius. However, the exact size and depth of the chamfer are not particularly critical because this is merely a recess or space into which displaced metal will move due to progressive coining. A step back shoulder or other recess in lieu of the chamfer may also prove effective provided that there is room to receive the displaced metal from the point 106 such that it does not interfere with movement of the shuttle 36 .
[0046] After the shuttle 36 has moved back and forth on several occasions, the metal sealing surface 100 of the shuttle 36 impacts the point 106 of the metal valve seat 102 , and a portion of the metal in the point 106 is displaced into the chamfer 104 . A metal to metal seal is therefore achieved between the metal valve seat 102 and the outwardly tapered metal sealing surface 100 of the flange 56 on the shuttle 36 .
[0047] [0047]FIG. 7 is an alternative embodiment of the dump valve in the vent position. The valve 210 is constructed in a manner similar to the valve of FIG. 4 and includes a body 246 defining a vent port 244 , a BOP adapter 250 defining a BOP port 242 and a supply adapter 248 defining a supply port 234 . The shuttle 236 includes an end portion 258 and opposite end portion 260 . The shuttle 236 includes a bore 280 having a shoulder 294 . A ball check valve assembly 283 includes a ball 284 that is held in place against a valve seat 288 by spring 286 which rests against the shoulder 294 . The valve seat 288 threadably engages the shuttle at shuttle threads 292 and seat threads 290 .
[0048] When the valve 210 is in vent position, as is shown by the flow arrows in FIG. 7 , the spring 286 holds the ball 284 against the valve seat 288 to prevent fluid flow to the supply port 234 . The end portion 258 has an O-ring groove 61 formed therein. An O-ring 62 is positioned in the O-ring groove 61 creating a seal between the adapter 248 and the shuttle 236 . Thus, when the valve 210 is in the vent position as shown, in FIG. 7 no fluid flows to supply because of the seal achieved by the O-ring 62 with adapter 248 and the ball check valve assembly 283 . However, when the valve 210 is in the open position, fluid pressure acting on the ball overcomes the spring force moving the ball away from the seal and allowing fluid to flow from supply to the BOP. The O-ring 62 makes a seal with adapter 248 to prevent fluid from escaping to vent when the valve is in the open position. The metal valve seat 102 and the metal sealing surface 100 on end portion 260 achieve a seal between the shuttle 236 and the adapter 250 , to likewise prevent fluid from escaping to vent when the valve is in the open position.
[0049] The diameter of the end portion 258 is larger than the diameter of end portion 260 . This step in diameter produces greater area on the supply end 258 . When the shuttle 236 is in the open position, and the BOP piston 20 has reached full travel stopping flow and equalizing the pressure across the shuttle, a difference in force is created by this greater area on the supply end portion 258 holding the shuttle in the open position. Applicants have determined that a metal to metal seal can be achieved if the area of end portion 258 is approximately 1.5 times greater than the area of the end portion 260 ; however, other area ratios maybe suitable, provided that a good seal is achieved when the valve is in the open position.
[0050] [0050]FIG. 8 illustrates a second alternative embodiment of the dump valve which includes the ball check assembly 283 , and including supply, vent and BOP ports of essentially the equal diameter. The body 346 defines the vent port 344 , and the adapters 350 and 348394 define the BOP port 342 and the supply port 334 respectively. The ball check valve assembly 283 includes a ball 384 , a spring 394386 and a valve seat 388 .
[0051] The metal valve seat 102 and the sealing surface 100 on the end portion 360 of shuttle 336 achieve a seal between the shuttle 336 and the adapter 350 , to prevent fluid from escaping to vent when the valve is in the open position.
[0052] The shuttle 336 has end portion 358 and opposite end portion 360 of approximately equal diameters. When in the open position, the spring 386 in the ball check valve results in the pressure on the supply side of the shuttle 336 to be greater than the pressure on the BOP side of the shuttle, resulting in a force pushing the shuttle 336 against the BOP adapter 350 , and effecting a seal between the tapered sealing surface 100 and the metal valve seat 102 .
[0053] [0053]FIG. 9 is a third alternative embodiment of the dump valve. The valve 410 is constructed in the same manner as the valve of FIGS. 3 - 5 , with the exception of the shuttle, the relative port diameters and the soft seal assembly. The shuttle 436 has end portion 458 and opposing end portion 460 . End portion 458 engages supply adapter 448 . End portion 460 engages BOP adapter 450 . Adapters 448 and 450 are of equal size and shape. In FIG. 9 the metal to metal seal illustrated in FIG. 6 is replaced by a soft seal created by O-ring 96 which is located in channel 98 of the shuttle 436 . Further, the diameters of the supply port 434 , vent port 444 and BOP port 442 are all the same diameter, which may be advantageous for particular applications. The type of seals employed do not require axial force to be energized as in the previous embodiments discussed.
[0054] The shuttle 436 has end portion 458 and opposing end portion 460 , both of which are of approximately equal diameter. Thus, the forces exerted by the fluid on the shuttle 436 are balanced when the shuttle 436 is in the vent position of FIG. 9 and the open position, not shown. As previously discussed, the type of seal is a matter of manufacturing convenience. The valve 410 uses two soft seals, i.e., the O-ring 96 and the O-ring 62 . As a matter of manufacturing choice, other types of seals could also be employed. A check valve could also be utilized in this concept if desired.
[0055] Having described the invention in detail, those skilled in the art will appreciate that modifications may be made of the invention without departing from its spirit and scope. Therefore, it is not intended that the scope of the invention be limited to the specific embodiments described. Rather, it is intended that the scope of the invention be determined by the appended claims and their equivalents. | In some prior art Blowout Preventer (BOP) operating systems, high velocity fluid flows and low differential pressures induced vibration in the system. This vibration may result in collapse and failure of hydraulic hoses in the system. A quick dump valve has been added at or near the open port on the BOP assembly to reduce vibration and other problems. The dump valve has a vent position and an open position. Several alternative embodiments add a ball check valve assembly to the shuttle in the quick dump valve. | 4 |
CROSS REFERENCE TO RELATED APPLICATION
This is a continuation-in-part of application Ser. No. 541,355 filed Jan. 15, 1975, now U.S. Pat. No. 4,000,551.
BACKGROUND OF THE INVENTION
The invention relates to the production of bulky, continuous filament yarn.
United Kingdom Pat. Specification No. 732,929 describes and claims a bulky, continuous filament yarn and a method and apparatus for its manufacture in which a multi-filament flat yarn is subjected to the action of a fluid stream in a zone of sufficient turbulence to separate the individual filaments and to form them into ring-like, crunodal loops and other convolutions. To accommodate the formation of these loops and other convolutions, the yarn is fed into the turbulence zone at a greater speed than it is withdrawn.
Whilst the resultant bulky yarn is suitable for the production of fabrics for some end uses, it does not have sufficient bulk for fabrics of some other end uses. For example boucle type yarns suitable for the production of upholstery fabrics cannot be produced by subjecting a single end of yarn to turbulence. In practice, fabrics produced by subjecting a single yarn end to turbulence are subject to pluckiness and lack of stability.
It has therefore been proposed, in United Kingdom Pat. Specification No. 893,020, to produce core and effect yarns in which a yarn providing the core filaments of the core and effect yarn are fed into a zone of fluid turbulence at a much lower speed than each of the filaments providing the loops and other convolutions necessary in highly bulked fancy yarn. However, although these core and effect yarns are suitable for the production of upholstery fabrics, they are not suitable for knitted or woven apparel fabrics.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a continuous filament yarn having improved bulkiness, stability and covering power hitherto unattainable by known methods of production.
According to the invention, there is provided a method of producing a bulky, continuous filament yarn including the steps of feeding primary and secondary continuous multi-filament yarns comprising, respectively, at least 20% and up to 80% of the total filaments into a treatment zone; providing within the treatment zone a fluid flow of sufficient turbulence to separate the individual filaments of the yarns, to form crunodal, ring-like loops and other convolutions at randomly spaced intervals along the lengths of the individual filaments of each secondary yarn and to cause the indivdual filaments of each secondary yarn to intermingle with each other and with the individual filaments of each primary yarn; wetting one of the yarns prior to feeding it into the treatment zone; and withdrawing the intermingled filaments from the treatment zone and collecting the intermingled filaments in the form of a single yarn; each primary yarn being fed into the treatment zone at a rate between 4 and 26% higher than the rate at which the intermingled filaments are withdrawn from the treatment zone and each secondary yarn being fed into the treatment zone at a rate which is at least 2.5% higher than the rate of feed of each primary yarn and up to 30% higher than the rate at which the intermingled filaments are withdrawn from the turbulent zone.
A preferred embodiment of the invention includes the steps of pre-treating at least one primary continuous multi-filament yarn by the application of an aqueous liquid and feeding primary and secondary continuous multi-filament yarns of polymeric material comprising said pre-treated yarn and at least one secondary yarn so that each yarn to which aqueous liquid has been applied enters the treatment zone while still wet.
Thus, the present invention also provides a method of producing bulky, continuous filament yarn of polymeric material in which at least 20% of the filaments are substantially straight and the remainder of the filaments are formed at randomly spaced longitudinal intervals with crunodal, ring-like loops and other convolutions separated by relatively straight portions and are intermingled with each other and with the substantially straight filaments so that, when a gradually increasing tensile load is imposed on the bulky yarn, all the filaments break simultaneously, the method comprising the steps of pre-treating at least one primary continuous multi-filament yarn of polymeric material by the application of an aqueous liquid; feeding primary and second continuous multi-filament yarns of polymeric material comprising said pre-treated primary yarn and at least one secondary yarn and respectively providing at least 20% and the remainder of up to 80% of the total filaments into a treatment zone within an air nozzle device so that each yarn to which the liquid has been applied enters the treatment zone while still wet; providing within the treatment zone a fluid flow of sufficient turbulence to separate the individual filaments of the yarns, to form crunodal, ring-like loops and other convolutions at randomly spaced intervals along the lengths of the individual filaments of each secondary yarn while the filaments of each primary yarn remain substantially straight and free from crunodal, ring-like loops and to cause the individual filaments of each secondary yarn to intermingle with each other and with the substantially straight individual filaments of each primary yarn; withdrawing the intermingled filaments from the treatment zone and collecting the intermingled filaments in the form of a single bulky yarn, each primary yarn being fed into the treatment zone at a rate between 4 and 26% higher than the rate at which the intermingled filaments of the bulky yarn are withdrawn from the treatment zone and each secondary yarn being fed into the treatment zone at a rate which is at least 2.5% higher than the rate of feed of each primary yarn and up to 30% higher than the rate with which the bulky yarn is withdrawn from the treatment zone.
A sufficiently turbulent fluid flow is provided in the treatment zone by means of a conventional air nozzle provided for this purpose, for example; as described in United Kingdom Patent Specification No. 732,929. In passing into the nozzle, the yarns are blown about and whipped violently so that the individual filaments are first separated and then the filaments of each secondary yarn are swirled into crunodal, ring-like loops and other convolutions which interlock with the other filaments. When the resultant bulky yarn is subjected to a gradually increasing tensile load, this inter-locking ensures that part of the load is borne by the filaments of the or each secondary yarn.
Although it is clear that the pre-treatment of at least one primary yarn with an aqueous liquid results in a bulky yarn in which the primary and secondary yarns are more effectively intermingled, it is not entirely clear how this improvement is brought about. However, it is believed that the liquid has a two-fold effect. Firstly, gas turbulence within the treatment zone forms the liquid into a spray which is more effective than the turbulent gas in forming crunodal loops and other convolutions in the filaments of the or each secondary yarn and, secondly, the liquid acts as a lubricant which facilitates the intermingling of the crunodal loops and other convolutions of the filaments of the or each secondary yarn with the filaments of the or each primary yarn. It has been found that the overall effect of the liquid in providing an improved bulky yarn is increased if the aqueous liquid is applied to at least one primary yarn rather than to at least one secondary yarn.
In the production of this bulky yarn, by a method according to the present invention, the primary and secondary yarns may be passed through at least two separate feeding means which are operable to feed the yarns at different speeds. However, where different yarns are to be fed at the same speed, it is not necessary to provide separate feeding means for each such yarn; they can be passed through the same feeding means. Feeding means, downstream of the treatment zone, may then be provided in order to collect the bulky yarn at a further, lower speed.
As a consequence of the difference in over-feeds which are applied to the constituent yarns, the individual filaments of the bulky yarn are subjected to various degrees of strain during the bulking process. As a result, when the bulky yarn is subjected to shrinkage, as by the application of heat, two phenomena are observed; firstly, the tighter filaments of each primary yarn have a tendency to contract and create greater bulk in the yarn and, secondly, the loops of the filaments of each secondary yarn which appear on the surface of the bulky yarn have a tendency to be pulled back into the main body of the bulky yarn, thereby reducing pickiness or pluckiness of the yarn.
The foregoing unique properties can be used to advantage to obtain still further improvement in bulkiness and reduced pickiness of the bulky yarn. This is achieved by subjecting the bulky yarn to a heat relaxing process, either as a separate operation or, preferably, as a step in the method of producing the bulky yarn.
To achieve maximum shrinkage with a synthetic yarn, it is preferable to use a contact heater or, alternatively, a tube heater which heats the yarn by a combination of both convection and conduction.
The bulky yarn formed from the intermingled filaments is fed on to or through the heater in a relaxed condition to achieve a shrinkage which is equivalent or somewhat in excess of the potential boiling water shrinkage for most synthetic yarns; this shrinkage is approximately 10%.
The yarn is therefore overfed into the heater to achieve a tension low enough to ensure that full shrinkage can take place. Many forms of heater are available, but the preferred type comprises a multi-path contact heater of approximately one meter in length which is totally enclosed to increase its efficiency. The yarn is fed upwards to the top of the heater, around a roller and back through the heater, around a further roller disposed below the heater and then upwards through the heater once again. After several passes around the upper and lower rollers, the yarn is fed up to a take-up package. It is also possible to improve bulking and loop retraction in separate operations subsequent to the preparation of the bulky yarn. With knitwear, this can be done by subjecting garments to high pressure steaming at 130° C.
The heat shrinkage obtained gives improved stability during finishing and, since potential shrinkage has been decreased, fabric formed from the bulky yarn will not have the same tendency to crease during finishing of the fabric. The development of longitudinal creases in fabric is a well-known phenomenon and could cause considerable trouble during normal fabric finishing. The further reduction in pickiness of the yarn also reduces the yarn to yarn friction within the fabric and this will improve the recovery from extension and will reduce the amount of creasing developed in the fabric during normal use.
The intermingled filaments withdrawn from the treatment zone, where they are subjected to turbulent fluid flow, are eventually collected on a wind-up device, for example; a down-twister or cheese-winder and, in order to ensure that the bulky yarn is wound at an appropriate tension, it may be passed through a pair of take-up rolls which, together with the wind-up device, ensure that the bulky yarn is fed to the wind-up device with a suitable under-feed, typically between 5 and 10%.
The method according to the present invention is particularly suitable for the production of bulky yarns from continuous filament yarns of polyester and polyamide. However, continuous filament yarns of other polymeric material can also be used, for example: polyolefin yarns, viscose rayon yarns and cellulose acetate yarns. Variations in texture and bulk may be obtained by using constituent yarns of different materials, by using constituent yarns of different structures and by varying the relative rate of overfeed of the different constituent yarns through the treatment zone.
It has been found that by using different over-feeds for different constituent yarns passed through the treatment zone and limiting the overfeeds to 30%, bulky yarns may be produced at a much higher speed than if all the constituent yarns were fed through the treatment zone at the same speed. This therefore gives rise to greater economies in production and creates yarns which can be produced at speeds more economically than hitherto known.
The relative overfeeds of the constituent yarns will depend on the denier of the final yarn, the denier of the constituent yarns and also on the filament denier of the constituent yarns and should be maintained within 1%. It has been found by experiment, that the relative overfeeds are extremely critical and a change in filament denier or any other characteristic of the constituent yarns requires a modification of the relative overfeeds to produce a yarn which has acceptable bulk and is reasonably free from pluckiness when made into a woven or knitted fabric.
The interlocking of the filaments of the bulky yarn provides greater stability than has hitherto been attainable. This not only improves the pilling properties of fabrics made from the yarn, but improves the efficiency of subsequent processing, particularly where the yarn is used as warp in a woven fabric. The resistance to abrasion brought about by the improved interlocking of the filaments also enables the yarns to be woven without size.
Five bulky, continuous filament yarns, and their methods of manufacture according to the invention, are hereinafter described by way of example, with reference to the accompanying drawings, in which:
DESCRIPTION OF THE DRAWINGS
FIGS. 1 and 2 are schematic side and front elevations of apparatus for performing a method of producing a bulky, continuous filament yarn, according to the invention;
FIG. 3 is an enlarged elevational view of the bulky yarn provided by the method described with reference to FIGS. 1 and 2;
FIGS. 4 to 6 are schematic elevational views of two filaments from each of three multi-filament components of the bulky yarns shown in FIG. 3; and
FIGS. 7 and 8 are schematic side and front elevations of a modified form of the apparatus shown in FIGS. 1 and 2 for producing a bulky, continuous filament yarn from two constituent yarns of polymeric material.
DESCRIPTION OF PREFERRED EMBODIMENTS
As shown in FIGS. 1 and 2, a 167 decitex 72 filament primary yarn 1 of polyester and two secondary yarns 2 and 3 comprising, respectively, a 78 decitex 20 filament yarn of polyhexamethylene adipamide (sold under the trade name nylon) and a 167 decitex 72 filament polyester yarn are fed over axially spaced portions 11, 12 and 13 of a stepped feed roll and held in driving engagement with the feed roll by three pressure rollers 21, 22 and 23 (FIG. 2) to form three separate pairs of feed rolls. The rotational speed of the feed roll and the diameters of the portions 11, 12 and 13 of the feed roll are such that the primary yarn 1 and the two secondary yarns 2 and 3 passing through the three separate pairs of feed rolls are withdrawn from creels (not shown) at rates of 336, 345 and 363 meters per minute. The three yarns 1, 2 and 3 withdrawn from the creels are fed into a treatment zone in a conventional air nozzle device through yarn guides 25, 26 and 27. However, the 167 decitex 72 filament secondary yarn 3 is pre-treated before entering into the nozzle device 24 by being passed through a yarn guide 28 immersed in water 29 in a pan 30 and is fed into the treatment zone along a path which is inclined to the path of the yarn through the treatment zone, whereas the other two yarns 1 and 2 are fed into the treatment zone along a path which is colinearly aligned with the rectilinear path of the yarn and the treatment zone. Inside the air nozzle device 24, the wet yarn 3 and the yarns 1 and 2 pass through the treatment zone where turbulent air flow causes the filaments of the different yarns to intermingle so as to form a single composite bulky yarn 31 which passes between a pair of cylindrical feed rolls 32 having a rotary speed sufficient to withdraw the bulky yarn 31 from the nozzle device 24 at a rate of 300 meters per minute. The yarns 1, 2 and 3 are thus fed into the treatment zone within the nozzle device 24 at rates of 36, 45 and 63 meters per minute higher than the 300 meters per minute the bulky yarn 31 is withdrawn. As a result of these overfeeds of 12, 15and 21%, there is considerable slack in the filaments of the three yarns as they pass through the treatment zone. The filaments of the primary yarn are therefore separated from each other and the filaments of the secondary yarns are blown about and whipped violently in such manner that the individual filaments are first separated and then swirled into crunodal, ring-like loops and other convolutions which interlock the filaments of the two secondary yarns and also interlock these filaments with the filaments of the primary yarn which are separated by the turbulence, but not themselves formed with convolutions.
After formation of the composite, bulky yarn 31, it is fed over a contact heater 33 to a take-up mandrel 34 to effect relaxation of stress induced in the filaments by the turbulence within the treatment zone. As shown in FIGS. 1 and 2, the yarn 31 is trained around rollers 35 and is passed several times around the contact heater 33, which is heated to a temperature of about 220° C, where it is heated by convection and conduction. To accommodate a 10% shrinkage of the yarn 31 during the heat relaxation operation, the yarn 31 is passed over the contact heater 33 with a 15% overfeed so that, although the yarn 31 is fed to the contact heater 33 at a rate 300 meters per minute, it is withdrawn at a rate of 255 meters per minute.
The yarn 31 is then passed from the contact heater 33 to the take-up mandrel 34 with sufficient underfeed to remove the slack in the yarn 31. Thus, with an underfeed of 5.9%, the yarn 31 withdrawn from the contact heater 33 at a rate of 255 meters per minute is wound onto the take-up mandrel 34 at a rate of 270 meters per minute so as to allow for the 10% shrinkage of the yarn 31 fed over the contact heater 33.
The bulky yarn 31 produced by this method has the appearance illustrated in FIG. 3.
As shown in FIG. 4, filaments 1A and 1B representing two of the 72 filaments of the primary yarn are separated from each other so as to permit the insertion of convolutions formed in the filaments of the two secondary yarns, but are not themselves formed with crunodal, ring-like loops. The filaments 2A and 2B shown in FIG. 5 and the filaments 3A and 3B shown in FIG. 6 represent, respectively, two of the 20 filaments and two of the 72 filaments of the two secondary yarns and show the formation of randomly spaced crunodal, ring-like loops 2C formed in the filaments 2A and 2B being separated by longer lengths of substantially straight filament than the loops 3C formed in the filaments 3A and 3B. After formation of the loops shown in FIGS. 5 and 6, these loops interlock the filaments of the two secondary yarns with each other and with the filaments of the primary yarn. Thus, when a gradually increased tensile load is applied to the yarn 31 the loops are prevented from collapsing and so the load is borne by all of the filaments and, on further increase in tensile loading, all of the filaments break substantially simultaneously. The primary yarn 1 provides 72 of the 164 filaments of the bulky yarn 31, that is to say: approximately 44% of the filaments of the bulky yarn.
In a second example of the method of forming bulky yarn, according to the present invention, a 150 denier 48 filament primary yarn of polyester and three secondary yarns respectively comprising two 100 denier 34 filament polyamide yarns and a further 150 denier 48 filament polyester yarn are fed through the apparatus illustrated in FIGS. 1 and 2 so that the yarns are passed through a zone of turbulence by means of the three separate pairs of feed rolls and a single pair of withdrawal rolls so that the primary yarn is given an 8% overfeed, two secondary yarns of polyamide are given an overfeed of 18% and the secondary yarn of polyester is given an overfeed of 24%. Thus, for a withdrawal rate of 300 meters per minute, the primary yarn is fed into the treatment zone at a first rate of 324 meters per minute and the secondary yarns are fed at rates of 354, 354 and 372 meters per minute. The composite yarn resulting from this combination has 164 filaments which are so intermingled as to provide a bulky texture. The 48 filaments (more than 29% of the total) of the primary yarn are relatively free of crunodal, ring-like loops, but the remaining filaments are formed with crunodal, ring-like loops and other convolutions and are interlocked with each other and with the 48 filaments of the primary yarn.
In the apparatus shown in FIGS. 7 and 8, a 167 decitex 68 filament primary yarn 1 of polyester and a 167 decitex 68 filament secondary yarn 2 of polyester are fed over axially spaced portions 11 and 12 of a stepped feed roll and held in driving engagement with the feed roll by two pressure rollers 21 and 22 (FIG. 8) which, together with the stepped feed roll, form two separate pairs of feed rolls. The rotational speed of the stepped feed roll and the diameters of the portions 11 and 12 of the feed roll are such that the primary yarn 1 and the secondary yarn 2 passing through the two separate pairs of feed rolls are withdrawn from creels (not shown) at rates of 547 and 582 meters per minute. The two yarns 1 and 2 withdrawn from the creels are fed to the conventional air nozzle device 24 through yarn guides 25, 26 and 27. However, the 167 decitex 68 filament primary yarn 1 is pre-treated before entering into the nozzle device 24 by being passed through a yarn guide 28 immersed in water 29 in a pan 30. The wet primary yarn 1 and the secondary yarn 2 then pass axially through the air nozzle device 24 along a rectilinear path through the treatment zone (not shown) inside the nozzle device 24 in which a turbulent air flow causes the filaments of the different yarns to intermingle so as to form a single bulky yarn 31 which passes between a pair of cylindrical feed rolls 32 having a rotary speed sufficient to withdraw the bulky yarn 31 from the nozzle device 24 at a rate of 461 meters per minute. The yarns 1 and 2 are thus fed into the treatment zone within the nozzle device 24 at rates of 86 and 121 meters per minute higher than the 461 meters per minute the bulky yarn 31 is withdrawn. As a result of these overfeeds of 18.7% and 26.2% there is considerable slack in the filaments of the two yarns as they pass through the treatment zone. The filaments of the primary yarn are therefore separated from each other and the filaments of the secondary yarns are blown about and whipped violently in such manner that the individual filaments are first separated and then swirled into crunodal, ring-like loops and other convolutions which interlock the filaments of the secondary yarn and also interlock these filaments with the filaments of the primary yarn which are separated by the turbulence, but not themselves formed with convolutions.
The bulky yarn is then wound into a package on a take-up mandrel 34 at the rate of 500 meters per second.
With a method such as this the input titre of the constituent yarns is 334 decitex and the final titre of the bulky yarn is 378 decitex. Although not shown, it is also possible to subject the composite bulky yarn issuing from the air nozzle device 24 to heat treatment as described with reference to the apparatus illustrated in FIGS. 1 and 2.
The bulky yarn 31 produced by this method has an appearance which is similar to that schematically illustrated in FIG. 3.
As shown in FIG. 4, filaments 1A and 1B representing two of the 68 filaments of the primary yarn 1 are separated from each other so as to permit the insertion of convolutions formed in the filaments of the secondary yarn 2, but are not themselves formed with crunodal, ring-like loops. The filaments 2A shown in FIG. 5 represent two of the 68 filaments of the secondary yarn 2 and show the formation of randomly spaced crunodal, ring-like loops 2C along the lengths of the filaments. After formation of the loops shown in FIG. 5, these loops interlock the filaments of the secondary yarn 2 with each other and with the filaments of the primary yarn 1. Thus, when a gradually increased tensile load is applied to the resultant bulky yarn 31, the loops are prevented from collapsing and so the load is borne by all of the filaments and, on further increase in tensile loading, all of the filaments break substantially simultaneously. The primary yarn 1 and the secondary yarn 2 both provide 68 of the 136 filaments of the bulky yarn 31, that is to say 50 % of the filaments of the bulky yarn.
In a fourth example of the method of forming bulky yarn, according to the present invention, by means of the apparatus illustrated in FIGS. 7 and 8, an additional 78 decitex 20 filament primary yarn of nylon is fed through the apparatus illustrated in FIGS. 7 and 8 so that the two primary yarns are given an 15.4% overfeed and the secondary yarn of polyester is given an overfeed of 20.6%. Thus, for a withdrawal rate of 460 meters per minute, the primary yarns are fed into the treatment zone at a rate of 531 meters per minute and the secondary yarn is fed at a rate of 555 meters per minute. The bulky yarn resulting from this combination has 156 filaments which are so intermingled as to provide a bulky texture. The 88 filaments (more than 56% of the total) of the primary yarns are relatively free of crunodal, ring-like loops, but the remaining filaments are formed with crunodal, ring-like loops and other convolutions and are interlocked with each other and with the 88 filaments of the primary yarns.
After withdrawing the bulky yarn from the treatment zone at a rate of 460 meters per minute, it is then wound into a package on the take-up mandrel at a rate of 485 meters per minute. The titre of the constitutent yarns is thus increased from 412 decitex to 461 decitex.
In a fifth example of the method of forming bulky yarn, according to the present invention, two 78 decitex 34 filament primary yarns of nylon are fed through the apparatus illustrated in FIGS. 7 and 8 together with two secondary yarns respectively comprising a 220 decitex 52 filament triacetate yarn and a 78 decitex 34 filament nylon yarn. In this case the feed rates of the primary and secondary yarns and the package take-up rate are the same as in the third example and the titre of the constituent yarns is increased from 454 to 518 decitex.
In each of the third, fourth and fifth examples, only one primary yarn is subjected to pre-treatment with water. However, in each case, it is also possible to pre-treat at least one secondary yarn. Similarly, in the fourth and fifth examples, it is possible to pre-treat more than one primary yarn with water. | A method of producing a bulky continuous filament yarn which includes the steps of feeding primary and secondary continuous multi-filament polymeric yarns into a treatment zone within an air nozzle device, with one of the yarns being pre-treated by the application of water so that said one yarn is wet when fed into the treatment zone. The yarns in the treatment zone are subjected to a turbulent fluid flow which causes the individual filaments of the yarns to separate, and also causes ring-like loops to be formed at randomly spaced intervals along the individual filaments of the secondary yarn. The filaments of the yarns become intermingled within the treatment zone and are withdrawn and collected in the form of a single yarn. The primary yarn is fed into the treatment zone at a rate between 4 and 26% greater than the rate at which the intermingled filaments are withdrawn from the treatment zone, and the secondary yarn is fed into the treatment zone at a rate which is at least 2.5% greater than the rate of feed of the primary yarn and up to 30% greater than the rate at which the intermingled fibres are withdrawn from the treatment zone. | 3 |
This application claims the benefit of provisional application 60/054,794 filed Aug. 5, 1997.
BACKGROUND OF THE INVENTION
This invention relates to an emergency exit system and in particular to an emergency exit system for use on a helicopter or other aircraft.
Vehicle accidents occurring in water have a lower survival rate than accidents occurring on land. In water accidents, the vehicles usually sink very rapidly, either in an upright or inverted position. Underwater conditions are drastically different from land based conditions. Visibility is reduced—the majority of people can see only 1.5 meters underwater and 3.1 meters in the best lit conditions. Survivors of a crash or forced landing must depend on their breath-holding ability to make a successful escape. Generally, a person's breath-holding ability is reduced 25-50% in water under 15° C. Maximum breath-holding time can be as short as 10 seconds. Survivors are often disoriented due to the sudden immersion in water, loss of gravitational references, poor depth perception, nasal inhalation of water and darkness. Disorientation is magnified when the vehicle is inverted. Under the latter condition, finding a handle to jettison an escape door or window, which is a simple procedure to execute in an upright position on dry land, can be a most challenging task even if the handle is only a few centimeters away from the survivor's hand.
Usually handles for open escape doors or windows are small, and are positioned between knee and chest level. The various positions would not be obvious to the survivor unless he or she is familiar with the particular escape system Most existing mechanisms are adapted to remove an entire door or window, including the frame, requiring a complicated jettison mechanism, which is not always dependable. Moreover, existing systems do not provide feedback to indicate that the door, window or hatch as been successfully jettisoned.
GB-A-761 627 and U.S. Pat. No. 3,851,845 disclose systems for the jettisoning of aircraft canopies or doors which are inappropriate for use in a door or window release. The U.S. reference teaches the use of lever or a lever and a handle combination for releasing a door. When submerged in water such a system could be difficult to operate, particularly when it is necessary to operate a handle and a separate lever to effect release of the door.
BRIEF SUMMARY OF THE INVENTION
The object of the present invention is to provide an emergency exit system of the type which includes a plurality of actuators adapted'to operate independently of one another to effect release of a window or door panel to provide an escape exit.
Accordingly, the present invention relates to an emergency exit system including a frame for mounting in a vehicle, said frame having an opening for closing by a panel, a plurality of spaced apart latch means for releasably latching said panel in the frame; release means for simultaneously releasing all of said latch means; and principal actuation means located at a plurality of locations around the periphery of said frame for actuating said release means when any of said actuation means is actuated, characterised by cable means forming part of said release means and extending around a substantial portion of said frame to interconnect the release means associated with each said latch means.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is described below in greater detail with reference to the accompanying drawings, which illustrate preferred embodiments of the invention, and wherein:
FIG. 1 is a perspective view of a window emergency exit system in accordance with the invention;
FIGS. 2 and 3 are front elevation views of the interior of the exit system of FIG. 1 with parts removed and showing the plungers in the panel latching and panel release positions, respectively;
FIG. 4 is a isometric view of portions of actuation and release mechanisms used in the exit system of FIG. 1;
FIG. 5 is a schematic, partly a sectioned view taken along line 5 — 5 of FIG. 1;
FIG. 6 is an elevation view of the interior of the exit system of FIG. 1 with parts removed;
FIG. 7 is a front elevation view of the interior of a door emergency exit system;
FIG. 8 is a front elevation view of the door exit system of FIG. 7 with parts removed;
FIG. 9 is a schematic, cross section taken generally along line, 9 — 9 of FIG. 7;
FIG. 10A is a front view of a hinge assembly used in the exit system of FIG. 7; and
FIG. 10B is a front view of a plate and a section of cable for releasably retaining the hinge assembly of FIG. 1
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIGS. 1 to 3 , one embodiment of the emergency exit system, which is generally indicated at 2 , is a window for mounting in the fuselage of an aircraft such as a helicopter (not shown). However, the system may also be a door, a hatch or any other type of exit adapted for mounting in a closed body such as the body of a vehicle, e.g. a car, bus or truck, the fuselage of an airplane or a wall of a building.
Generally, the emergency exit system 2 includes a rectangular frame 4 defining a central opening 6 , a closure panel 8 such as a metal sheet or window releaseably secured in the opening 6 by a plurality of latches 10 extending from the frame 4 ; a release mechanism 12 (FIGS. 2 and 3) in the frame 4 and an actuation mechanism on the inner side of the frame 4 including four bars 14 (FIG. 1 ), which are independently operable to simultaneously effect the release of all of the latches 10 to enable jettisoning of the closure panel 8 to provide an emergency exit.
The frame 4 includes interconnected exterior and interior panels 16 and 18 , respectively. The interior panel 18 is sufficiently thick to contain the actuation mechanism 12 (FIG. 2 or 3 ). Four closed compartments 20 extend from the corners of the inner panel 18 for receiving the bars 14 therebetween. The compartments 20 contain parts of the release mechanism 12 and an emergency lighting assembly 21 (FIG. 6 ), both of which are described in detail below.
In contrast to prior art emergency exit systems, the exit system 2 of the present invention includes a plurality of actuation bars 14 . The bars 14 are mounted in obvious locations, i.e. they extend along the interior of the sides 22 and the top and bottom ends 23 and 24 , respectively of the frame 4 , so that they can be easily located and accessed, thus significantly improving the chances of escape and survival of trapped survivors. Each bar 14 includes an elongated cylindrical body 25 with a press fitted lever 26 at one end thereof. The bars 14 are individually connected to the release mechanism 12 in such a manner as to be independently operable. Actuation of any one of the bars 14 will simultaneously disengage all of the latches 10 to release the panel 8 from the frame 4 . This minimizes the number of operations and amount of energy required by the survivor to release the panel 8 . All of the energy of the operator will be applied to the release of the panel 8 rather than for actuation of the remaining bars 14 . Moreover, if one bar 14 malfunctions, another may be used to serve the same function. The panel 8 is jettisoned by pulling any one of the bars 14 towards the operator and away from the frame 4 .
The bars 14 are rotatably mounted relative to the compartments 20 between first and second limit positions. In the first limit position, the panel 8 is secured in the opening 6 . In the second limit position, the panel 8 is released from the frame 4 .
Each release mechanism 12 is connected to one end of each bar 14 . Referring to FIGS. 2 to 4 , rotation of one bar 14 is transmitted to its associated release mechanism 12 and then to the plurality of latches 10 to simultaneously retract each latch 10 inwardly into the frame 4 to release the panel 8 . The release mechanism 12 is switchable between a locked or latched position (FIG. 2) in which the latches 10 extend inwardly from the frame 4 and a release position (FIG. 3) in which the latches 10 are retracted into the frame 4 .
Each release mechanism 12 is designed to translate rotational movement of the bar 14 and a lever 26 at one end of the bar into movement necessary to disengage the latches 10 . Referring to FIG. 4, each release mechanism 12 includes a helical gear or rack 28 mounted on a shaft 29 near one end thereof. The gear 28 is connected by a gear or pinion 30 and a shaft 31 to a lever 26 . Rotation of the lever 26 around the longitudinal axis of the shaft 31 results in a corresponding rotation of the shafts 29 and 31 . The shaft 29 is rotatably mounted in ball bearings (not shown) in arms 33 and 34 of a generally C-shaped bracket 35 . The shaft 31 is also mounted in the bracket 35 perpendicular to the shaft 29 . It will be appreciated that the bracket 35 and the shafts 29 and 31 are housed in the compartments 20 . The end of the shaft 29 extending through the arm 34 of the bracket 35 extends through an opening in the frame 4 and carries a pinion 40 . The pinion 40 meshes with a rack 42 for imparting longitudinal movement thereto when the pinion is rotated. The pinion 40 is retained on the shaft 29 by a key (not shown) and a nut 44 .
A cable 45 extends through and is freely slidable in the rack 42 . The cable 45 extends around idler pulleys 47 located at the corners of the frame 4 . A conventional cable tensioner 48 (FIGS. 2 and 3) maintains the cable 45 under the desired tension. A stop 50 is fixedly mounted on the cable 45 for engaging one end of the rack 42 . When the rack 42 is moved in one direction (indicated by arrows A in FIG. 2 ), it pushes against the stop 50 to move the cable 45 in the same direction. Movement of the cable 45 causes rotation of a second lever 54 (FIG. 4) mounted in the frame for operating a latch 10 . The lever 54 includes a tapering body 56 with a generally U-shaped notch 57 in an outer end thereof for receiving a pin 59 attached to the cable 45 . Thus, movement of the cable 45 will cause rotation of the lever 54 , the inner end 60 of which is rotatably mounted in the frame 4 . Such inner end 60 of the lever 54 includes teeth defining a pinion for engaging a rack 62 slidably mounted in the frame 4 . The rack 62 forms part of the latch 10 . A pin 63 with a tapered outer end extends outwardly from the rack 62 for retaining the panel 8 in the frame 4 . When the pin 63 is retracted, the panel 8 is released for jettisoning.
It is readily apparent that rotation of one lever 26 will cause movement of the cable 45 , and consequently simultaneous release of all of the latches 10 . Movement of the lever 26 and the cable 45 in the opposite direction will result in extension of the pin 63 to the latched or locking position (FIG. 4 ). In the locked position the pins 63 engage grooves or indentations 65 (FIG. 2) in the panel 8 . From FIGS. 2 and 3, it will be noted that a rack 42 and pinion 40 arrangement is associated with each bar 14 , so that rotation of any bar 14 results in the release of all of the latches 10 .
Once the latches 10 have been release, the bars 14 are locked in the release position by a locking mechanism generally indicated at 68 in FIG. 5 . Each locking mechanism 68 includes a lever 69 (FIGS. 1 and 5) mounted on the end of each bar 14 opposite to the end carrying the lever 26 . The lever 69 is mounted on one end of a shaft 70 , which is rotatably mounted in one end 71 of the compartment 20 and in an L-shaped bracket 73 . An arm 74 is mounted on the inner end 75 of the shaft 70 for rotation therewith. The arm 74 is guided between the panel latched and release positions by a pin 77 extending inwardly from the bracket 73 into an arcuate slot 78 in the arm. The arm 74 and consequently the lever 69 are releasably retained in the panel latched position by a detent pin 80 , which extends into a shallow conical depression 81 in the bracket 73 . The pin 80 extends outwardly from a cylindrical barrel 81 mounted in the end of the arm 74 opposite to the end 75 receiving the shaft 70 . A helical spring 83 bears against the head 84 of the pin 80 for biasing the outer end thereof into the depression 81 . When the bar 14 is rotated from the panel latching position (shown in solid lines in FIG. 5) to the panel release position (shown in phantom outline in FIG. 5) the arm 74 is also rotated. The pin 80 escapes from the depression 81 and is rotated with the arm 74 to the panel release position in which the pin 80 encounters a hole 86 extending through the bracket 73 and the end 71 of the compartment 20 . Thus, the arm 74 and consequently the lever 69 and the bar 14 are locked in the panel release position.
Referring to FIGS. 2 and 3, a plurality of ejectors 88 are provided on the interior of the frame 4 . The ejectors 88 are spring loaded plungers for biasing the panel 8 outwardly from the frame 4 . Immediately following release of the panel 8 by the latches 10 , the ejectors 88 push the panel 8 outwardly to clear the opening 6 .
In operation, one or more bars of the actuation mechanism is pulled towards the operator and away from the limit positions defined by the detent pin 80 , the depression 81 and the hole 86 . Rotation of a bar 14 causes pivoting of a lever 26 on one end of the bar 14 , and consequently rotation of the shafts 31 and 29 , and the pinion 40 . Rotation of the pinion 40 results in movement of the rack 42 and the cable 45 which translates into rotation of all of the levers 54 to release the latches 10 . The panel 8 is thus free to move and is pushed out of the frame 4 by the ejectors 88 .
An auxiliary actuator generally indicated at 89 (FIGS. 2 and 3) for the panel 8 includes a pulley 90 rotatably mounted in one corner of the frame 4 . A notch in the pulley 90 engages a pin 91 , which is attached to the cable 45 . The auxiliary actuator can override the release mechanism 12 . The pulley 90 is rotated by either of two levers defined by handles 94 (one shown—FIG. 1) mounted on the ends of a shaft carrying the pulley. The handles 94 are located on the interior and exterior lower corners of the frame 4 (i.e. inside and outside the window). Rotation of either handle 94 results in simultaneous release of all latches 10 .
With reference to FIG. 1, a preferred form of panel 8 includes a sash 96 carrying a panel, which is sealed in the sash 96 by a rubber molding 98 . The panel 8 can be removed from the sash 96 by removing the molding 98 .
Once removed, the panel 8 can be re-installed in the opening 6 by pushing the panel as far as possible into the opening to compress the plungers of the ejectors 88 . The detent pins 80 are pushed out of the holes 86 , and the bars 14 are rotated to return the pins 80 to the latched position in the recesses 81 . The panel 8 is secured in the opening 6 by rotating either one of the handles 94 to return the latches 10 to locked position.
Referring to FIG. 6, the emergency lighting assembly 21 is used to illuminate the opening 6 and to provide an indication where the exit system is located and whether the panel 8 is latched or released. When the lighting is constant, the panel 8 is in the latched condition, and strobe lighting indicates that the panel 8 has been released. The lighting system 21 includes a plurality of high intensity light emitting diodes (LEDS) 100 in the bars 14 and on the auxiliary release 89 , a strobe switch 102 on the frame 4 to indicate when the panel 8 has been jettisoned, light actuation elements (not shown) and a power pack 103 external to the frame 4 . The power pack 103 is connected to the remainder of the lighting system by a cable 105 . The power pack 103 includes a microprocessor (not shown) for controlling the lighting system.
The light actuation elements include an immersion sensor, an impact sensor, a roll over sensor and a pilot operated on-off switch (none of which are shown). The sensors are mounted on the aircraft fuselage or incorporated in the power pack 103 . The immersion sensor is triggered when the aircraft is submerged in water, the impact sensor is triggered when a predetermined impact force has been exceeded, and the roll over sensor is triggered when the aircraft rolls over. The pilot switch is mounted on the console of the aircraft, permitting manual activation of the lighting system. All of the sensors and the switch are wired in parallel so that any one of them can be used to activate the emergency lighting system.
When the lighting system is activated, the LEDs 100 will be simultaneously activated to illuminate the release bars 14 and the handles 94 . The bars 14 and the handles 94 will remain illuminated until the system is deactivated, or until the panel 8 is released and jettisoned. The strobe mode is activated by one of the spring loaded ejectors 88 which closes the strobe switch 102 . Strobe lighting will continue as long as the panel 8 is free of the frame 4 .
A second embodiment of the emergency exit system for use in a door is illustrated in FIGS. 7 to 10 . The second embodiment of the system includes a frame 4 with an opening 6 therein which is closed by a panel 8 (in this case defining a door). The panel 8 includes a window 110 , and flanges 111 extending along the periphery thereof for sealing against the fuselage 112 (FIG. 9) of a helicopter in the closed position.
The panel 8 is mounted in the frame 4 by means of hinges 113 , which permit rotation of the panel 8 between the open and closed positions. The panel 8 is normally opened and closed using a handle 114 and latch pins 115 (FIG. 7 ), all of which are connected to the handle 14 . An actuating mechanism similar to the same mechanism in FIGS. 1 to 4 includes a plurality of independently operated bars 14 for initiating release of the door panel 8 . The bars 14 are connected to a release mechanism generally indicated at 12 (FIG. 8) housed in compartments 116 in the manner described above in connection with FIGS. 1 to 4 . In the embodiment of the invention, movement of one of the bars 14 to the release position causes actuation of the release mechanism, which includes the latches 117 . The release mechanism also releases the hinges 113 to release the panel 8 completely from the frame 4 . The latches 117 are interconnected by a cable 118 (FIG. 8 ), which extends around pulleys 119 at the bottom corners of the frame 4 and returns around the top end thereof, i.e. the cable 118 extends in two rows around the top and sides of the frame 4 . Grooved rollers 122 are provided in the frame 4 for guiding the cable 118 around the frame.
Each latch 117 is pivotally mounted on the frame 4 to secure the panel 8 in the opening 6 . An associated plunger 115 is mounted in the panel 8 adjacent the latch 117 to permit latching and unlatching of the door panel 8 during normal operation. More specifically, during normal operation, the door panel is latched by rotating the handle 114 (counterclockwise as shown in FIG. 7) to cause the plunger 115 to extend outwardly from the side of the panel into engagement with the latches 117 . Rollers 122 on the outer ends of the plunger 115 engage the inner sides of the latches 117 (FIGS. 7 and 9. By rotating the handle 114 in the opposite direction, the plungers 115 are retracted into the panel 8 to unlatch the panel permitting swinging of the door panel on the hinges 113 to the open position (FIG. 8 ).
As best shown in FIG. 8 each latch 117 includes an arm 123 connected to a pinion 124 (FIG. 8) rotatably mounted in the frame 4 . The pinion 124 meshes with a rack 125 mounted on the cable 118 . The rack 125 is engaged by a stop 127 (similar to the stops 50 ). When the cable 118 moves, the stop 127 moves the rack 125 to rotate the pinion 124 which in turn causes pivoting of the tab 123 through 45 to release the latch 115 .
Referring to FIGS. 10A and 10B, each hinge assembly 113 includes an arm 130 with holes therein for receiving bolts 131 . A narrow end 133 of the arm 130 is rotatable mounted on a pin defined by a bolt 134 in a clevis 136 . The bolt 134 is retained in the clevis 136 by nut 137 . The body 139 of the clevis 136 tapers to an annular groove 140 and a head 141 . The head 141 is inserted into the large end 143 of a keyhole slot 144 in a plate 145 mounted on the cable 120 . By moving the head 141 into the narrow end 146 of the slot 144 , the clevis 136 and the plate 130 are retained in engagement with the cable 120 . When the cable 120 moves (upwardly in FIG. 10 B), the clevis 136 and consequently the entire hinge is release. At the same time, the arms 123 of the latches 117 rotate 45 to release the plungers 115 , whereby the entire door panel 8 is released for jettisoning.
The second embodiment of the invention also includes an auxiliary release mechanism 89 similar to the same mechanism in the first embodiment of the invention. | An emergency exit system for use on a helicopter or other aircraft includes a frame ( 4 ) defining an opening ( 6 ) for receiving a panel ( 8 ) to close the opening ( 6 ); a plurality of latches ( 10, 117 ) for releasably securing the panel ( 8 ) in the opening ( 6 ); a plurality of release mechanisms ( 12 ); a cable ( 45, 118 ) extending around at least a major portion of the frame ( 4 ) for releasing the panel ( 8 ); and a plurality of actuators ( 14 ) strategically located around the opening and connected to the cable ( 45, 118 ), whereby actuation of any one of the actuators ( 14 ) causes simultaneous release of all of the latches ( 10, 117 ) so that the panel ( 8 ) can be jettisoned. | 4 |
CITATION TO PRIOR APPLICATION
This is a continuation-in-part with respect to U.S. patent application Ser. No. 10/037,754 filed Oct. 22, 2001 now U.S. Pat. No. 6,681,859.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to systems and methods for producing or delivering heat at or near the down hole end of production tubing of a producing oil or gas well for improving production therefrom.
2. Background Information
Free-flowing oil is increasingly difficult to find, even in oil wells that once had very good flow. In some cases, good flowing wells simply “clog up” with paraffin. In other cases, the oil itself in a given formation is of a viscosity that it simply will not flow (or will flow very slowly) under naturally ambient temperatures.
Because the viscosity of oil and paraffin have an inverse relationship to their temperatures, the solution to non-flowing or slow flowing oil wells would seem fairly straight forward—somehow heat and oil and/or paraffin. However, effectively achieving this objective has proven elusive for many years.
In the context of gas wells, another phenomena—the buildup of iron oxides and other residues that can obstruct the free flow of gas through the perforations, through the tubing, or both—creates a need for effective down hole heating.
Down hole heating systems or components for oil and gas wells are known (hereafter, for the sake of brevity, most wells will simply be referred to as “oil wells” with the understanding that certain applications will apply equally well to gas wells). In addition, certain treatments (including “hot oil treatments”) for unclogging no-flow or slow-flow oil wells have long been in use. For a variety of reasons, the existing technologies are very much lacking in efficacy and/or long-term reliability.
The present invention addresses two primary shortcomings that the inventor has found in conventional approaches to heating oil and paraffin down hole: (1) the heat is not properly focused where it needs to be; and (2) existing down hole heaters fail for lack of design elements which would protect electrical components from chemical or physical attack while in position.
The present inventor has discovered that existing down hole heaters inevitably fail because their designers do not take into consideration the intense pressures to which the units will be exposed when installed. Such pressure will force liquids (including highly conducive salt water) past the casings of conventional heating units and cause electrical shorts and corrosion. Designers with whom the present inventor has discussed heater failures have uniformly failed to recognize the root cause of the problem—lack of adequate protection for the heating elements and their electrical connections. The down hole heating unit of the present invention addresses this shortcoming of conventional heating units.
Research into the present design also reveals that designers of existing heaters and installations have overlooked crucial features of any effective down hole heater system: (1) it must focus heat in such a way that the production zone of the formation itself is heated; and (2) heat (and with it, effectiveness) must not be lost for failure to insulate heating elements from up hole components which will “draw” heat away from the crucial zones by conduction.
However subtle the distinctions between the present design and those of the prior art might at first appear, actual field applications of the present down hole heating system have yielded oil well flow rate increases which are multiples of those realized through use of presently available down hole heating systems. The monetary motivations for solving slow-flow or no-flow oil well conditions are such that, if modifying existing heating units to achieve the present design were obvious, producers would not have spent millions of dollars on ineffective down hole treatments and heating systems (which they have done), nor lost millions of dollars in production for lack of the solutions to long-felt problems that the present invention provides (which they have also done)
SUMMARY OF THE INVENTION
It is an object of the present invention to provide an improved down hole heating system for use in conditioning oil and gas wells for increased flow, when such flow is impeded because of viscosity and/or paraffin blockage conditions.
It is another object of the present invention to provide an improved design for down hole heating systems which has the effect of more effectively focusing heat where it is most efficacious in improving oil or gas flow in circumstances when such flow is impeded because of oil viscosity and/or paraffin blockage conditions.
It is another object of the present invention to provide an improved design for down hole heating systems for oil and gas wells which design renders the heating unit useful for extended periods of time without interruption for costly repairs because of damage or electrical shorting caused by unit invasion by down hole fluids.
It is another object of the present invention to provide an improved method for down hole heating of oil and gas wells for increasing flow, when such flow is impeded because of viscosity and/or paraffin blockage conditions.
In satisfaction of these and related objects, the present invention provides a down hole heating system for use with oil and gas wells which exhibit less than optimally achievable flow rates because of high oil viscosity and/or blockage by paraffin (or similar meltable petroleum byproducts). The system of the present invention, and the method of use thereof, provides two primary benefits: (1) the involved heating unit is designed to overcome an unrecognized problem which leads to frequent failure of prior art heating units—unit invasion by down hole heating units with resulting physical damage and/or electrical shortages; and (2) the system is designed to focus and contain heat in the production zone to promote flow to, and not just within, the production tubing.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an elevational view of a producing oil well with the components of the present down hole heating system installed.
FIG. 2 is an elevational, sagittal cross section view of the heating unit connector of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1 , the complete down hole heating system of the present invention is generally identified by the reference numeral 10 . System 10 includes production tubing 12 (the length of which depends, of course, on the depth of the well), a heat insulating packer 14 , perforated tubing 16 , a stainless steel tubing collar 18 , and a heating unit 20 .
Heat insulating packer 14 and stainless steel collars 18 are included in their stated form for “containing” the heat from heating unit 20 within the desired zone to the greatest practical degree. Were it not for these components, the heat from heating unit 20 would (like the heat from conventional down hole heater units) convect and conduct upward in the well bore and through the production tubing, thereby essentially directing much of the heat away from the area which it is most needed—the production zone.
Perhaps, it goes without saying that oil that never reaches the pump will never be produced. However, this truism seems to have escaped designers of previous down-hole heating schemes, the use of which essentially heats oil only as it enters the production tubing, without effectively heating it so that it will reach the production tubing in the first place. largely containing the heat below the level of the junction between the production tubing 12 and the perforated tubing 16 , as is achieved through the current design, has the effect of focusing the heat on the production formation itself. This, in turn, heats oil and paraffin in situ and allows it to flow to the well bore for pumping, thus “producing firs the viscous materials which are impeding flow,” and then the desired product of the well (oil or gas). Stainless steel is chosen as the material for the juncture collars at and below the joinder of production tubing 12 and perforate tubing 16 because of its limited heat conductive properties.
Physical and chemical attack of the electrical connections between the power leads and the heater rods of conventional heating systems, as well as shorting of electrical circuits because of invasion of heater units by conductive fluids is another problem of the present art to which the present invention is addressed.
The patent application which serves as a priority basis for the present invention discloses an embodiment that tremendously increases down hole wiring connection integrity. However, referring to FIG. 2 , the present invention is even better at preventing the aforementioned electrical problems. In fact, the unique combination of the materials, particularly ceramic cement, a highly durable insulation means, and the use of connector pins, provides protection against shortage and other connection damage not previously possible. Such an improvement is of great significance as the internal connection for a down hole heating unit must be impenetrably shielded from the pressures and hostile chemical agents that surround the unit in the well bore.
Referring in combination to FIGS. 1 and 2 , heating unit 20 includes heating unit connector 30 . Heating unit connector 30 is responsible for ensuring the integrity of the connection between surface wiring leads 24 and heater rod wiring leads 25 . The electrical current for heater rod 26 is supplied by cables 22 , which run down the exterior of production tubing 12 and connect to surface wiring leads 24 at the upper end of heating unit 20 .
As shown in FIG. 2 , heating unit connector 30 is comprised of two substantially identical pieces. The upper piece, generally referred to by numeral 32 , houses surface wiring leads 24 . The lower piece, generally referred to by numeral 34 , houses heater wiring 26 .
Heater unit connector 30 also contains two connector pins (male and female), where each connector pin has a distal and a medial end. The union between male connector pin 40 and female connector pin 42 takes place at the medial end of each connector piece, or at the center-most portion of heater unit connector 30 . Male connector pin 40 , at its distal end, has a female receptacle that receives a male connection from heater wiring leads 25 . At its medial end, male connector pin 40 has a male extension that is plugged into the medial end of female connector pin 42 .
Female connector pin 42 contains female receptacles at both its medial and distal end. At its distal end, female connector pin 42 receives a male connection from surface wiring leads 24 . At its medial end, female connector pin 42 receives male connector pin 40 . Importantly, the improvements provided by the present invention do not depend on any specific connector pin configuration. In fact, as will become apparent to those skilled in the art, different connector pin configurations or different connector pin types may work equally as well.
Connector pieces 32 and 34 each contain, in their distal portion, a high temperature ceramic cement filled region, generally designated by numeral 36 . The ceramic cement of region 36 serves to enclose the junction between each connector pin and the respective wiring of each piece. In the preferred embodiment, the high temperature ceramic cement is an epoxy material which is available as Sauereisen Cement #1, which may be obtained from the Industrial Engineering and Equipment Company (“Indeeco”) of St. Louis, Mo., USA.) However, as will become apparent to those skilled in the art, other materials may serve to perform the desired function.
Upon drying, the high temperature ceramic cement of region 36 becomes an essentially glass-like substance. Shrinkage is associated with the cement as it dries. As such, in the preferred embodiment, each heater unit connector piece contains a pipe plug 38 . Pipe plug 38 provides an access point through which additional ceramic cement can be injected into each piece, thereby filling any void which develops as the ceramic cement dries. Further, pipe plug 38 may be reversibly sealed to each piece so that epoxy can be injected as needed while the strength of the seal is maintained.
Connector pieces 32 and 34 further contain, in the medial portion, an insulator block region, generally designated by numeral 39 . Insulator region 39 houses each connector pin so that the union between male connector pin 40 and female connector pin 42 is suitably insulated from any outside chemical or electrical agent.
In order to withstand the corrosive chemicals and enormous external pressure, the outer surface of heater unit connector 30 must be incredibly strong. The aforementioned elements of connector 30 are encased in a steel fitting assembly 50 (“encasement means”), each component of which is welded with continuous beads, using the “TEG” welding process, to each adjoining component. In the preferred embodiment, the outer surface of connector 30 is comprised of stainless steel, which is joined using the process of “TEG” welding. This welding process allows the seams of joined components to withstand the extreme conditions of the bore well.
Finally, each connector piece is secured to the other by fitting assembly 60 . Fitting assembly 60 and sealing fitting 62 are, as would be apparent to anyone skilled in the art, designed to engage one another so as to form a sealed junction. In the preferred embodiment, this union is a standard two inch union that is modified by “TEG” welding. That is, the union is welded using the TEG process so that it will withstand the extreme environmental conditions of the bore well.
The shielding of the electrical connections between surface wiring leads 24 and heater wiring leads 25 is crucial for long-term operation of a down hole heating system of the present invention. Equally important is that power is reliably delivered to that connection. Therefore, solid copper leads with KAPTON insulation are used, such leads being of a suitable gauge for carrying the intended 16.5 Kilowatt, 480 volt current for the present system with its 0.475 inch diameter INCOLOY heater rods 26 (also available from Indeeco).
The present invention includes the method for use of the above-described system for heat treating an oil or gas well for improving well flow. the method would be one which included use of a down hole heating unit with suitably shielded electrical connections substantially as described, along with installation of the heat-retaining elements also as described to properly focus heat on the producing formation.
In addition to the foregoing, it should be understood that the present method may also be utilized by substituting cable (“wire line”) for the down hole pipe for supporting the heating unit 20 while pipe is pulled from the well bore. In other words, one can heat-treat a well using the presently disclosed apparatuses and their equivalents before re-inserting pipe, such as during other well treatments or maintenance during which pipe is pulled. It is believed that this approach would be particularly beneficial in treating deep gas wells with iron sulfide occlusion problems.
Although the invention has been described with reference to specific embodiments, this description is not meant to be construed in a limited sense. Various modifications of the disclosed embodiments, as well as alternative embodiments of the inventions will become apparent to persons skilled in the art upon reference to the description of the invention. It is, therefore, contemplated that the appended claims will cover such modifications that fall within the scope of the invention. | A down hole heating system for use with oil and gas wells which exhibit less than optimally achievable flow rates because of high oil viscosity and/or blockage by paraffin (or similar meltable petroleum byproducts). The heating unit the present invention includes shielding to prevent physical damage and shortages to electrical connections within the heating unit while down hole (a previously unrecognized source of system failures in prior art systems). The over-all heating system also includes heat retaining components to focus and contain heat in the production zone to promote flow to, and not just within, the production tubing. | 4 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Not Applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable.
THE NAMES OF THE PARTIES TO A JOINT RESEARCH OR DEVELOPMENT
[0003] Not Applicable.
BACKGROUND OF THE INVENTION
[0004] 1. Field of the Invention
[0005] The present invention relates to alarm systems and in particular to a mobile self-contained security system transportable to remote locations for securing the location against theft or other intrusions, the system comprising a secure sealed container weighted at the bottom to anchor it and a securely attached mounting pole with universal mounting bases to receive any of a variety of security equipment to fit the needs of the location including sensing equipment to detect and visually record intruders and notify a remote location of the intrusion, a variety of alarms including a high decibel siren and strobes simulating police lights.
[0006] 2. Description of Related Art Including Information Disclosed Under 37 CFR 1.97 and 1.98
[0007] New construction theft is at an all time high. Builders are continuously being frustrated by theft of their construction materials. Prior art devices do not adequately provide secure systems which are mobile and self-contained adapted with any necessary security devices to secure individual remote locations.
[0008] U.S. Pat. No. 5,117,223 for a combination portable alarm system and storage container for parts thereof discloses a portable alarm system for a construction site or the like which is provided with and consists of a cabinet, a stanchion supported on the cabinet, an alarm unit supported on the stanchion, and a key pad to program the alarm unit.
[0009] U.S. Pat. No. 5,463,595 for a portable security system for outdoor sites discloses a security system suitable for use in monitoring property at an outdoor site, that includes a portable housing which supports a motion detector for sensing motion within a detection zone.
[0010] U.S. Pat. No. 4,943,799 for a portable alarm system with sealed enclosure discloses a portable alarm system which includes a compact portable sealed housing having an electronic alarm control circuit therein, as well as external detectors.
[0011] U.S. Pat. No. 5,117,223 for a combination portable alarm system and storage container for parts thereof is for a portable alarm system for a construction site or the like with a cabinet, a stanchion supported on the cabinet, an alarm unit supported on the stanchion, and a key pad to program the alarm unit. When not in use the stanchion and alarm unit are stored within the cabinet.
[0012] U.S. Pat. No. 5,463,595 for a portable security system for outdoor sites comprises a security system (10) suitable for use in monitoring property at an outdoor site that includes a portable housing (12) that supports a motion detector (14) for sensing motion within a detection zone. The security system further includes an ultrasonic transducer (74) and several alarm generators capable of repelling a human intruder, including a high intensity illumination source (18), high decibel siren (82), strobe light (19), and a speaker (78) for transmitting a prerecorded message. When an intrusion is initially detected by the motion detector, the ultrasonic transducer is activated to emit an ultrasonic signal that is irritating to nonhuman animals, thus clearing the detection zone of nonhuman intruders. If after sounding of the ultrasonic transducer motion is still detected, one or more of the alarms is activated. Additionally, an automatic telephone dialer (86) may be included in the system and activated by the system as another type of alarm, in response to detected intrusion. The system is integrated within the portable housing and is resistant to false alarms, making it suitable for use in monitoring property stored at an outside site. A method for utilizing the security system to protect property is also disclosed.
[0013] U.S. Pat. No. 4,943,799 provides a portable alarm system with sealed enclosure which includes a compact portable sealed housing having an electronic alarm control circuit therein. An electrical AC cord supplies power to the control circuit and plugs into the housing. A telephone jack connects a telephone circuit to a dialer circuit within the control circuit. A digital key pad is secured to the housing and has a plurality of switches actuable exteriorly of the housing whereby to program the control circuit by a lessor person and for actuating or deactuating the control circuit by a lessee user person. A receiver circuit is also provided in the housing and is connected to the control circuit. One or more wireless infrared detectors are detachably secured to the housing and positioned to detect moving objects within an environment to be protected. The detectors have infrared transmitters, of different frequencies, and transmit alarm signals to the receiver. The receiver has a first channel which is responsive to a first detector and is connected to the control circuit through a delay circuit so that the control circuit only switches to an alarm state to generate an alarm code on the telephone line after a predetermined time delay. The second channel of the receiver has no delay circuit. A siren is connected to the control circuit and secured to the housing to generate an audible local alarm upon activation of the control circuit to the alarm state.
[0014] U.S. Pat. No. 6,154,130 for a portable room security system is for use in hotel rooms, apartments, vehicles having sleeping areas (such as motor homes, RV's, trailers, etc.) and the like. The system integrates into a single housing a smoke detector and a movement sensor, both serially connected to an audio alarm and a visual alert. The system further includes a magnetically isolated slot for holding hotel key cards, as well as a series of hooks for holding several key rings. Also available is a bracket mounted to the housing for holding a flashlight. The system is optionally operated using a remote control device, and may include circuitry enabling automatic telephone dialing to alert outside assistance in the event of an alarm. Two types of structure may be used to suspend the device from an associated door. The first is a pliable extension bar and hook which suspends the device from a door knob. The second is a bracket extension piece enabling the device to be hung from the top of a door. This version is particularly useful to prevent small children from altering the settings.
[0015] U.S. Pat. No. 6,049,274 for a portable security system includes a control circuit 12 electrically connected with a motion sensor 14, an audible alarm 16 and a visual alarm 18. These components are held within a housing 20 which has a standard light globe/tube electrical connector 22 attached to one end 24 for allowing connection to mains power through a corresponding standard light globe/tube socket. A standard light globe 26 is demountably connected within the housing 20 to illuminate an area in the same manner as if the globe 26 were connected directly into the socket which receives the connector 22. A portable remote controller 28 switches the control circuit 12 between an ON state in which the control circuit is active to operate the audible and visual alarms 16, 18 upon detection of a moving body by the motion detector 14; and, an OFF state in which the control circuit deactivates the motion sensor 14 and allows the light globe 26 to be operated as a standard light globe by the switch for the socket to which the connector 22 is connected. Thus, the system 10 can be simply installed in an conventional light socket.
[0016] U.S. Pat. No. 5,587,700 for a portable security alarm unit is made up of a housing component containing control electronics, powered by an external power source, a back-up battery connected to the control electronics and wiring that connects the control electronics and/or battery to external accessories such as motion sensors, a siren, a temperature sensor and to a motion sensor and keyboard built into the frontally located walling of the housing component. There is also a slidable panel component that slides on tracks built into extensions of the roofing and flooring of the housing component such that the slidable panel component is capable of covering completely at any one time either the keyboard or motion sensor both of which are built in adjacent one another into the frontally located walling of the instant device's housing component.
[0017] U.S. Pat. No. 6,864,789 for a personal property security device monitors personal property using a wireless interface to a communication network is presented. The device is comprised of a security module that interfaces with a wireless transceiver such as a cellular telephone. The security module includes a detection monitor the alarms upon a condition and initiates a dialing command to the wireless telephone. The wireless telephone includes a preprogrammed number of a user and is readily reprogrammable to other numbers. Once the communication link is established, the user may listen to the audible conditions around the security device and determine the legitimacy of the alarm. Optional enhanced interrogation of the security device is also contemplated. The security device further includes a location identifier, an example of which is a tracking transmitter that emits a beacon signal for tracking by the user or others.
[0018] U.S. Pat. No. 6,650,239 for an outdoor intrusion detection alarm includes a portable housing (1), a plurality of adjustable fasteners (21) and (22), an augmented switch (5), and a sensor line (3) for sensing human and/or animal intrusions into a predetermined perimeter or boundary configuration, which can be variable in conformity with terrain and flora. A battery powered high decibel piezo siren (7) activates when any intrusion occurs. The sensor line is released, retrieved, and stored on a reel that is an integral part of the housing, completing a lightweight alarm system that fits in a coat pocket or backpack pouch of a camper, hiker, or soldier. The system can also be used for protecting gardens and fruit trees, automobile and airplane displays, and comparable things.
[0019] U.S. Pat. No. 6,181,244 for a construction site portable monitoring system is for use at sites, such as construction sites. The portable monitoring system can provide enhanced security at such sites and may be quickly set up and taken down. A portable monitoring system, in accordance with one embodiment of the invention, includes a housing and a plurality of portable sensing devices and a plurality of mounting platforms both capable of being removably stored in the housing. The mounting platforms may be easily retrieved from the housing and disposed about the site and are each capable of detachably mounting one or more of the portable sensing devices. The portable sensing devices each include a sensor for sensing a stimulus and a transmitter, coupled to the sensor, for transmitting a signal associated with the stimulus. The housing further includes a communication system for receiving the transmitted signals from each of the portable sensing devices and communicating signals associated with the sensed stimuli to an external system.
[0020] U.S. Pat. No. 6,288,642 for a self-contained security system comprises at least one satellite unit coupled in signal communication to a main unit, the main unit for emitting an alerting stimulus in response to a signal received from the satellite unit indicating the presence of a security threat.
[0021] U.S. Pat. No. 5,565,844 for an intrusion detector employs a remote, 360 degree infrared detector. The system includes a base unit with a receiver, controller, and phone jack, a remote sensor which is adjustable along a vertical axis and includes a 360.degree. infrared motion sensor, and a central monitoring station in communication with the base unit via a telephone network. The remote sensor may be selectively positioned to detect movement in a surrounding area definable by the user. The base unit may be programmed to contact the monitoring station when the sensor detects motion, and also to receive test signals from the monitoring station and verify that the system is operational.
[0022] U.S. Pat. No. 4,742,336 for a portable intrusion detection warning system is housed in a portable carrying case in the configuration of a briefcase with handle for convenient portability and inconspicuous placement at a desired location near a space to be monitored. Intrusion detectors are removed from the carrying case and placed in the space to be monitored. The intrusion detectors may include infrared motion sensors and radio transmitters for transmitting detection signals to a radio receiver in the carrying case. An electronic controller receives the detection signals from the radio receiver and delivers actuating data signals to a digital communicator and digital dialer with a telephone line output. The digital communicator captures a telephone line with dialing signals and sends further coded signals corresponding to different monitored spaces and intrusion detectors from which detection signals are received. The electronic controller includes an arming circuit and key switch for arming and disarming the monitoring and warning system. The external power supply plug, telephone jack and key switch are mounted on the carrying case so that the components are operable from outside the carrying case with the intrusion detectors in place and the briefcase configuration carrying case closed and locked. Internal battery standby power supply is also provided.
[0023] U.S. Pat. No. 4,151,520 for a portable self-contained alarm with remote triggering capability comprises a portable housing having an audio alarm positioned therein and a battery powered electronic circuit for activating the alarm. The circuit comprises a battery, an arming switch, a triggering switch, an audio alarm, and a latching circuit and oscillator circuit utilizing an integrated circuit therein. The circuit also includes a means for connecting auxiliary devices thereto and a means for coupling an AC adapter. A magnetically operated reed switch and a mechanically operated pull switch comprise the normally open triggering switch. The triggering switch also contains means for adapting any activator wired normally open to the triggering switch. The oscillator circuit drives the audio alarm whenever any of the triggering switches are closed and the latching circuit maintains the oscillator in an operating mode.
[0024] U.S. Pat. No. 4,319,228 for a portable intrusion alarm is provided in a compact enclosure permitting its movement from location to location as needed. The alarm includes one or more motion detectors, some of which may be battery operated, one or more alarm devices, such as sirens, strobe lights, and remote etc., door switches and appropriate relays for operating the system. A battery back up system insures that the alarm is always activated.
[0025] U.S. Pat. No. 5,587,701 for a portable alarm system is disclosed in which the alarm functions are contained within a portable enclosure, communication is maintained between the enclosure and wireless security contacts placed at points of entry, and the alarm is capable of initiating a telephone call to a security monitor station either by conventional hard wired telephone lines within a building, or by cellular transmission, or via 800 MHz trunking.
[0026] What is needed is a mobile self-contained security system transportable to remote locations for securing the location against theft or other intrusions, the system comprising a secure sealed container weighted at the bottom to anchor it and a securely attached mounting pole with universal mounting bases to receive any of a variety of security equipment to fit the needs of the location including sensing equipment to detect and visually record intruders and notify a remote location of the intrusion, a variety of alarms including a high decibel siren and strobes simulating police lights.
BRIEF SUMMARY OF THE INVENTION
[0027] An object of the present invention is to provide a mobile self-contained security system transportable to remote locations for securing the location against theft or other intrusions, the system comprising a rugged secure sealed container capable of withstanding the demanding environment of a construction site weighted at the bottom to anchor it and a securely attached mounting pole with universal mounting bases to receive any of a variety of security equipment to fit the needs of the location including sensing equipment to detect and visually record intruders and notify a remote location of the intrusion, a variety of alarms including a high decibel siren and strobes simulating police lights.
[0028] Another object of the present invention is to provide a tamperproof, waterproof, sealed container and mounting pole.
[0029] In brief, a mobile, reusable housing and mounting platform for the use of security products/devices and services those items can provide. This product would allow the items contained within to work outside the normal parameters they were originally designed for. For example, home security systems are traditionally designed to be installed in a home or business. However, by installing them within this housing, they could be used to protect houses while under construction (i.e. as a jobsite deterrent system). Likewise, cameras and a digital video recorder could be added to create a mobile video device. While the invention is intended primarily as a job site deterrent system, this product can be used in many applications. Such as guard tour check in stations. Several units can be set up on a single site to ensure the guard is making their tours as scheduled failing to checking in at one of the stations could call the monitoring center and report the missed round.
[0030] An advantage of the present invention is that it provides a portability for use in construction job sites and other sites that would need a temporary security system that is rugged and yet substantial enough in size to withstand the demanding environment of a construction site.
[0031] Another advantage of the present invention is that it provides not only a wired power supply, but a large capacity backup battery in the base for supplying power to the security system for up to one week if the wired power supply is lost
[0032] An added advantage of the present invention is that it provides additional security add-ons to the basic system using the mounting pole, such as video and audio monitoring.
[0033] An extra advantage of the present invention is the ability to a wirelessly link multiple units together to add greater coverage and simplified operation to larger projects.
[0034] A further advantage of the present invention is that it provides a high decibel siren and red and blue strobes simulating police lights to deter theft and other suspicious activity.
[0035] A supplementary advantage of the present invention is the ability to connect to the job-sites existing hardwired window and door sensors via a wireless connection module adding to the systems overall perimeter intrusion detection capabilities
[0036] One more advantage of the present invention is that it provides a compact, self-contained mobile security system for monitoring and recording activity, and reporting intrusions at unsecured unoccupied locations to deter theft and other crimes.
[0037] An additional advantage of the present invention is that it provides a system that is tamper proof and waterproof.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0038] These and other details of the present invention will be described in connection with the accompanying drawings, which are furnished only by way of illustration and not in limitation of the invention, and in which drawings:
[0039] FIG. 1 is a perspective view showing the compact, self-contained mobile security system of the present invention;
[0040] FIG. 2 is a perspective view showing the control panel for the system of FIG. 1 showing the keypad and digital readout window;
[0041] FIG. 3 is an exploded partially broken perspective view of the system of FIG. 1 showing the components aligned for assembly.
DETAILED DESCRIPTION OF THE INVENTION
[0042] In FIGS. 1-3 , a compact, self-contained mobile security system 10 for monitoring and recording activity, and reporting intrusions at unsecured, unoccupied locations to deter theft and other crimes comprises a barrel-shaped reusable mobile container 20 with a center mounting pole 40 for removably installing any of a variety of security devices.
[0043] In FIGS. 1 & 3 , the reusable mobile container 20 comprises an enclosed housing fabricated of shock resistant waterproof material having a bottom portion 22 for resting on a horizontal external surface, a top portion 21 covering an opening for accessing the interior of the container for installing and removing any of a variety of security devices in the container, and a series of support poles 28 around the interior. The top portion 21 seals closed on the bottom portion, and a rigid mounting pole 40 with a cap 41 at the top extends upwardly through a sealed pole opening 23 in the top portion, the sealed connector 47 for the pole connecting to the quick connect harness 26 in the base, to form a sealed tamperproof, waterproof container 20 and mounting pole 40 .
[0044] In FIG. 3 , a weighted ballast 18 of poured concrete is contained in a bottom portion of the mobile container 20 for maintaining the portable container in an upright position. A mounting platform 16 is attached to the interior of the transportable container to support the mounting pole 40 formed from PVC pipe that can receive any of a variety of security devices attached thereto. An electronic control circuit board 27 is also housed within the sealed transportable container 20 to which all of the security devices are connected electrically.
[0045] In FIGS. 1-3 , a control panel with keypad 30 is attached to the exterior of the portable container 20 , the control panel 30 communicates with the electronic control circuit 27 to control a series of security devices electrically communicating with the electronic control circuit. The control panel 30 is programmed to receive a security code by an authorized user to deactivate the security system during authorized use of the location and to activate the security system for securing the location when not in authorized use. In FIG. 2 , the control panel comprises status indicator lights 31 to indicate if the system is activated or not, a readout area 35 , and keys 30 that feature both numbers 33 and symbols 34 .
[0046] In FIGS. 1 & 3 , the security system 10 accommodates a plurality of security devices attached to the mounting platform 16 and the mounting pole 40 which electrically communicate with the electronic control circuit 27 housed in the control circuit box 25 . The security devices comprise at least one security device, and can include a 122 db ear piercing siren 29 housed within the transportable container for sound notification of intrusion and deterrence, at least one high luminance strobe light 42 A & B attached to a top portion of the mounting post for visual notification of intrusion and deterrence, a voice module 43 A for recording voices and sound and broadcasting voices and sound for sound monitoring and deterrence, any of a variety of motion detection devices 43 B including passive infrared devices and microwave devices and any of a variety of camera recording devices mounted on the mounting pole 40 for 360 degree visual monitoring and recording and transmission to at least one remote location, and a communication device for dispatching personnel to the location from a remote location. The system 10 further comprises an auxiliary connection used on sites that are pre-wired for alarm systems in buildings to enable the arming of doors and windows once they have been installed.
[0047] In FIG. 3 , the security system 10 is powered by a wired power supply connection for powering all components of the system and a large capacity backup battery 17 housed in the bottom 22 of the mobile container 20 for supplying power to the security system for up to one week if the wired power supply is lost.
[0048] FIGS. 1 & 3 show at least one high luminance strobe 42 A & B preferably comprising a red strobe and a blue strobe to simulate police strobe lights is mounted to the pole 40 .
[0049] FIG. 3 shows the electronic control circuit board 27 connected to a universal wiring harness 24 for electrically connecting the plurality of security devices.
[0050] In use, at a remote location, such as a construction site, after a building has been framed, and the portable security system 10 of the present invention is armed and put into place on the job site, the system of the present invention will then begin deterring intruders. The present invention may comprise a 4-camera job-site security device with recording, monitoring, intrusion detection and alarm sensing capabilities 43 A & B mounted on a 7-foot pole 40 and installed on a remote site. It will detect their presence and sound an ear-piercing 122 db siren 29 and flash high luminance red and blue strobes 42 A & B to discourage intruders from committing crimes on the property. An LCD keypad 30 , supplied for all units at a development site, plugs into a front of the present invention and can be used to track all the times the device was triggered and set off alarms and can be used to track all the times the device was armed and disarmed and with which code. When the communication feature is activated the customer can receive notification of alarms, trouble signals, when and by who armed or disarmed the system by a phone call from the monitoring center personnel, a text message or an e-mail. The present invention can be disarmed during construction times and re-armed after sub-contractors have left for the day. The system can be programmed to auto-arm at a predetermined time so if a contractor forgets to arm the system upon leaving the job-site, it limits the exposure of the site to theft. After doors and windows are installed, the present invention can connect to the pre-wired alarm system contacts in the structure to arm them as well. Options are also available for voice module, camera, recording devices, wireless devices and dispatched center monitoring, as well.
[0051] A wired power supply connection powers all components of the system and a large capacity backup battery 17 supplies power for up to one week if ac power is lost.
[0052] The system 10 thereby forms a compact, yet substantial and rugged self-contained mobile security system for monitoring and recording activity, and reporting intrusions at unsecured unoccupied locations to deter theft and other crimes.
[0053] It is understood that the preceding description is given merely by way of illustration and not in limitation of the invention and that various modifications may be made thereto without departing from the spirit of the invention as claimed. | A secure sealed container and mounting pole house any of a variety of security equipment. Sensing equipment, a high decibel siren, and strobes simulating police lights are removably attachable to a universal mount and control circuit. A control panel connected to the circuit enables and disables the alarm, and monitors system activity. | 6 |
FIELD OF THE INVENTION
The present invention is generally related to a massaging bed rest, and more particularly is related to a massaging bed rest with rotatable armrests.
BACKGROUND OF THE INVENTION
Cushioned bed loungers are known in the art. Bed loungers normally include a back portion and arm rests or elbow rests. The back portion may be contoured and may include a padded neck or head rest. Chair back massagers also are known in the art. One form of prior art back massager is in the form of a pad containing a mechanical massage arrangement powered by electricity. In use, a person places the massager against the back of a chair, automobile seat, or couch and then sits downs and leans back against the massaging device. Other configurations have the massaging elements built into the seat back, for example in a lounge chair or automobile seat. Such massagers include a back portion including a massaging element driven by an electric motor.
U.S. Pat. No. 5,895,365, by Tomlinson, discloses a bed rest cushion for providing a vibrating massage including a back portion and two armrests. The two armrests are pivotally coupled to the back portion. However, the armrests are coupled to allow the armrest to rotate outward from the back portion. The armrests do not rotate about the sides of the back portion. The rotation of the bed rest cushion described by Tomlinson does not facilitate storage of the bed rest cushion, nor using the bed rest as a flat massaging cushion for placement in a chair or under the chest of a person when laying down on their stomach.
Thus, a heretofore unaddressed need exists in the industry to address the aforementioned deficiencies and inadequacies.
SUMMARY OF THE INVENTION
In one aspect, the invention features a foldable massaging bed cushion for supporting a person in a sitting position. The massaging bed cushion contains a backrest with two side edges, two armrests rotatably coupled to the backrest, and one or more massaging units within the backrest. The two armrests can rotate from a sitting position to a folded position along the two side edges of the backrest.
The two armrests can be perpendicular to the backrest in the sitting position. In addition, the two armrests can rotate from zero to one hundred and eighty degrees from the backrest. The sitting position is formed by rotating the two armrests from about forty-five to about one hundred and thirty-five degrees from the backrest. Preferably, the sitting position is formed by rotating the two armrests to ninety degrees (90°) from the backrest. The backrest and the two armrests can form nearly a rectangular top profile in the folded position.
Other features and advantages of the present invention will be or become apparent to one with skill in the art upon examination of the following drawings and detailed description. It is intended that all such additional features and advantages be included within this description, be within the scope of the present invention, and be protected by the accompanying claims.
BRIEF DESCRIPTION OF THE DRAWINGS
Many aspects of the invention can be better understood with reference to the following drawings. The components in the drawings are not necessarily to scale, emphasis instead being placed upon clearly illustrating the principles of the present invention. Moreover, in the drawings, like reference numerals designate corresponding parts throughout the several views.
FIG. 1 is a perspective view of the massaging cushion unfolded for use in a sitting position, in accordance with a first exemplary embodiment.
FIG. 2 is a side view of the massaging cushion of FIG. 1 unfolded for use in the sitting position.
FIG. 3 is a front view of the massaging cushion of FIG. 1 unfolded for use in the sitting position.
FIG. 4 a is a block diagram illustrating interaction of the interior components of the massaging cushion of FIG. 1 , in accordance with the first exemplary embodiment of the invention.
FIG. 4 b is a block diagram illustrating the interaction of the interior components of the massaging cushion of FIG. 1 , in accordance with a second exemplary embodiment of the invention.
FIG. 5 is a perspective view of the massaging cushion of FIG. 1 folded into a storage position or for use in a laying down position.
FIG. 6 is a top view of the massaging cushion of FIG. 1 folded into a flattened position for use in a laying down position or for storage in accordance with the first exemplary embodiment of the invention.
FIG. 7 is a perspective view of a massaging cushion folded into a flattened position for use in a lying down position or for storage in accordance with a third exemplary embodiment of the invention.
DETAILED DESCRIPTION
FIG. 1 is a perspective view, FIG. 2 is a side view, and FIG. 3 is a front view of the massaging cushion 100 unfolded for use in a sitting position, in accordance with a first exemplary embodiment of the invention. The massaging cushion 100 comprises a backrest 102 , a right armrest 104 , and a left armrest 106 . An axle 108 couples the right armrest 104 and left armrest 106 to the backrest 102 . In addition, the axle 108 runs through a lower portion 110 of the backrest 102 . The axle 108 allows the right armrest 104 and left armrest 106 to rotate about the backrest 102 as indicated by the arrows shown in FIG. 1 and FIG. 2 . When the massaging cushion 100 is unfolded into a sitting position, the user sits between the right armrest 104 and left armrest 106 . The right and left arms of the user rest on the right armrest 104 and the left armrest 106 , respectively. The back of the user rests on a front surface 118 of the backrest 102 of the massaging cushion 100 . The weight of the arms and upper body of the user rests upon the right armrest 104 and left armrest 106 . The weight on the armrests 104 and 106 upon the floor provides a frictional force that prevents the backrest 102 from sliding backwards when using the massaging cushion 100 in the sitting position. Alternatively, while resting on the massaging cushion 100 , a back surface 120 of the backrest 102 may be leaned against a wall, a back portion of a bed, or any other surface that will prevent the backrest 102 from moving backward.
The axle 108 allows the right armrest 104 and left armrest 106 to rotate about the backrest 102 . In the first exemplary embodiment, the right armrest 104 and left armrest 106 can rotate one hundred and eighty degrees from the backrest 102 . When the massaging cushion 100 is in the sitting position, the right armrest 104 and left armrest 106 are rotated between about ninety degrees to about one hundred and twenty degrees from the backrest 102 . The lower backside of the user prevents the backrest 102 from rotating out of the sitting position. The user can adjust the slant of the backrest 102 by moving the lower backside of the user closer or further away from the lower portion 110 of the backrest 102 . By moving the lower backside of the user closer to the backrest 102 , the angle between the armrests 104 and 106 and the backrest 102 is decreased. By moving the lower backside of the user further away from the lower portion 110 of the backrest 102 , the backrest 102 is allowed to rotate, increasing the angle between the armrests 104 and 106 and the backrest 102 .
The left armrest 106 and right armrest 104 may rotate about the axle 108 together or separately. As an example, movement of the left armrest 106 may force the right armrest 104 to rotate with the left arm rest 106 . Alternatively, the left armrest 106 may rotate about the axle 108 independent from the right armrest 104 These different examples of movement of the left armrest 106 and right armrest 104 may be made possible by a series of gears, joints, or any other device known by those having ordinary skill in the art that may allow and/or limit rotation about the axle 108 .
In another embodiment, a rotation latch (not shown) can be used to prevent the backrest 102 from rotating out of the sitting position. The rotation latch prevents the right armrest 104 and left armrest 106 from rotating beyond a desired angle from the backrest 102 . For example, the rotation latch can allow the backrest 102 to rotate one hundred degrees from the right armrest 104 and the left armrest 106 . This allows the massaging cushion 100 to remain in the sitting position without relying on support from the arms and lower backside of the user. In addition, the rotation latch can also be an adjustable latch that allows the user to set a maximum angle of rotation. This allows the user to customize and set the maximum angle between the armrest 104 , 106 and the backrest 102 that is allowed by the massaging cushion 100 .
A control panel 112 located on a top surface of the right armrest 104 allows the user to activate one or more massaging units 114 and one or more heating units 116 . The location of the control panel 112 provides easy access by the hands of the user when the user is being supported by the massaging cushion 100 adjusted to the sitting position. The control panel 112 is not limited to being located on the top surface of the right armrest 104 . The control panel 112 can instead be mounted on a variety of different locations and surfaces of the massaging cushion 100 . The control panel 112 can contain various displays, switches, and knobs used to control the one or more massaging units 114 and the one or more heating units 116 . For example, the knobs or switches can be used to control the amount of heat provided by the heating units 116 . The knobs or switches can also be used to control the massaging intensity and motion of the massaging units. The display can be a Light Emitting Diode (LED) display that shows the current settings of the one or more massaging units 114 and one or more heating units 116 .
The one or more massaging units 114 can be located within the backrest 102 . In addition, the one or more massaging units 114 can be built into the cushion of the backrest 102 . The massaging units 114 can be a variety of massaging devices arranged within the backrest 102 , for example, but not limited to, massage motors, pulsating transducers, and powered rollers. The location of the massaging units 114 can be a variety of locations and surfaces on the massaging cushion 100 , for example, but not limited to, the top surface or inside surface of the armrests 104 and 106 .
Along with the one or more massaging units 114 , the massaging cushion 100 can also have the one or more heating units 116 . Similar, to the massaging units 114 , the one or more heating units 116 can also be built into the cushion of the backrest 102 . The heating units 116 also can be located in a variety of locations and surfaces of the massaging cushion 100 . In addition, the heating units 116 may be located within the armrests 104 , 106 . During use, the heating unit 116 can generate heat when current is applied to the heating element. Other means for providing heat would be known by those having ordinary skill in the art.
The control panel 112 can regulate both the one or more massaging units 114 and the heating units 116 . The control panel 112 can also selectively activate the massaging units 114 and heating units 116 in a variety of patterns, providing different massaging sequences. These sequences can be stored in a memory of the control panel 112 . A user can select a desired sequence on the control panel 112 and the control panel 112 can activate the different massaging units 114 and heating units 116 based on the selected pattern of the user.
FIG. 4 a is a block diagram illustrating interaction of interior components 400 a of the massaging cushion 100 in accordance with a first exemplary embodiment of the invention. The control panel 112 a can be electrically coupled to each massaging unit 114 a and each heating unit 116 a. A power source 402 a supplies the power to operate the control panel 112 a. The control panel 112 a selectively supplies power to each of the massaging units 114 a and each of the heating units 116 a depending on the control panel 112 a setting. The control panel 114 a controls each massaging unit 114 a and each heating unit 116 a by varying the amount of current supplied to each massaging unit 114 a and each heating unit 116 a.
FIG. 4 b is a block diagram illustrating interaction of interior components 400 b of the massaging cushion 100 in accordance with a second exemplary embodiment of the invention. The power source 402 b can be electrically coupled to the control panel 112 b, the one or more massaging units 114 b, and the one or more heating units 116 b. The power source 402 b supplies power directly to each component. The control panel 112 b can be electrically coupled to each massaging unit 114 b and each heating unit 116 b or the control panel 112 b can be connected to each massaging unit 114 b and each heating unit 116 b by wireless communication. The control panel 112 b signals each of the massaging units 114 b and each of the heating units 116 b by electrical pulse or a wireless communication protocol based on the desired setting selected by the user via the control panel 112 b. Each of the massaging units 114 b and each of the heating units 116 b respond to the signals by adjusting to the desired setting. For example, a heating unit 116 b that receives the signals from the control panel 112 b to increase the temperature, would increase the current to the heating unit 116 b.
The power source 402 a and 402 b can be a battery mounted within the backrest 102 , the right armrest 104 , or the left armrest 106 . In addition to the power source 402 a, 402 b being a battery, the power source 402 a, 402 b can also be an electrical plug that enters through a surface on the massaging cushion 100 . The user would plug the electrical plug into a wall socket to supply the power to run the control panel 112 , the one or more massaging units 114 , and the one or more heating units 116 . The power source 402 a, 402 b can also be a combination of the electrical plug and the battery. For example, the battery can be a rechargeable battery that supplies the power for the massaging cushion 100 when the massaging cushion 100 is used in a location remote from a wall socket. The massaging cushion 100 can also have the electrical plug used to recharge the battery or supply power when the massaging cushion 100 is used in a location within reach of a wall socket.
The massaging cushion 100 can be constructed of a solid frame with foam or padding material located between the solid frame and a cover. The cover can be made from a variety of materials, for example, but not limited to, fabric, leather, or vinyl. The solid frame can be made of a variety of materials, for example, wood, metal, or plastic. Instead of a solid frame surrounded by padding material, the frame can also be constructed using a semi-hard foam rubber. The semi-hard foam rubber would not require the additional padding material. The control panel 112 , massaging units 114 , and heating units 116 can be supported by the solid frame or the semi-hard foam rubber frame within the massaging cushion 100 . The massaging cushion 100 can be constructed to have a relatively flat surface profile as shown in FIGS. 1-3 . The massaging cushion 100 can also be constructed to have a more contoured profile that conforms to the contours of the human body.
FIG. 5 is a perspective view and FIG. 6 is a top view of the massaging cushion 100 folded into a flattened position for use in a lying down position or for storage in accordance with the first exemplary embodiment of the invention. The right armrest 104 and left armrest 106 may be folded inline with the backrest 102 . This allows the massaging cushion 100 to have a rectangular shape when in the flattened position to facilitate storage. Due to rectangular shape when in the flattened position, multiple massaging cushions 100 can be stacked vertically or the massaging cushion can be easily stored on a shelf in the folded position. In addition, when in the flattened position, the massaging cushion 100 easily fits within a rectangular storage device, such as, but not limited to, a box.
The massaging cushion 100 can also be used as a massaging pillow in the folded position. The user can sit on top of the massaging cushion 100 while the massaging cushion 100 provides a massage to the lower back and thighs of the user. A user can also use the massaging cushion 100 in the folded position to prop up the chest of the user when the user is lying on their stomach. In this position the massaging cushion 100 can be used to provide a massage to the chest of the user. As previously discussed, the massaging units 114 and heating units 116 can be provided on a variety of surfaces and locations on the massaging cushion 100 . The massaging units 114 and heating units 116 can be provided on both the back surface 120 and the front surface 118 of the backrest 102 . This allows the user to use the massaging cushion 100 in the sitting position or in the folded position as a pillow while maintaining easy access to the control panel 112 . The massaging units 114 and heating units 116 can also be centrally located within the backrest 102 so as to provide a massaging effect and heating to both the back surface 120 and the front surface 118 of the backrest 102 from within the backrest 102 .
FIG. 7 is a top view of the massaging cushion 700 folded into a flattened position for use in a lying down position or for storage in accordance with a third exemplary embodiment of the invention. In the third exemplary embodiment, the axle 108 shown in FIG. 1 does not run all the way through the backrest 102 . Instead, in the third exemplary embodiment of the right armrest 706 is coupled to the backrest 702 by a right axle 707 and the left armrest 704 is coupled to the backrest 702 by a left axle 709 . The right axle 707 and left axle 709 allow the right armrest 706 and left armrest 704 to rotate about the backrest 702 . The third exemplary embodiment also allows the right armrest 706 and left armrest 704 to rotate independently about the backrest 702 .
It should be emphasized that the above-described embodiments of the present invention are merely possible examples of implementations merely set forth for a clear understanding of the principles of the invention. Many variations and modifications may be made to the above-described embodiment(s) of the invention without departing substantially from the spirit and principles of the invention. All such modifications and variations are intended to be included herein within the scope of this disclosure and the present invention and protected by the following claims. | A foldable massaging bed cushion for supporting a person in a sitting position has a backrest with two side edges, two armrests rotatably coupled to the backrest, and one or more massaging units within the backrest. The two armrests can rotate from a sitting position to a folded position along the two side edges of the backrest. The foldable massaging bed cushion can also have one or more heating units and one more massaging units located within the backrest and a control panel to control the massaging units and heating units. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
Reference is made to provisional utility patent application No. 60/438,536 entitled “Microwave alerting system for vehicles” filed by John A. Scholz on 8 Jan. 2003 with the USPTO.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
I certify that the invention described in this utility patent application has been developed privately and has no relation whatsoever to any federally sponsored research or development programs.
REFERENCE TO A SEQUENCE LISTING, A TABLE, OR A COMPUTER PROGRAM LISTING COMPACT DISK APPENDIX
Not Applicable.
BACKGROUND OF THE INVENTION
The invention relates to a microwave vehicle-to-vehicle signaling device that uses an electronic warning signal impressed on a microwave signal in order to provide two-way communications among vehicles. The microwave signaling device transmits and receives warning signals, and provides electronic control signals for controlling visible and audible warning indications to the driver of a vehicle in response to the electronic warning signal.
One way to reduce traffic noise and improve the effectiveness of warning signals exchanged among vehicles is to equip each vehicle with a microwave vehicle-to-vehicle signaling device that is capable of both transmitting warning signals by means of a microwave signal and receiving warning signals from other vehicles by means of a microwave signal. The microwave vehicle-to-vehicle signaling device transforms received microwave signals into control signals that are suitable for controlling devices for producing sounds, for example the sound of an automobile horn that is generated by means of speakers arranged around a driver of a vehicle. The amplitude of the sound from each speaker is controlled by the signaling device in such a way as to provide an indication of the direction to the origin of the received warning signals. The amplitude and frequency of the sound from each speaker is also controlled by the signaling device in such a way as to provide an indication of the distances to vehicles that are transmitting warning signals. The sounds are generated within the vehicle at an amplitude that is inaudible or nearly inaudible outside of the vehicle. The microwave vehicle-to-vehicle signaling device also produces control signals that are suitable for controlling lamps or displays located within the field of view of the driver of each receiving vehicle, which provides assistance to drivers with hearing difficulties.
One object of the invention is to reduce or eliminate noise due to audible vehicle-to-vehicle signaling devices by confining most or all audible warning sounds, for example those produced by automobile horns, to the passenger compartment of each vehicle. The effective range of a warning signal transmission is limited by atmospheric absorption and by the transmitted signal power.
Another object of the invention is to provide control signals that are suitable for producing sounds within a vehicle by controlling a set of audio speakers or other sound producing devices in such a way as to allow the driver to determine the general directions and relative distances of microwave transmitters that are transmitting the warning signals.
Another object of the invention is to increase the effectiveness of audible police vehicle or emergency vehicle warning signals by reducing the ambient noise level in the environment. Alternatively, the invention allows a police vehicle or an emergency vehicle to reduce the amplitude of its audible vehicle-to-vehicle signaling device. The invention reduces the need for police and emergency vehicles to produce high amplitude audible warning signals, which are normally necessary to penetrate closed vehicles and compete with sound from music, conversation, and ambient traffic noise. The ambient traffic noise also includes automobile horn sounds, which would be reduced in amplitude by the invention. The microwave signals produced by the invention are inaudible to humans.
A further object of the invention is to limit the duty cycle and pulse repetition frequency of the microwave vehicle-to-vehicle signaling device, for example to prevent excessive use of the signaling device.
A system for producing automobile horn sounds by synthetic means is described by Solow (U.S. Pat. No. 6,489,885), where a digital counter responsive to clock signals from an oscillator sequentially reads horn audio data from digital memory, which provides the data to a D/A converter and the output audio signal to a speaker for broadcast. Farmer (U.S. Pat. No. 5,979,586) describes a vehicle collision warning system that converts collision threat messages from a predictive collision sensor into intuitive sounds which are perceived by the occupant to be directed from the direction of the potential collision. The collision threat messages are derived from a range sensing circuit, for example a radar set mounted in the vehicle, and they are not transmitted from a second vehicle. Settles (U.S. Pat. No. 5,933,074) describes a radio transmitter that operates in conjunction with a microwave (RF) receiver installed in a vehicle to unlock the doors of the vehicle when a unique RF signal is broadcast within a defined range, and actuate the horn of the vehicle when the same RF signal is broadcast outside of the defined range. The radio transmitter is hand held and is typically carried on a key chain, and it actuates an audible horn sound from a single remote vehicle, thereby increasing the ambient noise level.
The current invention describes a vehicle-to-vehicle signaling device for two-way communications that converts microwave warning messages sent by transmitting vehicles into control signals that are suitable for controlling devices that produce synthetic, intuitive sounds and displays in receiving vehicles. The sounds and displays are perceived by the drivers of receiving vehicles to be directed from the several directions and relative distances of transmitting vehicles. The range of a transmitted signal is confined to a limited distance around a transmitting vehicle by atmospheric absorption of the electromagnetic wave that carries the transmitted signal, and also by the transmitter power, which is set to a predetermined level. Receiving vehicles located beyond a limited distance from a transmitting vehicle do not react to the microwave warning messages due to the weakness of the signal. Vehicles that receive the microwave warning messages are also capable of transmitting microwave warning messages.
The purpose of the invention is to reduce the ambient noise level in the environment by reducing the noise produced by automobile horns and other audible vehicle-to-vehicle signaling devices, and also to improve the effectiveness of warning signals exchanged among vehicles.
BRIEF SUMMARY OF THE INVENTION
The invention consists of a microwave transceiver and a multiple channel controller.
The microwave transceiver generates and transmits warning signals by means of microwave frequency electromagnetic waves that are modulated to carry information. The microwave transceiver also intercepts the electromagnetic wave from any other transmitting microwave transceiver within a limited distance and converts it into control signals that are suitable for controlling sound or light producing devices.
The transmitting part of the microwave transceiver consists of a waveform generator for producing electronic warning signals, a modulator for impressing electronic warning signals onto an electronic carrier signal, an amplifier for increasing the power of the modulated electronic carrier signal, and an antenna designed to convert the modulated electronic carrier signal into an electromagnetic wave and radiate the electromagnetic wave within a defined solid angle.
The antenna is designed according to common practice to both transmit and receive the electromagnetic wave. It consists of a cluster of microwave transmitting and receiving elements, with each one pointed in a different direction in azimuth, preferably at equal intervals in angle. In a preferred embodiment of the invention, the antenna consists of a cluster of four microwave transmitting and receiving elements pointed in directions that are separated by 90 degrees in azimuth. When receiving, the antenna provides separate electronic warning signals on a number of separate electrical channels. The number of channels is equal to the number of elements in the cluster of microwave transmitting and receiving elements, and each element of the cluster provides signals to one electrical channel. For example, a cluster of four microwave transmitting and receiving elements produces four separate electrical channels for carrying electronic warning signals. When transmitting, the antenna accepts at least one input signal to be transmitted over all of the elements in the cluster simultaneously.
The receiving part of the microwave transceiver consists of the antenna, which receives the electromagnetic wave from within a defined solid angle and converts it into a modulated electronic carrier signal, an amplifier for increasing the power of the modulated electronic carrier signal, and a demodulator for retrieving electronic warning signals from the modulated electronic carrier signal.
The multiple channel controller transforms the electronic warning signals provided by the receiving part of the microwave transceiver into one or more digital or analog control signals that are suitable for controlling an audio system or a display to produce warnings. Each channel of the multiple channel controller is capable of converting the electronic warning signals into separate control signals in order to provide the driver of a vehicle with an intuitive impression of the directions and distances of nearby vehicles that are transmitting warning signals, for example by controlling the amplitude and tone of each speaker in a set of speakers.
When the driver of a first vehicle wishes to signal one or more drivers of other vehicles, the first driver activates a switch, for example the horn button on a steering wheel or the siren switch in a police car. This activates the microwave transceiver, which is mounted for example underneath the roof of the first vehicle.
The microwave transceiver in the first vehicle transmits a microwave warning signal in all directions in azimuth, and preferably within a limited angle in elevation. In a preferred embodiment, the elevation angle is confined by the design of the transceiver antenna to within several degrees of the plane of the road. Humans cannot hear microwave signals, but setting limits on the elevation angle conserves power. The receiving part of the microwave transceiver in the first vehicle is switched off temporarily during the time of the transmission to prevent the first vehicle from reacting to its own warning signals.
The microwave transceiver in each vehicle within a limited distance of the first vehicle intercepts the transmitted warning signal from the microwave transceiver of the first vehicle and transforms it into a set of electronic warning signals on separate electrical channels. Microwave transceivers located beyond a limited distance from the first vehicle, for example one hundred meters, do not respond to the microwave warning signal. This is due to the fact that propagation and atmospheric absorption cause the microwave warning signal to attenuate to a level that is not detected by a microwave transceiver that is located beyond a limited distance from the first vehicle.
The multiple channel controller transforms the set of electronic warning signals, provided by the microwave transceiver over separate electronic channels, into digital or analog control signals that are suitable for controlling an audio system or a visible display to produce warnings. The control signals from the multiple channel controller are designed to control an audio system or display in such a way as to give the driver of the vehicle an intuitive impression of the directions and distances and types of vehicles that are transmitting warning signals.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
A more complete appreciation of the present invention and many of the attendant advantages thereof will be readily obtained as the same becomes better understood by reference to the following detailed description when considered in connection with the accompanying drawings, wherein:
FIG. 1 illustrates the processes according to the invention whereby a microwave transceiver mounted in a first vehicle transmits microwave warning signals that are intercepted by a microwave transceiver mounted in a second vehicle. The microwave transceiver in the second vehicle converts the microwave warning signals into one or more separate electrical channels that carry electronic warning signals. The multiple channel controller in the second vehicle converts the electronic warning signals into one or more control signals that are suitable for controlling audible and visible warnings to the driver of the second vehicle.
FIG. 2 illustrates the processes according to the invention whereby a microwave transceiver transmits and receives warning signals and a multiple channel controller transforms received warning signals into control signals that are suitable for controlling audio and display devices. Activation of the microwave transceiver by the driver of a first vehicle causes an electronic warning signal to be generated by means of a waveform generator. The electronic warning signal is then impressed onto an electronic carrier signal by means of a modulator, and the modulated electronic carrier signal is amplified by means of an amplifier and then converted into a microwave frequency electromagnetic wave and radiated by means of an antenna. In a preferred embodiment, the antenna is a cluster of four microwave transmit and receive elements arranged in such a way that their directions of maximum sensitivity to the electromagnetic wave are separated equally in azimuth by 90 degrees. The microwave signal radiated by the microwave transceiver in the first vehicle is intercepted by the microwave transceiver in a second vehicle and converted by the antenna in the second vehicle into a set of modulated electronic carrier signals on one or more electrical channels. The modulated electronic carrier signal carried by each electrical channel is produced by one of the microwave elements in the antenna. The modulated electronic carrier signal on each channel is amplified by means of an amplifier and demodulated by means of a demodulator to retrieve the electronic warning signal sent from the first vehicle. The electrical channels produced by the second vehicle microwave transceiver are processed by the multiple channel controller into control signals that are suitable for controlling devices that produce audible and visible warnings.
FIG. 3 illustrates a preferred configuration of the antenna, which is constructed as an array of four microwave transmitting and receiving elements pointed at 90 degree intervals in azimuth. Each element provides a single output electrical channel in response to an incoming microwave warning signal, and each element is also capable of transmitting a microwave warning signal. The broadcast pattern of each element is designed in such a way that a uniform broadcast from all four elements taken together produces a microwave warning signal with uniform power in all directions in azimuth.
FIG. 4 shows the relative power in all directions in azimuth of the microwave warning signal broadcast by a first vehicle microwave transceiver, and also shows the relative sensitivity to the microwave warning signal of each element in the antenna array of a second vehicle microwave transceiver. Both microwave transceivers are capable of transmitting and receiving microwave warning signals. The microwave warning signal broadcast by the first vehicle microwave transceiver carries warning signals in the form of modulations applied to the wave. The sensitivity to microwave warning signals of the second vehicle microwave transceiver is characterized by four sensitivity lobes with sensitivity maxima spaced equally in azimuth. Upon arrival at the second vehicle, the microwave warning signal broadcast by the first vehicle microwave transceiver causes a response in each of the four microwave elements in the antenna array of the second vehicle microwave transceiver that is proportional to the distance between the two vehicles and also to the angle of arrival of the microwave warning signal at the second vehicle microwave transceiver.
FIG. 5 illustrates the processes according to the invention whereby the multiple channel controller transforms a set of electronic warning signals provided by the microwave transceiver on separate electrical channels into analog or digital control signals for controlling a set of speakers to produce warning sounds.
DETAILED DESCRIPTION OF THE INVENTION
The invention relates to a vehicle-to-vehicle signaling device that uses an electronic warning signal impressed on a microwave frequency electromagnetic wave in order to provide two-way communications among vehicles. The signaling device allows vehicles to transmit and receive warning signals, and provides electronic control signals for controlling visible and audible warning indications to the drivers of the vehicles in response to the microwave warning signal.
FIG. 1 provides an overview of the signaling process. When the driver of a first vehicle wishes to signal the driver of a second vehicle, the driver of the first vehicle activates a switch, for example a horn button, which causes the microwave transceiver 1 in the first vehicle to broadcast a microwave warning signal in all directions in azimuth. A second vehicle located within a limited distance of the first vehicle receives the microwave warning signal by means of the microwave transceiver 2 . The microwave transceiver 2 in the second vehicle intercepts the microwave warning signal from the microwave transceiver 1 of the first vehicle and transforms it into a set of electronic warning signals on one or more electrical channels. The multiple channel controller 3 transforms the electronic warning signals provided by the microwave transceiver 2 into digital or analog control signals for controlling audible and visible warnings 4 . The control signals for the audible and visible warnings 4 are designed to give the driver of the second vehicle an intuitive impression of the directions and relative distances of all transmitting vehicles, including the first vehicle. The microwave warning signal broadcast by the microwave transceiver 1 is modulated within the microwave transceiver 1 and demodulated within the microwave transceiver 2 in such a way as to prevent random microwave signals in the environment from producing false electronic warning signals within the signaling device, following modulation techniques known in the art. In a preferred embodiment of the invention, the electronic warning signal is unique to a specific type of vehicle, for example to differentiate between ambulances and automobiles.
FIG. 2 provides details of the microwave transceiver, which consists of a waveform generator 5 , a modulator 6 , an amplifier 7 , an antenna 8 , an amplifier 9 , and a demodulator 10 . The waveform generator 5 produces an electronic warning signal according to known practices within the art, for example by changing the phase of a sinusoidal waveform at regular intervals according to a digital code. In a favorable embodiment, waveform generator 5 is designed to limit the duty cycle and the pulse repetition frequency of the electronic warning signal in order to prevent excessive transmissions from the microwave transceiver. A pulse repetition frequency of 2 Hertz and a duty cycle of 20% produces a 100 millisecond signal every half second, for example. In another favorable embodiment, waveform generator 5 generates an electronic warning signal that is unique to a specific type of vehicle, for example an automobile, a police car, or an ambulance. Modulator 6 impresses the electronic warning signal onto an electronic carrier signal, also according to known practices within the art. The amplifier 7 increases the power of the modulated electronic carrier signal, which is then converted into an electromagnetic wave and radiated by means of the antenna 8 . In a favorable embodiment of the invention, the antenna 8 is characterized by a single-frequency radiation pattern that is omni-directional in azimuth and limited in elevation to several degrees within the plane of the road. In another favorable embodiment, the antenna 8 is a cluster of four microwave transmit and receive elements arranged in such a way that each element's direction of maximum sensitivity to the microwave warning signal is separated from its nearest neighbors by 90 degrees in azimuth. In another favorable embodiment, the sensitivity of the antenna 8 to the microwave warning signal is characterized by four sensitivity maxima separated equally in azimuth by 90 degrees, with the first sensitivity maximum directed at 45 degrees from the driving direction of the vehicle, and the sensitivity is also characterized by an elevation coverage that extends from the road surface to approximately five degrees above the road surface. A microwave warning signal broadcast from a transmitting microwave transceiver is intercepted by the antenna 8 and converted by the antenna 8 into a set of modulated electronic carrier signals on one or more electrical channels. The modulated electronic carrier signal carried by one electrical channel is produced by one of the microwave elements in the antenna 8 in response to the microwave warning signals incident upon the microwave element. Thus, there is a unique one-to-one correspondence between one electrical channel and one of the microwave elements. The modulated electronic carrier signal on each electrical channel in the receiving microwave transceiver is amplified by means of the amplifier 9 and demodulated by means of the demodulator 10 to produce a replica of the electronic warning signal generated by the waveform generator 5 in the transmitting microwave transceiver. The electrical channels provided at the output of the demodulator 10 are processed by the multiple channel controller 3 into control signals that are suitable for controlling audible and visible warnings 4 .
FIG. 3 illustrates a preferred configuration of the microwave transmitting and receiving elements that make up the antenna. The antenna is constructed as an array of four microwave transmitting and receiving elements 11 , 12 , 13 , and 14 pointed in unique directions that are separated by 90 degrees in azimuth. For example, the microwave transmitting and receiving element 11 is pointed in a direction that is 45 degrees in azimuth from the driving direction of the vehicle in which it is mounted, element 12 is pointed in a direction that is 135 degrees in azimuth from the driving direction of the vehicle, element 13 is pointed in a direction that is 225 degrees in azimuth from the driving direction of the vehicle, and element 14 is pointed in a direction that is 315 degrees in azimuth from the driving direction of the vehicle. Each element responds to the microwave warning signal by producing an electronic warning signal on a single electrical channel. The element that is oriented in the direction that is closest to the direction of the origin of the microwave warning signal produces the strongest response. The remaining elements produce relatively weak responses to the microwave warning signal.
FIG. 4 illustrates the relative power in all directions in azimuth of the microwave warning signal broadcast by a first vehicle microwave transceiver 1 , and also the relative sensitivity to the microwave warning signal in all directions in azimuth of a second vehicle microwave transceiver 2 , using an example antenna constructed from four transmitting and receiving microwave elements. The relative sensitivity pattern shown for the second vehicle microwave transceiver 2 is achieved for example by means of a simple printed circuit device known in the art as a patch antenna, and it is characterized in this case by four sensitivity lobes that are equally spaced in azimuth. Each sensitivity lobe corresponds to one microwave element in the antenna array. The microwave warning signal broadcast by the first vehicle microwave transceiver 1 carries warning signals in the form of modulations applied to the wave. The microwave warning signal is broadcast with equal power in all directions in azimuth, and confined to a few degrees in elevation. The second vehicle microwave transceiver 2 receives the microwave warning signal in each of its four sensitivity lobes. The relative amplitude of the response in each lobe is determined by the point at which the line of sight between the two microwave transceivers 1 and 2 crosses the lobe, and also by the distance between the microwave transceivers. To provide a uniform power response in all directions in azimuth, the sensitivity lobes overlap in azimuth at the point where their power sensitivities drop to one half of the maximum sensitivity in each lobe. In this way, the amplitude of the response generated by the four sensitivity lobes taken together is always proportional to the distance between the two vehicles, and does not depend on the angle of arrival of the microwave warning signal.
FIG. 5 illustrates the processes according to the invention whereby a multiple channel controller 3 transforms electronic warning signals provided over multiple electrical channels by a microwave transceiver 2 into control signals that are suitable for controlling a set of audio speakers 15 , 16 , 17 , and 18 . The control signals are designed to control the audio speakers in such a way as to provide information about the directions and relative distances to the origins of microwave warning signals received by the microwave transceiver 2 . For example, a microwave warning signal that originates from a microwave transceiver that is close to the microwave transceiver 2 and in the direction of the top of the figure results in a high amplitude sound played over audio speakers 15 and 18 . A microwave warning signal that originates from a microwave transceiver that is far from the microwave transceiver 2 and in the direction of the right side of the figure results in a relatively lower amplitude sound played over audio speakers 15 and 16 . In a preferred embodiment of the invention, the multiple channel controller 3 produces control signals that are capable of reproducing a number of simultaneous sounds through the audio speakers, for example the sound of an automobile horn and the sound of an ambulance siren or the sound of a fire truck siren. An emergency vehicle may be fitted with a microwave transmitter that operates at an increased power level or with a predetermined modulation in order to cause the multiple channel controller 3 to control the audio speakers 15 , 16 , 17 , and 18 in a predetermined and easily recognized manner. Microwave transceivers mounted in different models of automobiles may be designed with unique waveform generators in order to cause the multiple channel controller 3 to control the audio speakers to replay model-specific horn noises, which would help the driver of the receiving vehicle to identify the transmitting vehicle. | A microwave vehicle-to-vehicle signaling device that converts microwave warning signals transmitted by a first vehicle into control signals in a second vehicle that are suitable for controlling audio devices or displays in such a way that the warning signals are perceived by the driver of a second vehicle to originate from the direction and distance of the first vehicle. Receiving vehicles located beyond the defined distance do not react to the warning messages due to the weakness of the signal. | 6 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a toner used for developing electrostatic latent images formed in electrophotography, electrostatic recording method, electrostatic printing method and the like, preferably in electrophotography.
[0003] 2. Discussion of the Related Art
[0004] In order to improve low-temperature fixing ability, which is one of the major problems to be solved in electrophotography, a toner comprising a resin binder comprising a crystalline polyester has been proposed (Japanese Examined Patent Publication No. Hei 5-44032, Japanese Examined Patent Publication No. Sho 62-39428 and the like). However, there is a problem in that the storage stability is lowered due to the plasticizing effect with the resin and various additives.
[0005] Therefore, the use of a crystalline polyester together with an amorphous polyester has been proposed (Japanese Patent Laid-Open No. 2001-222138 (U.S. Pat. No. 6,383,705) and Japanese Patent Laid-Open No. Hei 11-249339). Although the storage stability and the low-temperature fixing ability are found to be improved to some extent, there has been earnestly desired a toner which can give a higher-quality image without the image fogging.
[0006] An object of the present invention is to provide a toner which comprises a resin binder comprising a crystalline resin, the toner being excellent in the storage property and the low-temperature fixing ability, and giving a high-quality image without the image fogging.
[0007] These and other objects of the present invention will be apparent from the following description.
SUMMARY OF THE INVENTION
[0008] The present inventors have found that the storage stability of the toner comprising a crystalline resin is improved by external addition of a large amount of fine inorganic particles, and perfected the present invention.
[0009] Specifically, the present invention relates to a toner comprising:
[0010] a resin binder comprising a resin having a ratio of a softening point to a maximal peak temperature of heat of fusion of 0.6 or more and less than 1.1 (hereinafter referred to as “crystalline resin”);
[0011] a colorant; and
[0012] fine inorganic particles, the fine inorganic particles being externally added thereto,
[0013] wherein a coating ratio of the fine inorganic particles on a surface of the toner is 130 to 300%.
DETAILED DESCRIPTION OF THE INVENTION
[0014] One of the features of the toner of the present invention resides in that a large amount of fine inorganic particles are externally added to the surface of the toner. Generally, in a toner which does not contain a crystalline resin as a resin binder, when an external additive is added to excess, free fine inorganic particles are increased, so that the adhesion strength of the toner onto an adherend such as paper is lowered. As a result, not only the low-temperature fixing ability is worsened, but also the frictional force between the toner and the carrier or the like is also lowered, thereby causing image fogging. However, in the toner comprising a crystalline resin of the present invention, even when an external additive is added to excess, the low-temperature fixing ability and the image fogging are not adversely affected, and lowering in the storage property caused by a crystalline resin is suppressed. The reason why such effects of the present invention are exhibited is unclear. However, it is presumed that an appropriate adhesion strength to an adherend and an appropriate friction property between the toner and the carrier or the charging blade are maintained because there is a strong interaction between the crystalline resin and the fine inorganic particles, thereby suppressing freeing of an external additive, though the fine inorganic particles are adhered in two or more layers onto the whole surface or a part of the surface of the toner of the present invention.
[0015] It is preferable that the toner of the present invention further comprises a resin having a ratio of a softening point to a maximal peak temperature of heat of fusion of from 1.1 to 4.0 (hereinafter referred to as “amorphous resin”) as a resin binder.
[0016] The content of the crystalline resin is preferably from 1 to 40% by weight, more preferably from 5 to 35% by weight, especially preferably from 10 to 30% by weight, of the resin binder from the viewpoints of the storage property and the low-temperature fixing ability. In addition, the weight ratio of the crystalline resin to the amorphous resin, crystalline resin/amorphous resin, is preferably from 1/99 to 40/60, more preferably from 5/95 to 35/65, still more preferably from 10/90 to 30/70.
[0017] The crystalline resin includes crystalline polyesters, crystalline polyester-polyamides, crystalline styrene-acrylic resins, crystalline hybrid resins in which two or more resin components including at least one crystalline resin component are partially chemically bonded to each other, and the like. Among them, from the viewpoints of the fixing ability and the compatibility with the amorphous resin, the crystalline polyesters and the crystalline hybrid resins are preferable, and the crystalline polyesters are more preferable.
[0018] In the present invention, the crystalline polyester is preferably a resin obtained by polycondensing an alcohol component comprising 80% by mol or more of an aliphatic diol having 2 to 6 carbon atoms, preferably 4 to 6 carbon atoms, with a carboxylic acid component comprising 80% by mol or more of an aliphatic dicarboxylic acid compound having 2 to 8 carbon atoms, more preferably 4 to 6 carbon atoms, more preferably 4 carbon atoms.
[0019] The aliphatic diol having 2 to 6 carbon atoms includes ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, neopentyl glycol, 1,4-butenediol, and the like. Among them, α, ω-linear alkane diol is preferable, and 1,4-butanediol and 1,6-hexanediol are more preferable.
[0020] It is desirable that the aliphatic diols having 2 to 6 carbon atoms are contained in the alcohol component in an amount of 80% by mol or more, preferably from 85 to 100% by mol, more preferably from 90 to 100% by mol. Especially, it is desirable that one of the aliphatic diols constitutes 70% by mol or more, preferably 80% by mol or more, more preferably from 85 to 95% by mol of the alcohol component.
[0021] The alcohol component may comprise a polyhydric alcohol component other than the aliphatic diol having 2 to 6 carbon atoms. The polyhydric alcohol component includes dihydric aromatic alcohols such as alkylene(2 or 3 carbon atoms) oxide(average number of moles: 1 to 10) adducts of bisphenol A such as polyoxypropylene(2.2)-2,2-bis(4-hydroxyphenyl)propane and polyoxyethylene(2.2)-2,2-bis(4-hydroxyphenyl)propane; and trihydric or higher polyhydric alcohols such as glycerol, pentaerythritol and trimethylolpropane.
[0022] The aliphatic dicarboxylic acid compound having 2 to 8 carbon atoms includes oxalic acid, malonic acid, maleic acid, fumaric acid, citraconic acid, itaconic acid, glutaconic acid, succinic acid, adipic acid, acid anhydrides thereof, alkyl(1 to 3 carbon atoms) esters thereof, and the like. Among them, fumaric acid is preferable. Incidentally, as described above, the aliphatic dicarboxylic acid compound refers to aliphatic dicarboxylic acids, acid anhydrides thereof and alkyl(1 to 3 carbon atoms) esters thereof, among which the aliphatic dicarboxylic acids are preferable.
[0023] It is desirable that the aliphatic dicarboxylic acid compounds having 2 to 8 carbon atoms are contained in the carboxylic acid component in an amount of 80% by mol or more, preferably from 85 to 100% by mol, more preferably from 90 to 100% by mol. Especially, it is desirable that one of the aliphatic dicarboxylic acid compounds constitutes 60% by mol or more, preferably from 80 to 100% by mol, more preferably from 90 to 100% by mol, of the carboxylic acid component. Above all, it is desirable that fumaric acid constitutes preferably 60% by mol or more, more preferably from 70 to 100% by mol, especially preferably from 80 to 100% by mol, of the carboxylic acid component, from the viewpoint of the storage property of the crystalline polyester.
[0024] The carboxylic acid component may comprise a polycarboxylic acid component other than the aliphatic dicarboxylic acid compound having 2 to 8 carbon atoms. The polycarboxylic acid component includes aromatic dicarboxylic acids such as phthalic acid, isophthalic acid and terephthalic acid; aliphatic dicarboxylic acids such as sebacic acid, azelaic acid, n-dodecylsuccinic acid and n-dodecenylsuccinic acid; alicyclic dicarboxylic acids such as cyclohexanedicarboxylic acid; tricarboxylic or higher polycarboxylic acids such as 1,2,4-benzenetricarboxylic acid (trimellitic acid) and pyromellitic acid; acid anhydrides thereof, alkyl(1 to 3 carbon atoms) esters thereof, and the like.
[0025] The polycondensation of the alcohol component with the carboxylic acid component can be carried out, for instance, by the reaction at a temperature of from 120° to 230° C. in an inert gas atmosphere, using an esterification catalyst, a polymerization inhibitor and the like as occasion demands. Concretely, in order to enhance the strength of the resin, the entire monomers may be charged at once. Alternatively, in order to reduce the low-molecular weight components, divalent monomers are firstly reacted, and thereafter trivalent or higher polyvalent monomers are added and reacted. In addition, the reaction may be promoted by reducing the pressure of the reaction system in the second half of the polymerization.
[0026] Here, in the present invention, the term “crystalline” means that a ratio of the softening point to the maximum peak temperature of heat of fusion (softening point/maximum peak temperature of heat of fusion) is from 0.6 or more and less than 1.1, preferably from 0.9 or more and less than 1.1, more preferably from 0.98 to 1.05. Also, the term “amorphous” means that a ratio of the softening point to the maximum peak temperature of heat of fusion (softening point/maximum peak temperature of heat of fusion) is from 1.1 to 4.0, preferably from 1.5 to 3.0.
[0027] The crystalline polyester has a softening point of preferably from 85° to 150° C., more preferably from 90° to 140° C., especially preferably from 100° to 135° C. The crystalline polyester has a maximum peak temperature of heat of fusion of preferably from 77° to 166° C., more preferably from 82° to 155° C., especially preferably from 91° to 150° C.
[0028] Incidentally, in the case where the crystalline polyester comprises two or more resins, it is desirable that at least one of them, preferably all of them, is the crystalline polyester described above.
[0029] The crystalline hybrid resin is preferably a resin comprising a crystalline polyester resin component as a crystalline resin component. Incidentally, in the present invention, regardless of being crystalline or amorphous, the hybrid resin is preferably a resin obtained by mixing a mixture of raw material monomers for two polymerization resins each having an independent reaction path, preferably a mixture of raw material monomers for a condensation polymerization resin, especially preferably a polyester, and raw material monomers for an addition polymerization resin, especially preferably a vinyl resin, preferably with a monomer, as one of the raw material monomers, which is capable of reacting with both of the above raw material monomers for the above two polymerization resins (dually reactive monomer), for instance, (meth)acrylic acid, to carry out the two polymerization reactions. Here, in the case of the crystalline hybrid resin, raw material monomers for at least one crystalline resin, preferably raw material monomers for a crystalline polyester, are used during the preparation.
[0030] The amorphous resin includes amorphous polyesters, amorphous polyester-polyamides, amorphous styrene-acrylic resins, amorphous hybrid resins and the like. Among them, from the viewpoints of the fixing ability and the compatibility with the crystalline resin, the amorphous polyesters and the amorphous hybrid resins are preferable, and the amorphous polyesters are more preferable.
[0031] The raw material monomers for the amorphous polyester are exemplified by the same polyhydric alcohol component, and the same polycarboxylic acid component such as carboxylic acids, carboxylic acid anhydrides and esters of carboxylic acids, as in the raw material monomers for the crystalline polyester. The amorphous polyester is obtained by polycondensing these components.
[0032] Incidentally, it is preferable that the amorphous polyester is either one of the following resins:
[0033] 1) in a case where monomers for accelerating crystallization of a resin, such as an aliphatic diol having 2 to 6 carbon atoms and an aliphatic dicarboxylic compound having 2 to 8 carbon atoms, are used, a resin in which crystallization is suppressed by using two or more of these monomers in combination, in each of the alcohol component and the carboxylic acid component, at least one of these monomers is used in an amount of from 10 to 70% by mol, preferably 20 to 60% by mol of each component, and these monomers are used in two or more kinds, preferably two to four kinds; or
[0034] 2) a resin obtained from monomers for accelerating amorphousness of a resin, preferably an alkylene oxide adduct of bisphenol A as an alcohol component, or a substituted succinic acid of which substituent is an alkyl group or alkenyl group as a carboxylic acid component, wherein the monomers are contained in an amount of from 30 to 100% by mol, preferably from 50 to 100% by mol, of the alcohol component or the carboxylic acid component, preferably of the alcohol component and the carboxylic acid component, respectively.
[0035] The amorphous polyester can be prepared in the same manner as in the crystalline polyester.
[0036] The amorphous hybrid resin can be prepared in the same manner as in the crystalline hybrid resin except that raw material monomers for an amorphous resin are used as the raw material monomers.
[0037] The amorphous resin has a softening point of preferably from 80° to 170° C., more preferably from 90° to 130° C., especially preferably from 95° to 120° C. The amorphous resin has a maximum peak temperature of heat of fusion of preferably from 50° to 85° C., more preferably from 60° to 75° C., a glass transition point of preferably from 45° to 80° C., more preferably from 55° to 75° C., and a weight percentage of component insoluble to THF of preferably from 0 to 50% by weight. Incidentally, glass transition point is a property intrinsically owned by an amorphous resin, and is distinguished from the maximum peak temperature of heat of fusion.
[0038] Incidentally, in the case where the amorphous resin comprises two or more resins, it is desirable that at least one of them, preferably all of them, is the amorphous resin having the properties described above.
[0039] The content of the crystalline polyester is preferably from 1 to 40% by weight, more preferably from 5 to 35% by weight, especially preferably from 10 to 30% by weight, of the resin binder, from the viewpoints of the storage property and the low-temperature fixing ability. In addition, the weight ratio of the crystalline polyester to the amorphous resin, crystalline polyester/amorphous resin, is preferably from 1/99 to 40/60, more preferably from 5/95 to 35/65, still more preferably from 10/90 to 30/70.
[0040] As the colorants, all of the dyes, pigments and the like which are used as colorants for toners can be used, and the colorant includes black colorants such as carbon blacks and composite oxides of metals; colored colorants such as Phthalocyanine Blue, Permanent Brown FG, Brilliant Fast Scarlet, Pigment Green B, Rhodamine-B Base, Solvent Red 49, Solvent Red 146, Solvent Blue 35, quinacridone, carmine 6B, disazoyellow. These colorants can be used alone or in admixture of two or more kinds. In the present invention, the toner may be any of black toner, color toner and full-color toner. The content of the colorant is preferably from 1 to 40 parts by weight, more preferably from 3 to 10 parts by weight, based on 100 parts by weight of the resin binder.
[0041] The external additives include fine inorganic particles made of silica, alumina, titania, zirconia, tin oxide, zinc oxide or the like. Among them, it is preferable that silica having a small specific gravity is contained from the viewpoint of prevention of the embedment of the external additive.
[0042] The silica is preferably a hydrophobic silica which is previously hydrophobically treated, from the viewpoint of the stability in environmental resistance. The method of hydrophobic treatment of the silica is not particularly limited. The agent for hydrophobic treatment includes hexamethyldisilazane, dimethyldichlorosilane, silicone oil, methyltriethoxysilane, and the like. Among them, hexamethyldisilazane is preferable. It is preferable that the amount of the agent for hydrophobic treatment is from 1 to 7 mg/m 2 per surface area of the silica.
[0043] The fine inorganic particles have an average particle size of preferably from 6 to 200 nm, more preferably from 7 to 100 nm, especially preferably from 8 to 50 nm, from the viewpoints of the fluidity and the protection of the photoconductor and the like.
[0044] It is desirable that the coating ratio of the toner with the fine inorganic particles is from 130 to 300%, preferably from 150 to 250%, more preferably from 170 to 230%. When the coating ratio is too low, the storage property is lowered. On the other hand, when the coating ratio is too high, the fixing ability is lowered, thereby causing the image fogging.
[0045] In the present invention, the coating ratio (f) of the toner with the fine inorganic particles is calculated by the following equation:
f (%)={square root}3/2π×( D ·ρτ)/( d·ρs )× C× 100
[0046] wherein
[0047] d is an average particle size of fine inorganic particles;
[0048] D is a number-average particle size of an untreated toner; ρτ and ρs are a true specific gravity of an untreated toner and a true specific gravity of fine inorganic particles, respectively; and C is a weight ratio of fine inorganic particles to an untreated toner.
[0049] Incidentally, in the case where the fine inorganic particles comprise two or more kinds of fine inorganic particles having different average particle sizes, the coating ratio (f) of a toner as a whole is the sum of the coating ratios of the respective fine inorganic particles. For example, in the case where fine inorganic particles (1) and fine inorganic particles (2) are externally added, the coating ratio (f) of the toner as a whole is f 1 +f 2 wherein the coating ratios of the fine inorganic particles (1) and the fine inorganic particles (2) are f 1 and f 2 , respectively.
[0050] The content of the fine inorganic particles is appropriately determined based on the coating ratio of the toner. As one measure, the content is preferably from 0.7 to 5 parts by weight or so, more preferably from 1 to 3 parts by weight or so, especially preferably from 1.1 to 2.7 parts by weight or so, based on 100 parts by weight of the toner before external addition of fine inorganic particles (untreated toner).
[0051] Further, the toner of the present invention may appropriately contain an additive such as a charge control agent, a releasing agent, an electric conductivity modifier, an extender, a reinforcing filler such as a fibrous substance, an antioxidant, an anti-aging agent, a fluidity improver, and a cleanability improver.
[0052] The charge control agent includes positively chargeable charge control agents such as Nigrosine dyes, triphenylmethane-based dyes containing a tertiary amine as a side chain, quaternary ammonium salt compounds, polyamine resins and imidazole derivatives, and negatively chargeable charge control agents such as metal-containing azo dyes, copper phthalocyanine dyes, metal complexes of alkyl derivatives of salicylic acid and boron complexes of benzilic acid.
[0053] The releasing agent includes waxes such as natural ester waxes such as carnauba wax and rice wax; synthetic waxes such as polypropylene wax, polyethylene wax and Fischer-Tropsch wax; petroleum waxes such as montan wax, alcohol waxes. These waxes may be contained alone or in admixture of two or more kinds.
[0054] The toner in the present invention can be prepared by a surface treatment step comprising mixing an untreated toner with an external additive using a Henschel mixer or the like. The untreated toner is preferably a pulverized toner, and obtained by, for instance, homogeneously mixing a resin binder, a colorant and the like in a mixer such as a Henschel mixer or a ball-mill, thereafter melt-kneading with a closed kneader, a single-screw or twin-screw extruder, or the like, cooling, roughly pulverizing the resulting product using a hammer-mill, and further finely pulverizing with a fine pulverizer utilizing a jet stream or a mechanical pulverizer, and classifying the pulverized product to a given particle size with a classifier utilizing rotary stream or a classifier utilizing Coanda effect. The toner has a number-average particle size of preferably from 3 to 15 μm.
[0055] The toner of the present invention can be used alone as a developer, in a case where the fine magnetic material powder is contained. Alternatively, in a case where the fine magnetic material powder is not contained, the toner may be used as a nonmagnetic one-component developer, or the toner can be mixed with a carrier and used as a two-component developer.
EXAMPLES
Softening Point
[0056] Softening point refers to a temperature corresponding to ½ of the height (h) of the S-shaped curve showing the relationship between the downward movement of a plunger of flow tester (flow length) and temperature, namely, a temperature at which a half of the resin flows out, when measured by using a flow tester of the “koka” type (“CFT-500D,” commercially available from Shimadzu Corporation) in which a 1 g sample is extruded through a nozzle having a dice pore size of 1 mm and a length of 1 mm, while heating the sample so as to raise the temperature at a rate of 6° C./min and applying a load of 1.96 MPa thereto with the plunger.
Maximum Peak Temperature of Heat of Fusion and Glass Transition Point
[0057] The maximum peak temperature of heat of fusion is determined using a differential scanning calorimeter (“DSC Model 210,” commercially available from Seiko Instruments, Inc.), by raising its temperature to 200° C., cooling the hot sample from this temperature to 0° C. at a cooling rate of 10° C./min., and thereafter heating the sample so as to raise the temperature at a rate of 10° C./min. In addition, the glass transition point refers to the temperature of an intersection of the extension of the baseline of equal to or lower than the maximum peak temperature and the tangential line showing the maximum inclination between the kickoff of the peak and the top of the peak by the determination mentioned above.
Number-Average Particle Size of Toner
[0058] Measuring Apparatus: Coulter Multisizer II (commercially available from Beckman Coulter)
[0059] Aperture Diameter: 100 μm
[0060] Analyzing Software: Coulter Multisizer AccuComp Ver. 1.19 (commercially available from Beckman Coulter)
[0061] Electrolyte: Isotone II (commercially available from Beckman Coulter)
[0062] Dispersion: 5% electrolyte of EMULGEN 109P (commercially available from Kao Corporation, polyoxyethylene lauryl ether, HLB: 13.6)
[0063] Dispersing Conditions: Ten milligrams of a test sample is added to 5 ml of a dispersion, and the resulting mixture is dispersed in an ultrasonic disperser for 1 minute. Thereafter, 25 ml of an electrolyte is added to the dispersion, and the resulting mixture is dispersed in an ultrasonic dispersing apparatus for another 1 minute.
[0064] Measurement Conditions: One-hundred milliliters of an electrolyte and a dispersion are added to a beaker, and the particle sizes of the particles are determined for 20 seconds under the conditions for concentration satisfying that the determination for 30000 particles are completed in 20 seconds to obtain its number-average particle size.
Preparation Example of Crystalline Polyester
[0065] The raw material monomers as shown in Table 1 and 2 g of hydroquinone were reacted under nitrogen gas atmosphere at 160° C. for 5 hours. Thereafter, the temperature was raised to 200° C., and the ingredients were reacted for 1 hour, and further reacted at 8.3 kPa for 1 hour. The resulting resin is referred to as Resin a.
TABLE 1 Resin a 1,4-Butanediol 1013 g (90) 1,6-Hexanediol 143 g (10) Fumaric Acid 1450 g (100) Softening Point (° C.) 122.0 Maximum Peak Temperature (° C.) 124.6 of Heat of Fusion
Preparation Examples of Amorphous Resin
[0066] (i) The raw material monomers as shown in Table 2 and 4 g of dibutyltin oxide were reacted under nitrogen gas atmosphere at 220° C. for 8 hours. Thereafter, the ingredients were further reacted at 8.3 kPa until the desired softening point was reached. The resulting resin is referred to as Resin A.
[0067] (ii) The raw material monomers as shown in Table 2 and 4 g of dibutyltin oxide were reacted under nitrogen gas atmosphere, with raising the temperature from 180° to 210° C. for 8 hours. Thereafter, the ingredients were further reacted at 8.3 kPa until the desired softening point was reached. The resulting resin is referred to as Resin B.
TABLE 2 Resin A Resin B BPA-PO 1) 2000 g (41.8) BPA-EO 2) 800 g (18.0) Ethylene Glycol 400 g (19.5) Neopentyl Glycol 1200 g (34.9) Terephthalic Acid 600 g (26.5) 1900 g (34.6) Dodecenylsuccinic Anhydride 500 g (13.7) Trimellitic Anhydride 700 g (11.0) Softening Point (° C.) 150.0 143.2 Maximum Peak Temperature (° C.) 66.0 67.1 of Heat of Fusion Glass Transition Point (° C.) 62.3 64.9
Examples 1 to 6 and Comparative Examples 1 to 4
[0068] A resin binder, a colorant, a charge control agent and a releasing agent, as shown in Table 3, were sufficiently mixed together with a Henschel mixer. Thereafter, the mixture was melt-kneaded using a co-rotating twin-screw extruder (entire length of the kneading portion: 1560 mm; screw diameter: 42 mm; barrel inner diameter: 43 mm), with adjusting the rotational speed of the roller to 200 rpm, a heating temperature within the roller to 100° C., and a feeding rate of the mixture to 10 kg/h. The average residence time of the mixture was about 18 seconds. The resulting melt-kneaded product was cooled and roughly pulverized. Subsequently, the resulting product was pulverized with a jet mill and classified, to give an untreated toner having a number-average particle size of 7.5 μm.
[0069] An external additive as shown in Table 3 was added to 100 parts by weight of the resulting untreated toner, and mixed with a Henschel mixer, to give a toner.
Test Example 1
[0070] Four grams of a toner was placed in a 20-cc plastic-bottle (commercially available from K.K. Sanplatech), and allowed to stand, with the lid open, under environmental conditions of a temperature of 45° C. and a humidity of 60% for 72 hours. The extent of aggregation of the toner was visually examined, and the storage property was evaluated according to the following criteria. The results are shown in Table 3.
Evaluation Criteria
[0071] ⊚: No aggregation being observed;
[0072] ◯: Substantially no aggregation being observed;
[0073] Δ: Aggregation being observed; and
[0074] X: Entirely aggregated.
Test Example 2
[0075] Four parts by weight of a toner and 96 parts by weight of a silicon-coated ferrite carrier (commercially available from Kanto Denka Kogyo Co., Ltd., average particle size: 90 μm) were mixed for 10 minutes with a turbuler mixer, to give a developer. Next, the resulting developer was loaded in a modified apparatus of a copy machine “AR-505” (commercially available from Sharp Corporation). The development of fixed images was carried out, with sequentially raising the temperature of the fixing roller from 90° to 240° C. The image-bearing sheets used was “CopyBond SF-70 NA” (commercially available from Sharp Corporation, 75 g/m 2 ).
[0076] A sand-rubber eraser to which a load of 500 g was applied, the eraser having a bottom area of 15 mm×7.5 mm, was moved backward and forward five times over a fixed image obtained at each fixing temperature. The optical reflective density of the image before or after the eraser treatment was measured with a reflective densitometer “RD-915” manufactured by Macbeth Process Measurements Co. The temperature of the fixing roller at which the ratio of the optical density after the eraser treatment to the optical density before the eraser treatment initially exceeds 70% is defined as the lowest fixing temperature. The low-temperature fixing ability was evaluated according to the following evaluation criteria. The results are shown in Table 3.
Evaluation Criteria
[0077] ⊚: A lowest fixing temperature being lower than 130° C.;
[0078] ◯: A lowest fixing temperature being 130° C. or higher and lower than 150° C.; and
[0079] X: A lowest fixing temperature being 150° C. or higher.
Test Example 3
[0080] A developer was loaded in the same apparatus as in the Test Example 2, and solid images were printed out. Subsequently, blank sheet of paper was printed and fixed at 180° C. Lab determination was carried out using “MINOLTA DP-300” (commercially available form MINOLTA CO., LTD.) at a total of 5 points: one point in the middle of a sheet, two points 5 cm from top of the sheet and 5 cm from right and left edges, and two points 5 cm from bottom and 5 cm from right and left edges, to determine ΔE. The extent of generation of the image fogging was evaluated from the obtained value of ΔE according to the following evaluation criteria. The results are shown in Table 3.
Evaluation Criteria
[0081] ⊚: ΔE being less than 0.3;
[0082] ◯: ΔE being 0.3 or more and less than 0.6;
[0083] Δ: ΔE being 0.6 or more and less than 1.0; and
[0084] X: ΔE being 1.0 or more.
TABLE 3 Charge Coating Control Releasing External Ratio Storage Low-Temp. Image Resin Binder Colorant Agent Agent Additive (%) Property Fixing Ability Fogging Example 1 a/A = 20/80 MOGUL-L = 4 T-77 = 1 Carnauba = 1 TS-530 = 1.5 179 ⊚ ⊚ ⊚ 2 a/A = 20/80 ECB-301 = 4 LR-147 = 1 Carnauba = 1 TS-530 = 1.5 179 ⊚ ⊚ ⊚ 3 a/A = 20/80 MOGUL-L = 4 T-77 = 1 Carnauba = 1 TS-530 = 1.5 202 ⊚ ⊚ ⊚ NAX-50 = 1.0 4 a/B = 20/80 MOGUL-L = 4 T-77 = 1 Carnauba = 1 TS-530 = 1.5 179 ∘ ⊚ ⊚ 5 a/A = 20/80 MOGUL-L = 4 T-77 = 1 Carnauba = 1 TS-530 = 2.3 274 ⊚ ∘ ∘ 6 a/A = 20/80 MOGUL-L = 4 T-77 = 1 Carnauba = 1 TS-530 = 1.2 143 ∘ ⊚ ⊚ Comparative Example 1 a/A = 20/80 MOGUL-L = 4 T-77 = 1 Carnauba = 1 TS-530 = 0.5 60 x ⊚ ⊚ 2 a/A = 20/80 MOGUL-L = 4 T-77 = 1 Carnauba = 1 TS-530 = 0.9 107 Δ ⊚ ⊚ 3 a/A = 20/80 MOGUL-L = 4 T-77 = 1 Carnauba = 1 TS-530 = 3.0 357 ⊚ ∘ Δ 4 A = 100 MOGUL-L = 4 T-77 = 1 Carnauba = 1 TS-530 = 1.5 179 ⊚ x x
[0085] It is seen from the above results that the toners of Examples 1 to 6 exhibit an excellent low-temperature fixing ability without impairing the storage property, so that excellent fixed images can be obtained without the image fogging. On the other hand, in Comparative Examples 1 and 2 where the coating ratios with silica are too low, a plasticized crystalline polyester is likely to be exposed to the toner surface, so that the storage property is impaired, and in Comparative Example 3 where the coating ratio with silica is too high, the image fogging is generated due to the reduction in the triboelectric force. Also, in Comparative Example 4 where a crystalline polyester is not contained, the low-temperature fixing ability is poor and the image fogging is generated, nevertheless the coating ratio with silica is of the same level as those of Examples.
[0086] According to the present invention, there can be provided a toner which comprises a resin binder comprising a crystalline resin, the toner being excellent in the storage property and the low-temperature fixing ability, and giving a high-quality image without the image fogging.
[0087] The present invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the following claims. | A toner comprising a resin binder comprising a crystalline resin; a colorant; and fine inorganic particles, the fine inorganic particles being externally added thereto, wherein a coating ratio of the fine inorganic particles on a surface of the toner is 130 to 300%. The toner can be suitably used for developing electrostatic latent images formed in electrophotography, electrostatic recording method, electrostatic printing method and the like. | 6 |
BACKGROUND OF THE INVENTION
[0001] The term “waterjet” denotes high-speed water jets generated at high static pressures with special pumps and nozzles. Such waterjets perform a wide range of useful work such as cleaning tanks, ship hulls and various structures and also cutting alloys and composite materials with computer-controlled nozzle movement. Static pressures of water as high as 80,000 pounds per square inch (psi) are generated with special motor-driven or engine-driven piston pumps and special fluid-powered pressure intensifiers, and with nozzles equipped with gem orifices. The term “waterjet technology” describes the various processes and applications of waterjets. The term “abrasive waterjet” describes a particular waterjet technology in which selected industrial abrasive particulates are added into the jet stream with special nozzles to further enhance the capability of waterjets. Very hard and difficult materials are cut or removed with such abrasive waterjets. In fact, it is the only method that can now be used to cut carbon-fiber laminates that are widely used in modern aircrafts.
[0002] The pumps and pressure intensifiers known for generating waterjets are positive-displacement piston pumps which have multiple pistons and check valves to build up the potential energy of a fluid. The energy transfer from the piston to the fluid is usually not smooth, due to factors such as fluid compressibility, the finite number of pistons in the pump, and the phase limitations. As a result, there are pressure pulsations in the output fluid. For example, a triplex crankshaft pump has only three cylinders and pistons operating at about 600 rotations per minute (rpm) and a double-acting hydraulic pressure intensifier has only two cylinders and pistons operating at about one stroke per second. These pumps are used to push or build water pressures from atmospheric to 55,000 psi or higher. The output pressure of water at the outlet of each cylinder is not phased properly with the output pressure of other cylinders to cover the entire cycle and to provide smooth pressure output. The rough power output is similar to automobile engines where the power output of a 3-cylinder engine is rougher or not as smooth as the power output of an 8-cylinder engine. Thus, if a waterjet nozzle is placed at the outlet of a triplex pump or a double-acting intensifier, the waterjet will not form a smooth stream. Instead, the waterjet will form a pulsed jet with a stream of water slugs. The water slugs are phased according to the piston motion of the pump. For example, a triplex pump operating at 600 rpm would generate a pulsed waterjet of 3×600=1800 pulses per minute. A double-acting intensifier operating at one stroke per second would produce a pulsed waterjet of 60 pulses per minute.
[0003] However, in waterjet applications, nozzles are not positioned next to the pump. Tubes or hoses are used to transport the pressurized water from the pump to a remote or distant nozzle. Inside the tubes or hoses the pressure pulsations in the water is damped and only a portion remain at the nozzle. In many applications, the residue pressure pulsations present no problem but in double-acting intensifiers there may be a problem. Due to the very low stroke rate and the extreme pressures involved, water at the nozzle of an intensifier pump system may have pressure pulsations too high for applications such as abrasive waterjet cutting of composites. An additional pressure attenuator may be required to further damp out the pressure variations. In such applications, the smoothness of cut surface may be related to or a function of the pressure pulsation of the waterjet.
[0004] In many waterjet applications, a pulsed waterjet can be more effective than a continuous waterjet when each is at an identical pump power level. One reason is the mitigation of waterjet interference when a waterjet impacts a flat surface. When a continuous waterjet impacts a hard surface, the waterjet rebounds from the surface and collides with the incident waterjet. As a result, a significant portion of the waterjet energy is wasted. In a pulsed waterjet, the water slugs impact the surface individually and the energy of each slug of water has time to dissipate. If the waterjet slugs are phased properly, waterjet interference can be completely avoided. With a pulsed waterjet, the impact pressure on a surface can be greater if the mass of each water slug is greater. Reducing waterjet interference is one reason why waterjetting is widely applied today in industrial cleaning processes, such as by spinning a nozzle assembly at a high speed. Many waterjets generated at known pump pressures are supersonic, and it is difficult to avoid waterjet interference. Rotating a nozzle assembly at a high speed requires a rotating joint with good seals. The durability of such high-pressure seals is a maintenance issue in industrial processes. An impacting power of a waterjet is also reduced when the nozzle is rotating at a high speed.
[0005] There are many known investigations using pulsed waterjets for a wide range of jobs. One benefit of a pulsed waterjet is to remove materials, such as concrete, that have significant granular structures of materials. The waterjet pulses can better penetrate into pores of the porous structures, to rupture the structure and wash away the debris. Similar benefits of pulsed waterjet have been reported with coating removal. There are other benefits of using pulsed waterjets.
[0006] Even with the benefits of pulsed waterjets, the method is not applied widely today because the pulsed waterjet processes reported in several publications have not been commercialized. One highly publicized known pulsejet technology is not now commercialized, presumably because components involved in that particular pulsejet technology are not matured or there were technical difficulties not overcome. It is difficult to design an on-off valve for use with high-pressure water as the working fluid. To produce a pulsed waterjet at a nozzle is extremely difficult due to many factors. It is difficult to interrupt the flow of water at very high pressures.
[0007] Only some known pulsed waterjet processes are applied commercially, including one that uses an ultrasonic transducer placed at the tip of a waterjet nozzle to generate forced pulses at 20,000 cycles per second. Electrical energy is introduced into the nozzle assembly to generate the axial vibrations and forced waterjet pulses. Up to 1 kilowatt of electrical energy may be required to overcome the static water pressure at the nozzle. With this pulsed waterjet process it is possible to remove coatings at static pressures considerably lower than those associated with a conventional continuous waterjet. This 20 kHz pulsed waterjet process is not widely applied because of shortcomings and also the required electricity to power its nozzle. Mixing electricity and water in a handheld piece of field equipment is not a safe practice.
[0008] Pulsed waterjets are normally generated with available pumps. Once the pressure pulsations are dampened with tubes and hoses it can be difficult to recreate pressure pulsations at a waterjet nozzle. It is also difficult to interrupt the water flow at very high pressures. Problems, such as water hammer effect and metal fatigue, can occur if the flow interruption is not handled properly.
[0009] A process that allows a pulsed waterjet to be generated at a nozzle at a wide range of water pressures is valuable to the entire waterjet technology and would have applications in shipyards and concrete structure repairs and in everyday cleaning applications. It is particularly valuable if the process requires no energy from external or outside sources and requires no use of a heavy component with uncertain durability. This invention can be used to provide a waterjet process that produces a genuine pulsed waterjet by tapping a very small amount of water energy to produce waterjet pulses at a controllable frequency and at a wide range of static pressures. The apparatus and process of this invention will be valuable to waterjet technology and its use in industry.
SUMMARY OF THE INVENTION
[0010] This invention provides a method for generating a genuine pulsed fluid jet at a wide range of fluid pressures and flowrates without the need for an external power source or input and without the need for bulky, heavy, or unreliable equipment.
[0011] This invention can be used to generate a genuine pulsed fluid jet near or at a nozzle, to minimize the chance of pulsation dampening and to put the pulsejet to work.
[0012] This invention can incorporate the pulsejet technology into other mechanical and hydraulic systems to do useful work.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] This invention is explained in greater detail below in view of exemplary embodiments shown in the drawings, wherein:
[0014] FIG. 1 is a cross-sectional view of a pulsejet valve/nozzle, in a closed position, according to one embodiment of this invention;
[0015] FIG. 2 is a cross-sectional view of the pulsejet valve/nozzle, as shown in FIG. 1 , but in an open condition;
[0016] FIG. 3 is a cross-sectional view of a pulsing valve/nozzle assembly, in a closed condition, according to one embodiment of this invention;
[0017] FIG. 4 is a cross-sectional view of a pulsing valve/nozzle assembly, in an open condition, according to another embodiment of this invention;
[0018] FIG. 5 is a cross-sectional view of a pulsejet valve/nozzle assembly, in a closed condition, according to another embodiment of this invention;
[0019] FIG. 6 is a cross-sectional view, with a valve shuttle rotated 90 degrees, of the valve/nozzle assembly as shown in FIG. 5 , but in an open condition;
[0020] FIG. 7 is a cross-sectional view of a valve/nozzle assembly, in a closed condition, according to one embodiment of this invention;
[0021] FIG. 8 is a cross-sectional view of a pulsejet generator, in a closed condition, according to one embodiment of this invention; and
[0022] FIG. 9 is a cross-sectional view of a pulsejet generator, in an open condition, according to still another embodiment of this invention.
DETAILED DESCRIPTION OF THE INVENTION
[0023] This invention provides a method for generating pulsed fluid flow without using an external power source. The energy consumed in the process is derived from the potential energy contained in a pressurized fluid from a pressurized source. It is known that a pressurized fluid such as compressed air and pressurized water contains an enormous amount of energy introduced into the fluid during the pumping process. In this invention, a very small amount of fluid energy is taken from the pressurized fluid to generate flow discontinuities in a suitable valve so that the flow discontinuities become fluid jet pulses, particularly if a nozzle is placed downstream from the valve. The amount of energy consumed in generating the flow discontinuities is so relatively small that the fluid jet usefulness is not affected. Also, flow discontinuities do not normally cause a water hammer effect in the fluid system because the flow of fluid is not cut off completely.
[0024] In one embodiment of a pulsed fluid jet generator of this invention, such as shown in FIG. 1 , the pulsejet valve/nozzle 100 of this invention comprises a nozzle body 101 having a fluid inlet 102 , a fluid outlet 103 , and a cylindrical cavity 104 in communication with the inlet 102 and the outlet 103 . Inside the cavity 104 , a generally cylindrical valve poppet 105 has a tapered end 106 in contact with an outlet port 107 of the fluid outlet 103 and an other cylindrical end 108 accommodates a compression spring 109 that abuts the valve poppet 105 in one end and abuts a valve plug 110 on the other end. The valve poppet 105 has a central fluid passage 111 . The valve poppet 105 divides the valve cavity 104 into two parts, an upper cavity 112 and a lower cavity 113 . A poppet seal 114 can prevent fluid leakage across the valve poppet 105 although the valve poppet 105 is sized to fit the valve cavity 104 snugly, but is also free to slide up and down.
[0025] Still referring to FIG. 1 , in some embodiments, the valve/nozzle assembly 100 of this invention is assembled with the valve poppet 105 in an upright position, relative to the direction shown in FIG. 1 , and the spring 109 is compressed to exert a force on the valve poppet 105 urging it to butt against or abut the outlet port 107 , thus closing the valve/nozzle 100 . If fluid flows into this valve assembly, it will fill the lower cavity 113 but will be stopped by the valve poppet 105 , from being discharged through the outlet 103 . In some embodiments of this invention, the valve poppet 105 has a diameter D 1 and a cross-sectional area A 1 . The tapered end 106 contacts the outlet port 107 to form a contact or a seal circle, or a ring, of a diameter D 2 and of a cross-sectional area A 2 . Thus, in some embodiments, the valve poppet 105 has a donut-shaped cross-sectional area A 1 −A 2 =ΔA exposed to the fluid in the lower cavity 113 . If the fluid is pressurized to a value of Pf psi, then the fluid exerts a fluid-induced force Ff of P×ΔA pounds of force against the valve poppet 105 in lifting it. At the same time, the spring 109 exerts a spring force Fs on the valve poppet 105 to keep it down. If Fs is greater than Ff, then the valve poppet 105 will stay in place and the valve remains closed. On the other hand, if Ff is greater than Fs, then the valve poppet 105 is pushed up by the pressurized fluid, thus opening the outlet port 107 . The fluid will then flow from the inlet 102 through the lower cavity 113 to the outlet 103 . At the same time, the fluid will also flow through the fluid passage 111 of the valve poppet 105 into the upper cavity 112 . As a result, the pressurized fluid will be on both ends of the valve poppet 105 and the poppet lifting force Ff is eliminated or goes to zero. Here, the valve poppet 105 feels only the force from the spring 109 and thus moves down to close the outlet port 107 , thus returning the valve assembly 100 back to its earlier state and completing one cycle of its pulsing action. This cyclic motion can continue automatically as long as the pressurized fluid supply continues. The fluid flow out of the valve assembly 100 will be chopped and if a nozzle 115 is placed at the outlet 103 , a pulsed fluid jet will be formed, such as shown in FIG. 2 .
[0026] One example can be used to further explain the valve assembly 100 of this invention. If the valve poppet 105 has a diameter of 0.5 inches, then its cross-sectional area inside the cavity 104 is 0.196 square inches. If the tapered end 106 of the valve poppet 105 contacts the outlet port 107 with a seal ring of 0.312 inches, a cross-sectional area of 0.076 square inches, then the cross-sectional area of the valve poppet 105 exposed to the fluid inside the lower cavity 113 when the valve is closed is ΔA=0.196−0.076=0.120 square inches. If the spring 109 exerts a force of 20 pounds on the valve poppet 105 , then the outlet port 107 will be closed by this force. If a fluid such as water enters into the valve assembly 100 , for example at 100 psi, then the valve will not open because the fluid induced force Ff=100×0.120=12 pounds force, which is smaller than the spring force of 20 pounds. However, if the fluid pressure is increased to 200 psi, the fluid force on the valve poppet 105 will be increased to 24 pounds, which is greater than the spring force 20 pounds, and the valve poppet 105 will move up to open the outlet port 107 . This 200-psi pressurized water will then flow out of the valve assembly 100 but will also flow into the upper cavity 112 to balance the pressure across the valve poppet 105 . The 4 pound force differential is eliminated or goes to zero, and the valve poppet 105 then moves down to close the outlet port 107 . This cyclic motion can continue automatically as long as the force differential is significant and there is no appreciable fluid leakage across the valve poppet 105 with the valve in a closed condition. A pulsed waterjet can be generated at the nozzle 115 . The frequency of this cyclic fluid motion is a function of the flow rate of the fluid and the size of the valve cavity. The fluid pressure determines if the valve will function but will not affect the cyclic frequency. The opening of the nozzle is one parameter that determines the flow rate at a given pressure. Because the spring 109 is compressed by the fluid during each cycle of valve operation, energy is consumed and lost in the form of heat.
[0027] The use of the compression spring 109 in the valve assembly 100 of this invention has limitations. Because a spring or bias element can fatigue and fail, the spring can supply only a relatively limited force. A spring of 20 pound compression force is considered to be a relatively strong spring and is classified commonly as a die spring but can only handle fluid of relatively low pressures. At relatively high fluid pressures, the fluid pressure inside the lower cavity 113 usually does not diminish much and the spring 109 may not return the valve poppet 105 to its closed position to complete a clean cycle or a complete cycle. Thus, the valve poppet 105 may get hung up to create a leak or a leaking valve. In some embodiments, eliminating the spring 109 results in a suitable force from the fluid.
[0028] An improved pulsing valve/nozzle assembly 200 of this invention is shown in FIG. 3 . The valve assembly 200 comprises a valve body 201 having a fluid inlet 202 , a fluid outlet 203 , an upper cavity 212 and a lower cavity 213 connected by a passage 210 . A valve poppet 205 has a shoulder 206 and a central fluid passage 211 . The valve poppet 205 straddles across the upper cavity 212 and the lower cavity 213 through the passage 210 . The valve poppet 205 has a tapered end 208 situated or positioned in the lower cavity 213 and the shoulder 206 in the upper cavity 212 . There is a seal/bushing 214 around the valve poppet 205 in the upper cavity 212 that fits snugly against a cavity wall and around the valve poppet 205 to prevent fluid from leaking across the shoulder 206 . The seal/bushing 214 and the shoulder 206 divide the cavity to an upper cavity 212 and a lower cavity 216 . The lower cavity 216 has a small bleed hole 217 in communication with the outside environment. The valve poppet 205 is free to slide across the passage 210 for a short distance. The valve poppet 205 has a diameter D 1 and a cross-sectional area A 1 in the lower cavity 213 and a seal ring of diameter D 2 and a cross-sectional area A 2 when the valve poppet 205 is in contact with the outlet port 207 . The valve poppet 205 and the seal/bushing 214 in the upper cavity 212 define a diameter D 3 and a cross-sectional area A 3 . A spacer spring 209 can be inserted into the upper cavity 212 to keep the seal/bushing 214 in place and to urge the valve poppet 205 down, relative to the orientation shown in FIG. 3 when there is no fluid inside the valve/nozzle assembly 200 . In some embodiments of this invention, D 3 is greater than D 2 and D 1 , and is much greater than D 1 −D 2 . In some embodiments of this invention, there can be a seal/bushing 218 and the spring spacer 219 in the lower cavity 213 serving a purpose similar to that of the seal/bushing 214 and the spacer spring 209 in the upper cavity 212 . Any suitable nozzle 215 in the outlet 203 can be used to generate fluid jets.
[0029] As shown in FIG. 3 , when a fluid of pressure P enters into the lower cavity 213 , it encounters the surface A 1 −A 2 and quickly exerts a force of Ff=P(A 1 −A 2 ) to lift the valve poppet 205 up from the valve port 207 . Once lifted, the entire cross-sectional area of the valve poppet 205 is exposed to the fluid. Thus a force of Ff=PA 1 is exerted on the valve poppet 205 and pushes it to an uppermost position. Thus, the valve port 207 is wide open and the fluid flows through the outlet 203 and the nozzle 215 . At the same time, the fluid flows into the upper cavity 212 through the fluid passage 211 and encounters the cross-sectional area A 3 and exerts a force of Ff=P·A 3 to push the valve poppet 205 down. Because the lower cavity 216 below the shoulder 206 is exposed to an atmosphere, there is a net downward force of P(A 3 −A 1 ) to push the valve poppet 205 down. This force is very significant if D 1 and D 3 are relatively far apart. Because of this downward force, the valve poppet 205 will move down to close the outlet port 207 and thus complete one cycle of its up-and-down motion. This motion will continue as long as pressurized fluid continues to flow. A pulsed fluid jet can be generated at the nozzle 215 .
[0030] Another embodiment of a pulsejet valve/nozzle of this invention is shown in FIG. 4 . In this embodiment, the seal/bushing assemblies are eliminated. The valve poppet 305 sits inside the upper cavity 312 and the passage 310 with a snug fit to minimize fluid leakage. A small fluid leakage rate may not affect the function of this valve/nozzle assembly and can actually lubricate and thus assist the motion of the valve poppet 305 . One advantage of the valve/nozzle assembly 300 is its simple design. In some embodiments, one design requirement is that D 3 be greater than D 1 by a certain margin, which can be a function of the fluid pressure P and the sizing of the outlet port 307 .
[0031] Another embodiment of a pulsejet valve/nozzle assembly of this invention is shown in FIG. 5 . The valve/nozzle assembly 400 has an inline arrangement wherein a fluid flows into the valve body 401 from an upper inlet 402 into the upper cavity 412 , through the fluid passage 411 , and into the lower cavity 413 . The valve poppet 405 straddles the upper cavity 412 and the lower cavity 413 through the passage 410 . The valve poppet 405 has a tapered inlet end 409 and a tapered outlet end 408 . The valve poppet 405 has a side inlet port 420 situated or positioned in the upper cavity 412 and the side outlet port 419 situated or positioned in the lower cavity 413 . The inlet port 420 and the outlet port 419 are connected by the passage 411 . The tapered inlet end 409 mates with valve inlet port 414 and the tapered outlet end 408 mates with the valve outlet port 407 . The valve poppet 405 has a shoulder 406 that fits sealably or snugly inside the lower cavity 413 . The valve poppet 405 is free to slide up and down between the inlet port 414 and the outlet port 407 .
[0032] Referring to FIG. 6 , when a pressurized fluid enters into the valve/nozzle assembly 400 through the inlet 402 , it pushes down the valve poppet 405 and enters into the upper cavity 412 and into the side ports 420 . The fluid then flows through the passage 411 and enters the lower cavity 413 through the side port 419 . At this moment, the valve poppet 405 is down and the tapered outlet end 408 seals the outlet port 407 with a fluid induced force Ff=PA 1 , where A 1 is a cross-sectional area of the valve poppet 405 in the upper cavity 412 . The fluid of pressure P in the lower cavity 413 quickly sees the cross-sectional area of the poppet shoulder 406 and exerts a lifting force of a magnitude of P(A 3 −A 1 ), where A 1 is the cross-sectional area of the valve poppet 405 inside the lower cavity 413 . This lifting force cancels the downward force P·A 1 in the upper cavity 412 . As a result, the valve poppet 405 moves up and opens the outlet port 407 and closes the inlet port 414 . Simultaneously, the fluid inside the lower cavity 413 flows out of the nozzle 415 . As the fluid pressure inside the lower cavity 413 diminishes, the lifting force on the valve poppet 405 is reduced to a level of less than the downward force inside the upper cavity 412 , and the valve poppet 405 moves down to close the outlet port 407 and thus completes one cycle of the poppet movement. As long as the pressurized fluid flow continues, a pulsed fluid jet will be generated at the nozzle 415 . Fluid flow may be interrupted inside the valve/nozzle assembly 400 but will not be blocked completely. Thus, there will be no water hammer effect in the fluid system. This inline pulsejet valve/nozzle assembly 400 of this invention has one advantage of a relatively slim construction and a simple or logical flow pattern ideally, which is suited for use with handheld tools.
[0033] Another embodiment of a pulsejet valve/nozzle assembly 500 is shown in FIG. 7 , and comprises a valve body 501 having an inlet 502 , a cylindrical cavity 504 containing a valve cartridge 510 , and an outlet 503 with a nozzle 514 . The valve cartridge 510 connects the inlet 502 to the outlet 503 in a fluid tight manner. The valve cartridge 510 can have a cylindrical shape and can contain a flow modulating mechanism, such as discussed in this specification. The valve cartridge 510 has an inlet 521 , an inlet cavity 512 , a poppet 505 , an outlet cavity 513 , and an outlet 522 . The valve poppet 505 has an inlet side port 519 , a central fluid passage 511 , an outlet side port 520 , and tapered ends to mate with the inlet 502 and outlet 503 of the valve cartridge 510 . The valve cartridge 510 has a side bleed hole 517 connecting the cavity 516 inside the valve cartridge 510 to an outer atmosphere or the outside. When a pressurized fluid enters into the valve/nozzle assembly 500 of this invention, it flows into the valve cartridge 510 in which its flow is modulated by movement of the valve poppet 505 and the fluid can flow out of the nozzle 514 in the form of a pulsed jet. This cartridge arrangement can simplify the maintenance as the valve poppet 505 and its contact surfaces are subject to wear and the fluid leakage becomes too excessive. It is then the time for maintenance to replace the valve cartridge 510 . This cartridge arrangement can also provide a cartridge having one of various lengths to be used inside the same nozzle body so that various flow modulation frequencies can be used.
[0034] In some fluid jet applications, a mass of each fluid jet pulse needs to be substantial so that the pulse frequency can be reduced, which relates to the so-called water cannon technology, particularly when the fluid is water. The water cannon technology is known and characterized by the high power of the fluid pulses that can cause significant damage when impacting a surface. This capability can be useful in many geotechnical applications. This invention can provide the necessary technology to meet the needs of water cannons.
[0035] Referring to FIG. 8 , a pulsejet generator 600 of this invention comprises a gas accumulator cylinder 621 connected to one end of a valve inlet head 627 . The other end of the valve inlet head 627 is connected to a valve cylinder 601 . The valve inlet head 627 has an inlet cavity 611 with a tapered inlet port 613 in communication with a valve inlet 602 . The inlet cavity 611 has a tapered inlet port 613 connected to the valve inlet 602 and a central hole 615 that accommodates a cylindrical valve shuttle 605 . The valve shuttle 605 has a tapered inlet end 606 that is mateable with the inlet port 613 . The inlet cavity 611 has a seal 616 around the valve shuttle 605 to minimize fluid leakage. The valve cylinder 601 has a floating piston 617 that straddles around the valve shuttle 605 through a center hole 618 . The piston 617 has an outside diameter seal 619 and an inside diameter seal 620 to isolate or separate the fluids. The valve shuttle 605 has a side inlet port 608 inside the inlet cavity 611 , a central fluid passage 610 , and an outlet side port 609 inside the outlet cavity 612 . The valve shuttle 605 has an upper catch 623 in a gas cavity 604 on top of a piston 617 and a lower catch 624 in the outlet cavity 612 and below the piston 617 . The two catches 623 and 624 on the valve shuttle 605 define a distance that the valve shuttle 605 can travel. The gas cylinder 621 has a gas cavity 622 connected to the gas cavity 604 by the passage 625 drilled through the valve inlet head 627 . When the gas cylinder 621 is filled with a gas such as nitrogen or air to a pressure Pg, the gas will flow into the gas cavity 604 and will push the piston 617 down against the valve shuttle catch 624 and will move the shuttle 605 down to close the outlet port 614 . The outlet port 614 is tapered to mate with the tapered outlet end 607 of the valve shuttle 605 . As a result, the outlet port 614 can be closed by the valve shuttle 605 under a downward force exerted on the valve shuttle 605 in the cavity 611 . The gas pressure Pg can be selected based on characteristics of the system fluid and the intended application. In different embodiments of this invention, Pg is smaller than the pressure of the system fluid entering into the pulsejet generator 600 .
[0036] As a system fluid of pressure Pf flows into the inlet cavity 611 through the inlet 602 , the fluid can follow the side inlet port 608 , the passage 610 and the side outlet port 609 of the valve shuttle 605 and can enter into the cavity 612 . Once in the cavity 612 , the fluid encounters the closed outlet port 614 which it cannot open because of the fluid seating force in the cavity 611 . The fluid also encounters the piston 617 and pushes it upward. By design, the gas pressure in the cavity 604 is lower than the fluid pressure in the cavity 612 . Thus, the piston 617 can rise and eventually engage the catch 623 on the valve shuttle 605 . Now, the valve shuttle 605 can rise if the gas pressure in the cavity 604 is lower than the fluid pressure in the cavity 612 . The outlet port 614 can thus open and allow the system fluid to flow out or discharge. Now, the system fluid encounters the entire cross-sectional area of the outlet end 607 and pushes it up to keep the inlet port 613 closed until the fluid loses pressure. The piston 617 can move down with the fluid and engage the lower catch 624 to move the valve shuttle 605 down to the closed outlet port 614 . Thus, the valve shuttle 605 and the piston 617 complete one cycle of their movement. When the flow of pressurized system fluid continues, a pulsed fluid jet can be generated at the nozzle 626 . The cyclic movement of the piston 617 determines the frequency of the pulsejet and the volume of system fluid swept by the piston 617 determines the mass of each pulse. The gas pressure inside the gas cavity 604 can vary during each cycle because the gas is compressing and expanding but remains below that of the system fluid, otherwise the cyclic movement cannot continue. As a result, the pulsejet generated at the nozzle 626 varies in energy content in each slug of fluid, higher at the start of slug and lower at the end. The presence of a gas accumulator allows the use of a large nozzle to generate a pulsejet of high impact energy. If the gas accumulator is replaced with a strong spring, the ability to store energy can be limited and the operation may not be smooth.
[0037] In known waterjet operations, the water pressure often exceeds 10,000 psi, which is substantially higher than the gas pressure commonly employed in gas accumulator practices because gas at such high pressure becomes very dangerous and difficult to handle. To accommodate water at very high pressures, the gas accumulator used in the pulsejet generator 600 of this invention can be replaced with a gas pressure intensifier by incorporating a piston-plunger setup into the pulsejet valve/nozzle assembly of this invention. As a result, there is another embodiment of a pulsejet generator 700 of this invention, capable of handling system fluid of very high pressures. With this gas intensifier, a gas can be used to store energy at manageable pressures to accommodate water at pressures above 40,000 psi. Water, due to its non-compressible nature, is easier to handle than a gas at 4,000 psi.
[0038] Referring to FIG. 9 , the pulsejet generator 700 of this invention comprises a gas cylinder 726 with a gas chamber 731 , a gas piston 727 housed in the gas chamber 731 with an associated piston seal 728 , a hollow valve cylinder 701 attached to the gas cylinder 726 on one end, a hollow plunger 722 attached to the gas piston 727 on one end which has an end cap 718 at the other end, a valve inlet head 715 situated inside the valve plunger 722 , a fluid supply tube 725 in the center of the gas chamber 732 connecting an outside valve inlet 702 to the valve inlet head 715 through a center hole 729 on the gas piston 727 , a cylindrical valve shuttle 705 straddling across the end cap 718 , and a valve outlet 703 attached to the other end of the valve cylinder 701 . The valve inlet head 715 has an inlet cavity 711 with a tapered inlet port 713 connected to the valve inlet 702 . The inlet cavity 711 has a central hole 716 to accommodate the inlet end 706 of the valve shuttle 705 and a seal 717 around the valve shuttle 705 to prevent fluid leakage. The inlet end 706 is tapered to mate with the inlet port 713 . The plunger end cap 718 has a center hole 719 to accommodate the valve shuttle 705 and has an outside diameter seal 720 and an inside diameter seal 721 to prevent fluid leakage. The plunger end cap 718 defines the outlet cavity 712 and the plunger cavity 730 , which is connected to the atmosphere through a bleed 734 on the hollow plunger 722 and on the gas cylinder 726 . The valve shuttle 705 has a tapered outlet end 707 situated or positioned in the outlet cavity 712 . The inlet end 706 has a side inlet port 708 situated or positioned in inlet cavity 711 , an outlet side port 709 on the outlet end 707 in the outlet cavity 712 , and an internal fluid passage 710 connecting the two side ports. The valve shuttle 705 comprises an upper catch 723 situated or positioned in the plunger cavity 730 and a lower catch 724 situated or positioned in the outlet cavity 712 . The plunger end cap 718 can slide along the valve shuttle 705 between the two catches 723 and 724 . A cushion spring may be placed between the plunger end cap 718 and the lower catch 724 to soften the contact.
[0039] Still referring to FIG. 9 , the pulsejet generator 700 can be filled with a gas such as nitrogen or air in the gas chamber 731 to a pressure Pg, which can be determined by the pressure of the system fluid involved. The gas can push down the gas piston 727 and the plunger 722 , and the plunger end cap 718 will then push down the valve shuttle 705 to close the outlet port 714 . The pulsejet generator 700 can now be used to generate pulsed fluid jets.
[0040] When a pressurized system fluid, such as water, enters in the pulsejet generator 700 through the inlet 702 at a pressure Pw, it flows into the inlet cavity 711 through the supply tube 725 . In the cavity 711 , it exerts a force on the inlet end 706 of the valve shuttle 705 to push it down while the fluid flows through the valve shuttle 705 into the outlet cavity 712 . In the outlet cavity 712 , water sees or encounters the closed outlet port 714 and cannot open it. Instead, the water pushes the end cap 718 of the plunger 722 against the gas force acting on the piston 727 . If the water force is greater than the gas force, then the plunger end cap 718 rises along the seated valve shuttle 705 . Eventually, the plunger end cap 718 engages the upper catch 723 . At this point, if the water force pushing up the plunger end cap 718 is still greater than the gas force acting-on the piston 727 , then the valve shuttle 705 can be moved or dislodged from the outlet port 714 and water can flow into the valve outlet 703 and discharge at the nozzle 736 . At this time, water in the outlet cavity 712 sees the entire cross-sectional area of the outlet end 709 of the valve shuttle 705 and thus exerts a force pushing it upward to close the inlet port 713 of the valve inlet head 715 until water pressure inside the cavity 712 is reduced to a lower level. Once the outlet port 714 is open, the plunger end cap 718 can move down with the water and eventually engage the lower catch 724 and push down the valve shuttle 705 to close the outlet port 714 . Thus, the valve shuttle 705 and the plunger 722 complete one cycle of their up-and-down movement. If the water supply is continued, the pulsed waterjet can be produced at the nozzle 736 . A time period required to complete this cycle determines a frequency of the pulsed waterjet. The water pressure and the intensification ratio of the intensifier determine the energy content of the waterjet pulses. The intensification ratio is determined by the effective cross-sectional area of the gas piston 727 and the effective cross-sectional area of the plunger end cap 719 . If this ratio is 20 and the gas pressure inside the gas chamber 731 is 2000 psi, the pulsejet generator 700 can handle water at pressures above 40,000 psi. The total volume of the gas chamber 731 can affect the amount of water energy that can be stored during each pulse. Thus, the energy content of each waterjet pulse can also be affected by the gas volume. The larger the gas chamber 731 , the flatter can be the energy profile of a waterjet pulse. Greater energy in waterjet pulses often relates to greater power in doing work.
Example 1
[0041] To better illustrate this invention, a pulse valve/nozzle 200 was constructed according to the embodiment shown in FIG. 3 . The valve/nozzle 200 had a rectangular body 201 made of stainless steel with a side fluid inlet 202 of 0.156 inches in diameter, a cylindrical cavity 212 and 213 of 0.500 inches in diameter, and a bottom fluid outlet 203 of 0.156 inches in diameter. Attached to fluid outlet 203 was a nozzle 215 having a replaceable orifice. A valve shuttle 205 with the shoulder 206 was constructed of stainless steel and placed inside the upper cavity 212 with the seal/bushing 214 and 218 . The valve shuttle 205 had a diameter of 0.312 inches and the shoulder 206 had a diameter of 0.498 inches. The seal/bushing 214 and 218 were made of brass disks and polymer packed in a sandwich form and fit the valve shuttle 205 and the cavities 212 and 213 snugly but otherwise the valve shuttle 205 was free to slide. A side bleed hole 0.047 inches in diameter was drilled on the side of valve/nozzle body 201 , as shown in FIG. 3 . The valve/nozzle body 201 was 2 inches wide, 3.7 inches long, and 1 inch thick. The valve shuttle 205 was 2 inches long with the shoulder 206 of 0.1 inches thick and the tapered outlet end 208 of 60 degrees, and had a central fluid passage 211 of 0.125 inches in diameter. The outlet port 207 had a taper of 59 degrees and a contact ring of 0.250 inches in diameter was formed when the valve shuttle 205 made contact with the valve port 207 . Thus, a differential cross-sectional area of the valve shuttle 205 and the contact ring was 0.0764−0.0591=0.0273 square inches, which is the surface that fluid inside cavity 213 encountered while exerting an upward lifting force on the valve shuttle 205 . When 70 psi tap water was introduced into the lower cavity 213 , for example, a lifting force of about 2 pounds was produced. When constructed, the pulsejet valve/nozzle 200 was closed because of the compression spring 209 inside the upper cavity 212 . The spring 209 was relatively light, exerting an estimated force of less than 0.1 pound on the valve shuttle 205 .
[0042] The valve/nozzle 200 was tested with 70-psi tap water. When the water was introduced into the inlet 202 , a pulsed waterjet was issued or discharged at the nozzle 215 , immediately. The nozzle 215 was inserted with a sapphire orifice of 0.052 inches in diameter. The oscillation of the valve shuttle 205 inside the valve body 201 could be felt and heard but the waterjet pulses were not clearly visible with naked eyes. The pulses were bunched too closely due to the high pulsating frequency, which was estimated at 100 cycles per second. However, photographing this pulsejet with a digital camera clearly revealed the water pulses.
Example 2
[0043] A pulsejet generator was constructed according to the embodiment shown in FIG. 8 . The pulsejet generator 600 was constructed with 1¼-inch Schedule-40 PVC pipe rated for pressures up to 370 psi, and with pipe components such as a tee, an elbow and end caps. A PVC tee was used as the centerpiece of the pulsejet generator 600 . On one end of the tee was the gas accumulator 621 which was made of a 5-inch long section of PVC pipe and a cap and the other end was the valve cylinder 601 made of a 6-inch-long PVC pipe, an end plug, and a cap. The overall length of the assembled accumulator/valve cylinder combination was about 15 inches. A fluid inlet head 627 made of stainless steel was positioned in the center of the tee and had a fluid passage connected to the fluid inlet 602 . The inlet head 627 had a fluid inlet cavity 611 and a tapered inlet port 613 that mated with the tapered inlet end 606 of the valve shuttle 605 . The valve shuttle 605 was made of stainless steel and was 0.500 inches in diameter, 5 inches in length, and was machined to have the upper catch 623 and the lower catch 624 of 0.063 inches in height and 0.010 inches in thickness. The valve shuttle 605 had ends with a 60-degree taper and had the inlet side port 608 and the outlet side port 609 connected by an internal fluid passage 610 . The side ports were 0.125 inches in diameter and the fluid passage 610 was 0.250 inches in diameter. Generator 600 had a gas piston 617 straddling around the valve shuttle 605 between the catch 623 and the catch 624 . The gas piston 617 had an outside diameter of 1.312 inches and a center hole of 0.500 inches in diameter and was fitted with an outside diameter seal 619 and an inside diameter seal 620 around the valve shuttle 605 , and could travel a maximum distance of 3.0 inches between the catch 623 and the catch 624 . The volume of space swept by the gas piston 617 during its maximum travel was 3.3 cubic inches. The gas piston 617 divided the valve cylinder interior space into two parts, an upper gas cavity 604 and a lower outlet cavity 612 . The gas in the accumulator 622 could flow into the gas cavity 604 by the passage 625 drilled through the inlet head 627 . The valve shuttle 605 straddled across three cavities, the inlet cavity 611 , the gas cavity 604 and the outlet cavity 612 . The valve shuttle catch 623 was situated or positioned in the cavity 604 and the catch 624 situated or positioned in the cavity 612 .
[0044] Still referring to FIG. 8 , when the accumulator 622 was filled with compressed air to 60 psi, the gas piston 617 was pushed down with the valve shuttle 605 to close the outlet port 614 . The generator 600 was then ready for generating a pulsed fluid jet of choice. In this case, compressed air of 90 psi was selected as the system fluid in order to generate a pulsed air jet for a special application. When the 90-psi compressed air entered into the upper cavity 612 , it saw but could not open the closed outlet port 614 . Instead, the 90-psi air started to push the gas piston 617 upward with a total force of about 100 pounds, which was greater than the downward force of about 69 pounds on the gas piston from the 60-psi air in the accumulator 621 . As a result, the gas piston 617 started to move up while the outlet port 614 remained closed. After traveling for 3 inches, the gas piston 617 made contact with the upper catch 623 and exerted a lifting force on the valve shuttle 605 to open the outlet port 614 and to close the inlet port 613 . At this moment, 90-psi air in the cavity 612 saw the entire cross-sectional area of the valve shuttle 605 , thus exerting a force to keep the inlet port 613 closed. The 90-psi air in the cavity 612 started to flow out of the nozzle under the pushing force of the gas piston 617 . Quickly, the gas piston 617 caught up with the lower catch 624 and the valve shuttle 605 moved down to close the outlet port 614 , thus completing one cycle of the valve operation. This up-and-down movement of the gas piston 617 continued and the pulsed air jet was generated at the nozzle, which had an opening of 0.75 inches. The pulsed air jet was very unique due to the substantial amount of energy it packs. When generated in water, the air jet could propel a small boat such as a kayak or canoe. On the other hand, a continuous stream of compressed air would not be suitable for such use. Likewise, the pulsed air jet or other fluid jet from the generator 600 of this invention will find many other applications.
Example 3
[0045] A pulsejet generator 700 was constructed for water applications according to the embodiment shown in FIG. 9 . The generator 700 was made of two attached cylinders, an upper gas cylinder 726 made of carbon steel and a lower water cylinder 701 made of hardened stainless steel. The gas cylinder 726 was 9 inches long and 3.5 inches in diameter and the water cylinder 701 was 5.25 inches long and 2.5 inches in diameter for an assembled overall length of 14.5 inches. The gas cylinder 726 had a gas chamber 731 of 2.5 inches in diameter and housed a gas piston 727 made of aluminum alloy and was fitted with a polymeric outside diameter seal 728 . A hollow plunger 722 made of hardened stainless steel was attached to the gas piston 727 on one end and was fitted with an end cap 718 on the other end. The plunger 722 was housed inside the water cylinder 701 and was free to slide. The plunger end cap 718 was made of hardened stainless steel and was fitted with a polymeric outside diameter seal 720 and a polymeric inside diameter seal 721 around a cylindrical valve shuttle 705 . The valve shuttle 705 was made of hardened stainless steel and was 0.250 inches in diameter, 3.25 inches long, and had tapered ends 706 and 707 of 60 degrees. The valve shuttle 705 also had side ports 708 and 709 of 0.094 inches diameter and an inside fluid passage 710 of 0.125 inches in diameter connecting the two side ports 708 and 709 . The valve shuttle 705 also had machined catches 723 and 724 of 0.063 inches high and 0.010 inches thick.
[0046] Still referring to FIG. 9 , the constructed pulsejet generator 700 had a water supply tube 725 placed in the center of gas cylinder 726 connecting the outside water inlet 702 to a valve inlet head 715 situated or positioned inside the hollow plunger 722 . The water tube 725 , made of stainless steel, was 0.250 inches in outside diameter, was 0.094 inches in inside diameter, and was 6.5 inches in length. The valve inlet head 715 , made of stainless steel, was 0.560 inches in outside diameter and 1.0 inch in length, and had a tapered inlet port 713 of 60 degrees, an inlet cavity 711 of 0.312 inches in diameter, and a shuttle opening of 0.250 inches in diameter fitted with a polymeric seal 717 . The valve shuttle 705 straddled across cavities 711 , 730 , and 712 with its inlet side port 708 situated or positioned in the cavity 711 and its outlet port 709 in the cavity 712 . Seals 717 , 720 and 721 kept fluid leakage to a minimum. The cross-sectional area of the gas piston 727 was 4.91 square inches and the cross-sectional area of water tube was 0.049 square inches. Thus, the effective gas surface area on the gas piston 727 was 4.91−0.049=4.857 square inches. The cross-sectional area of plunger end cap 718 was 0.52 square inches. Thus, the intensification ratio of the pressure intensifier was 4.857÷ 0.52=9.34. This intensification ratio indicates that the maximum water pressure the pulsejet generator 700 could accommodate is 9.34×Pg, with Pg being the gas pressure inside the gas chamber 731 .
[0047] The pulsejet generator 700 was filled with compressed air to 300 psi. The gas piston 727 was pushed down by the compressed air and the outlet port 714 was closed. Tap water pressurized to 2000 psi from a motorized jet washer was introduced into the pulsejet generator 700 , and a pulsed waterjet issued or discharged immediately at the nozzle 736 , which had a sapphire orifice of 0.052 inches in diameter. The waterjet pulses could be seen with the naked eye and the modulating motion of the valve shuttle inside the generator was felt by hand. The frequency was estimated to be less than 20 cycles per second and the volume of water per pulse was estimated to be less than 0.5 cubic inches. The resultant pulsed waterjet appeared to be quite powerful and compared very favorably against a conventional straight waterjet issued or discharged by the same nozzle in impacting against a concrete block.
[0048] While in the foregoing specification this invention has been described in relation to certain preferred embodiments thereof, and many details have been set forth for purpose of illustration, it will be apparent to those skilled in the art that this invention is susceptible to additional embodiments and that certain of the details described herein can be varied considerably without departing from the basic principles of this invention. | An apparatus for generating high-speed pulsed fluid jets. A valve assembly has a valve body with an inlet and an outlet. A valve shuttle is slidably or movably mounted with respect to the valve body. The valve shuttle is positioned within a cavity of the valve body and divides the cavity into an upper or inlet cavity and a lower or outlet cavity. The valve shuttle has a passage in communication with the upper cavity and the lower cavity. In an open condition of the valve assembly, fluid communication is formed between the inlet, the inlet cavity, the passage, the outlet cavity and the outlet. | 8 |
BACKGROUND OF THE INVENTION
[0001] The present invention relates to a machine for automatically applying buttons or other metal fittings in general on a support, such as a fabric support, the machine including a mechanism for controlling or compensating for the excessive pressure or pushing force due to the presence of enlarged thickness portions.
[0002] More specifically, the field of the invention is that of the machine used for applying buttons (for example pressure buttons) and other metal fittings in general on a support such as a fabric support or other sheet material support in general.
[0003] As is known, prior machines for applying buttons on a fabric piece or sheet conventionally comprise a bottom punch element and a top punch element, the punch elements being driven in different driving directions, so as to mutually clamp, on respective faces of the fabric support, the two parts forming the button to be applied.
[0004] Said machines usually comprise moreover load or loading rods entraining respective portions of the buttons to be applied to the driving axis of the punches, said punches in turn operating for pressure crushing the button parts on the fabric support, to clamp said parts on the latter.
[0005] A drawback of the above mentioned machines is that the driving means or mechanism included therein for driving or operating the top punch element, are not adapted to provide a reliable holding, on the button parts which must be coupled to one another, of the pressure necessary for closing said button parts, and this, in particular, if the thickness of the support fabric is changed with respect to a rated fixed thickness value based on which the machine is calibrated.
[0006] Moreover, in prior machines of the above mentioned type, the load or loading rods are usually driven by a specifically designed servo-mechanism, which is separated from the punch element driving systems.
[0007] Such prior solution has the drawback that the machine construction is very complex thereby the machine cannot operate in a reliable manner and must be frequently switched off to repair possible jammings occurring therein.
SUMMARY OF THE INVENTION
[0008] Accordingly, the aim of the present invention is to provide a novel machine for automatically applying buttons and other metal fittings in general, which, with respect to prior like machines, is very simple construction wise and very reliable in operation.
[0009] Within the scope of the above mentioned aim, a main object of the present invention is to provide such a machine which is adapted to provide a desired closing force on the punch elements, at the point at which the button is applied to the fabric support, independently from the thickness both of the fabric support and of the parts forming said buttons.
[0010] Yet another object of the present invention is to provide such a machine which is further adapted to indicate possible failures in applying the button or metal fittings to the fabric support.
[0011] According to one aspect of the present invention, the above mentioned aim and objects, as well as yet other objects, which will become more apparent hereinafter, are achieved by the machine as claimed in claim 1 .
[0012] Preferred embodiments of the inventive machine are defined in the dependent claims.
[0013] Owing to the provision of a driving mechanism including a telescopic system for controlling the displacement of the top punch element, the inventive machine allows to hold a constant pressure on the button being applied, independently from the thickness of the button and the fabric support therefor.
[0014] With respect to the prior art in this field, and owing to the unified or standardized mechanism for driving both the punch elements and loading rods, the inventive machine provides moreover the advantage that it is much more simple construction wise and reliable in operation.
[0015] Finally, the provision in the system of a load cell allows to indicate possible failures in applying the buttons or metal fittings on the fabric support.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The above mentioned and further advantages, objects and features will become more apparent hereinafter from the following detailed disclosure of a preferred embodiment of the invention which is illustrated by way of a non limitative example, in the accompanying drawings, where:
[0017] FIG. 1 is a general outlay of the machine according to the present invention;
[0018] FIG. 2 is a side elevation view illustrating a detail of the driving mechanisms for driving the punch elements and loading rods, as included in the machine shown in FIG. 1 ;
[0019] FIG. 3 is a schematic view illustrating the conditions of the mechanisms of FIG. 2 , as the button parts are loaded toward the button applying region;
[0020] FIG. 4 illustrates the details shown in FIG. 3 , in a button applying condition;
[0021] FIG. 5 illustrates the details of FIG. 3 , as a button is applied on a support having an increased thickness;
[0022] FIG. 6 is an exploded view illustrating the detail of the top punch element driving system;
[0023] FIG. 7 illustrates a further detail of a cam system for adjusting the position of the bottom punch element.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0024] The inventive machine has been generally indicated by the reference number 1 in FIG. 1 .
[0025] Said machine essentially comprises two loaders 2 and 3 for feeding button parts or components, as respectively indicated by the reference numbers 4 and 5 , at a button applying axis 6 for applying said button to a support 7 (for example a support fabric, see FIG. 3 ).
[0026] Said button parts 4 and 5 are moreover driven toward their applying region, thereat operate a top punch element 8 and bottom punch element 9 , through respective guides 10 and 11 .
[0027] As is clearly shown in FIG. 2 , the inventive machine 1 comprises moreover a standardized driving mechanism for driving the bottom punch element 9 and loading rods 12 , 13 for loading said button parts 4 , 5 , said driving mechanism including a control lever 14 driven by a driving cam 15 .
[0028] Said lever 14 is pivoted on a pivot pin 16 and presents end portions 17 , 18 which respectively operate on the cam 15 and a middle lever 19 for controlling the movement of the bottom punch element 9 .
[0029] On said lever 14 a pawl 20 is moreover provided, which, as it is engaged inside a corresponding fork element 21 , drives said loading rods 12 and 13 through a rigid bush assembly 22 , rigid with the fork element 21 and designed for sliding on a guide rod 23 and small plate 24 in turn clamped to corresponding end portions of said loading rods 12 and 13 .
[0030] The front end portions of said loading rods push said respective button parts 4 , 5 into corresponding guides 25 and 26 , so as to drive them to their applying axis 6 .
[0031] At a middle position between said lever 14 and bottom punch element 9 , a further lever 19 is arranged, said further lever 19 being pivoted on a pivot pin 27 and having an end portion 28 abutting against the roller 18 of the lever 14 , whereas the end portion 29 drives the bottom punch element 9 .
[0032] More specifically, the pivot pin 27 of the lever 19 is of a cam or eccentric pivot pin, including a drive disc element 30 (see FIG. 7 ) having a cylindric portion 31 on the same axis as that of the drive disc, and a further cylindric portion 32 eccentrically arranged with respect to said cylindric portion 31 .
[0033] Due to the above construction, the vertical position of the lever 19 can be modified by causing the drive disc 30 to turn with respect to the machine body or frame.
[0034] On said cam 15 , which is driven by a suitable geared unit (not shown), is pivoted an end portion 33 of a telescopic rod 34 , the other end portion 35 of which will drive the top punch element 8 through knee joint 36 in turn pivoted to the machine body at its pivot pin 37 .
[0035] As is clearly shown in FIG. 6 , the telescopic rod 34 comprises a bottom arm 38 to be clamped, on a side, to a crank pin 39 of the cam 15 and, at the other side, to the telescopic rod cylinder 40 .
[0036] Inside said cylinder 40 are moreover arranged, in succession, a loading cell 41 , a cup spring pack 42 and a spacer element 43 .
[0037] This assembly is held in a set position, by pressurizing the spring pack 42 , and engaging the threaded bar 44 , also arranged inside the cylinder 40 , by a nut 45 .
[0038] A firm connection of the rod construction 34 is made by engaging the arm 38 on a corresponding end portion of the cylinder 40 (in the shown embodiment by engaging a pin, not shown, in respective engaging holes, as shown).
[0039] The threaded bar 44 is in turn rigid with the top arm 46 of the rod 34 , said top arm 46 being pivoted at 47 on the articulated or knee joint 36 (see FIG. 2 ).
[0040] The preloading condition of the cup spring pack 42 is obtained by screwing on the nut 45 on the threaded bar 44 , and being sensed or measured by a loading cell 41 .
[0041] Thus, as the cam 15 is rotatively driven (according to the arrow F 1 of FIG. 3 ) the following occurs:
[0042] the telescopic rod 34 will be driven in the direction of the arrow F 2 ;
[0043] the knee joint 36 will be opened by causing it to turn about its pivot pin 37 (arrow F 3 );
[0044] the top punch element 8 will be lowered (arrow F 4 ) in the direction of the button piece or part 4 supported by a respective button grip (not shown);
[0045] the lever 14 will be turned about its pivot pin 16 (arrow F 5 );
[0046] the loading rods 12 , 13 will be moved away or withdrawn from the button applying region (arrow F 6 );
[0047] the middle lever 19 will be rotatively driven about its pivot pin 27 (arrow F 7 ) by abutting the end portion 18 of the lever 14 against the corresponding portion of the lever 19 (arrow F 8 );
[0048] the bottom punch element 9 will be raised toward the respective button part or piece 5 (arrow F 9 ).
[0049] Thus, owing to the above disclosed movements, the button will be brought to its closure or applying condition clearly shown in FIG. 4 .
[0050] If, in such a closing or closure position, the thickness encountered by the punch elements 8 , 9 is larger than the above disclosed one, then the status of the machine will be that shown in FIG. 5 .
[0051] As is herein shown, in particular, the knee joint 36 has an opening angle f larger than that shown in FIG. 4 and the telescopic rod 34 will have its cylindric part 40 slightly removed or displaced away from the corresponding bearing point 48 of the arm 46 , by driving that same cylinder 40 in the direction of the arrow F 10 of FIG. 5 .
[0052] This displacement of the cylinder 40 will transfer to the cup spring pack 42 , the excess pushing due to the movement of the cam 15 toward its limit position, thereby preventing such excessive pushing from affecting the end portion of the top punch element 8 , thereby holding, at the button applying point, a preset pressure value.
[0053] The load cell 41 , in particular, operates to indicate to an operator a possible excessive or insufficient pushing of the spring, with respect to a present pushing range, which would indicate a failure in the button applying operation.
[0054] The machine as disclosed is susceptible to several modifications and variations, all of which will come within the scope of the following claims.
[0055] Thus, for example, the telescopic rod 34 can be replaced by a cylinder (either of a pneumatic or of a hydraulic type), the piston of which will affect the knee joint 36 and the pushing force of which would be controlled by a central control unit. | A machine is herein disclosed for automatically applying buttons or other metal fittings in general on a support, of a type comprising loader elements, guide and load rods for feeding parts of the buttons or metal fittings to the support, and punches, respectively a top and a bottom punch, for clamping the button or metal fitting parts on the support, the machine further comprising a telescopic rod for operating the top punch and to hold constant, at the button applying point, a preset pressure value, independently from the presence of possible enlarged thickness portions at the button applying point. | 0 |
CROSS-REFERENCE TO RELATED APPLICATION
This is application is a continuation of application Ser. No. 11/031,514, filed Jan. 7, 2005 now U.S. Pat. No. 7,901,634, which claims priority to and the benefit, under 35 U.S.C. 119(e), of the filing date of U.S. Provisional Application 60/535,615, filed Jan. 8, 2004 and titled “Apparatus and Methods for Processing Biological Samples”, both of which applications are incorporated by reference in their entirety.
FIELD OF THE INVENTION
This invention pertains to the fields of cytology and histology, molecular biology, biochemistry, immunology, microbiology and cell biology. In particular, the invention is related to the fields of molecular cytogenetics and immunohistochemistry and, even more particularly, to a method and an apparatus for processing, treatment, or even staining of at least one biological sample accommodated on a carrier member, such as a microscopic slide as well as to the control of the humidity and temperature during processing. Applications to which the present invention may relate especially include in-situ hybridization, fluorescent in-situ hybridization, cytology, immunohistochemistry, special staining, and microarrays, as well as potentially other chemical and biological applications.
BACKGROUND OF THE INVENTION
Histological and cytological techniques have been used to analyse biopsies and other tissue samples, as an aid to medical diagnosis and research. Cytology is the study of the structure of all normal and abnormal components of cells and the changes, movements, and transformations of such components. Cells are studied directly in the living state or are killed (fixed) and prepared by for example thin layer preparation systems, embedding, sectioning, and/or staining for investigation in bright field, fluorescent or electron microscopes. Histology is the study of groups of specialised cells called tissues that are found in most multi-cellular plants and animals. Histological investigation includes study of tissue and cell death and regeneration and the reaction of tissue and cells to injury, a disease state such as cancer or invading organisms such as HPV (Human Papilloma Virus). Because normal tissue has a characteristic appearance, histological examination is often utilised to identify diseased tissue.
In situ hybridisation (ISH), and Immunohistochemistry (IHC) analyses are useful tools in histological diagnosis and the study of tissue morphology. In situ hybridisation (ISH), immunocytochemistry and immunohistochemistry (IHC) seek to identify a detectable entity in a sample by using specific binding agents capable of binding to the detectable entity.
A biological sample is in this application to be understood as a biological sample such as histological samples, e.g. tissue and cell specimens, including cell lines, proteins and synthetic peptides, tissues, cell preparations, blood, bodily fluids, blood smears, metaphase spreads, bone marrow, cytology specimens, thin-layer preparations, and specifically biological samples on microscope slides. The biological sample may further suitably be selected from histological material, including formalin fixed and paraffin embedded material, cytological material, fine needle aspirates, cell smears, exfoliative cytological specimens, touch preparations, bone marrow specimens, sputum samples, expectorates, oral swabs, laryngeal swabs, vaginal swabs, bronchial aspirates, bronchial lavage, gastric lavage, blood, urine, and body fluids. Such biological samples may be subjected to various treatments. Further, the biological sample may be suitably selected from non human sources, including virus and fungus swabs, samples taken from medical equipment, veterinary samples and food. Also, samples may be taken from hair, organs, sperm and egg cells as well as cell grown in vitro. The biological samples are preferably from living or post-mortem tissues of Homo sapiens , but not limited to eukaroytic cells. Examples include detection of prokaryotic organisms, such as Escherichia coli 0157 in drinking water.
Slides can be any suitable solid or semi solid support for the biological sample. In particular, the support may be a microscope slide, a micro array, a membrane, a filter, a polymer slide, a chamber slide, a dish, or a Petri dish.
The current invention relates especially—but not exclusively—to in situ hybridisation (ISH). In situ hybridisation is a diagnostic method for characterization and evaluation of genes, chromosomes, cells, cell aggregates, tissues and other biological samples. In situ hybridisation can be used to evaluate and characterize the status, genetic abnormalities and other disease states, such as cancer or disease, caused by infectious organisms. Further, it can be used to characterize cells with respect to infectious agents such as, but not limited to, HPV, HIV (Human Immunodefiency Virus) and HCV (Hepatitis C Virus). Molecular genetic events, such as aneuploidy, gene amplification, gene deletion, RNA expression, RNA transportation, RNA location and chromosome translocations, duplications, insertions, or inversions that are difficult to detect with karyotype analysis, PCR (Polymerase Chain Reaction), or LCR (Ligase Chain Reaction) can be characterized by ISH.
The ISH techniques can have the potential to increase the survival chances of cancer patients by making possible earlier detection of malignancy and more accurate prognostic assessments following tumour surgery. The technique can also be applied to prenatal and postnatal genetic analysis. Furthermore, the technology can be used for simultaneous detection of multiple genetic anomalies in an individual cell, and thereby save assay time and limit specimen requirements.
Non limiting examples of diagnostically important ISH assays include detection of HER-2 (also known as HER-2/neu or c-erbB2), Topo II (breast carcinoma), telomers, EGFr, C-Myc (breast carcinoma), N-Myc (neuroblastoma); translocation probe pairs for BCR/ABL (chronic myelogenous leukemia), EWS (Ewing's sarcoma), C-Myc (Burkitt's lymphoma, T cell ALL), acute myeloid leukemia (AML), myeloproliferative disorders (MPD), Myelodysplastic Syndrome (MDS) and centromeric probes for chromosomes 17, 7, 8, 9, 18, X, and Y. Other examples include the analysis of Epstein-Barr virus, Herpes simplex virus and Human cytomegalo virus, Human papilloma virus, Varizella zoster virus and Kappa and Lambda light chain mRNAs. Yet other examples include the detection and analysis of samples of non-human origin, for example, food borne parasites and disease causing microbes and viruses. More specific examples include:
i) the analysis of HER-2/neu, also known as c-erbB2 or HER-2, which is a gene that has been shown to play a role in the regulation of cell growth. The gene codes for a transmembrane cell surface receptor that is a member of the tyrosine kinase family. HER-2 has been shown to be amplified in human breast, ovarian and other cancers;
ii) the analysis of aneuploidy for chromosomes 3, 7, 17 and loss of the 9p21 locus in urine specimens from patients with transitional cell carcinoma of the bladder;
iii) the detection and quantification of the lipoprotein lipase (LPL) gene located at 8p22 and the C-MYC gene located at the 8q24 region (Two genetic alterations observed in abnormal cells, such as Prostate cancer samples, are gain of 8q24 and 8p21-22 (LPL) loss of heterozygosity.);
v) the identification and enumeration of chromosome 8 in cells obtained from bone marrow. An association has been made between trisomy 8 and both myeloid blast crisis and basophilia (Trisomy 8 is a prevalent genetic aberration in several specific diseases like Chronic Myelogenous Leukemia (CML), acute myeloid leukemia (AML), and myeloproliferative disorders (MPD).);
v) the analysis of chromosome aneuploidy like translocations of the immunoglobulin heavy chain locus (IGH) located at 14q32 and frequently observed in patients with various hematological disorders (These IGH translocations result in the upregulation of oncogenes due to the juxtaposition of IGH enhancers with these oncogenes.);
vi) the identification of inv(16)(p13q22) where the CBFB gene located in 16q22 is fused to the MYH11 gene located in 16p13, resulting in a chimeric protein product detected in acute myeloid leukemia (AML);
vii) the detection of Human Papilloma Viruses (HPV), which are a group of small DNA viruses (There are more than 90 HPV types. Persistent HPV infection may result in cervical cancer, and has also been associated with other types of cancer, e.g. colon cancer. HPV types are classified according to the risk associated with the development of cervical cancer. Fifteen types are classified as high-risk, and these are detected in more than 99% of all cervical cancers.).
In summary, the in situ Hybridization (ISH) technique is a useful method for the analysis of cells for the occurrence of chromosomes, chromosome fragments, genes and chromosome aberrations like translocations, deletions, amplifications, insertions or inversions associated with a normal condition or a disease. Further, ISH is useful for detection of infectious agents as well as change in levels of expression of RNA.
The ISH techniques should be understood to include, for example, fluorescent in situ hybridization (FISH), chromogenic in situ hybridization (CISH), Fiber FISH, CGH, chromosome paints and arrays. In the following, the ISH technique and procedures are described in greater detail. ISH uses nucleic acid probes, designed to bind, or “hybridize,” with the target DNA or RNA of a specimen, usually fixed or adhered to a glass slide. DNA, RNA, PNA, LNA or other nucleic acid probes of synthetic or natural origin can be used for the ISH technique. The probes are labelled to make identification of the probe-target hybrid possible by use of a fluorescence or bright field microscope. The probe is typically a double or single stranded nucleic acid, such as a DNA or RNA. It is labelled using radioactive labels such as 31P, 33P or 32S, or non-radioactively, using labels such as digoxigenin, or fluorescent labels, a great many of which are known in the art. The hybrid is often further analysed with computer imaging equipment. Since hybridization occurs between two complementary strands of DNA, or DNA analogues, labelled probes can be used to detect genetic abnormalities, providing valuable information about prenatal disorders, cancer, and other genetic or infectious diseases.
Unlike other molecular DNA-based tests, which require cell lysis to free nucleic acids for analysis, ISH allows analysis of DNA in situ, that is, in its native, chromosomal form within the cell or even the nucleus. This feature permits the analysis of chromosomes, genes and other DNA/RNA molecules of individual cells. For direct-labelled probes, the results are detected by viewing the samples under a fluorescence microscope with appropriate filters. Indirect detection, like CISH, demands additional labelling steps, which typically require streptavidin or antibody-enzyme conjugates or fluorophore-labeled counterparts, and additional washing steps once the probe is bound to the target.
An exemplified general ISH procedure includes one or several of the following sequential procedural steps:
i) Mounting of the biological sample on slides ii) Baking at elevated temperatures iii) Dewaxing or deparaffination if necessary iv) Washing v) Target retrieval at elevated temperature vi) Denaturing at elevated temperature vii) Incubation with blocking reagents viii) Addition of probe mixture to the sample on the slide. x) Placing a coverslip over the sample and the probe mix and sealing with rubber cement. x) Hybridization at elevated temperatures. xi) Washing at elevated temperatures and removal of coverslip xii) Air drying and counterstaining xiii) Visualization according to the instruction for FISH or CISH xiv) Examination and evaluation in a microscope
In more detail, an exemplified FISH protocol for paraffin embedded tissue sections could include one or several of the following sequential procedural steps:
i) Cutting 2-4 micrometer tumour sections from a block ii) Mounting on slides iii) Baking at 60° C. for 30 minutes iv) Deparaffination using xylene v) Rehydration by immersing in ethanol/water mixtures vi) Pre treating by washing with an aqueous buffer for 10 minutes at 95° C. vii) Pepsin digesting for 10 minutes at ambient temperature viii) Washing repeatedly x) Dehydration in a series of cold ethanol/water mixtures x) Air drying xi) Addition of 10 microliter fluorescent labelled DNA or PNA probe mixture per slide xii) Sealing with a 22 by 22 mm glass coverslip and rubber cement at the edges xiii) Denaturing at 82° C. for 5 minutes, directly followed by xiv) Hybridization over night (18 hours) at 45° C. xv) Removal of the coverslip xvi) Stringent washing at 65° C. for 10 minutes xvii) Washing repeatedly with wash buffer xviii) Dehydration by immersing in a series of cold ethanol/water mixtures xix) Air drying xx) Mounting with 10 microliter anti fade solution with DAPI as counter stain xxi) Sealing with a coverslide xxii) Examination and evaluation in a fluorescence microscope
The hybridization mixture is typically a complex mixture of many components. Non-limiting examples of components include formamide, water, triton x-100, tween 20, Tris or Phosphate buffer, EDTA, EGTA, polyvinylpyrrolidine, dextran sulfate, Ficoll, or salmon sperm DNA.
Chromogenic in situ hybridization (CISH) uses labelled probes, which can be visualized by the use of immunological staining methods similar to the IHC staining procedures. CISH has some differences compared to FISH techniques: The genetic aberrations may be viewed within the context of tissue morphology—simultaneous examination of histopathology and ISH results. Also, the results may be visualized with a standard bright field microscope, and the chromogenic dye (for example DAB) generated on the slide is permanent with no or little fading of fluorescent signals.
In addition to ISH, the current invention also relates to immunohistochemistry and immunocytochemistry. The general exemplified formalin fixed paraffin embedded (FFPE) immunohisto chemical (IHC) chromogenic staining procedure may involve the steps of: cutting and trimming tissue, fixation, dehydration, paraffin infiltration, cutting in thin sections, mounting onto glass slides, baking, deparaffination, rehydration, antigen retrieval, blocking steps, applying primary antibody, washing, applying secondary antibody-enzyme conjugate, washing, applying enzyme chromogen substrate, washing, counter staining, cover slipping and microscope examination.
As described above, the sample treatment of the slides is complicated, laborious and uses many different reagents at various temperatures for prolonged periods. It should be understood that under normal conditions only small amount of reagents, 200 μl or even less, are applied to the sample. Thus, the reagent and sample are very easily dried out, especially under high temperatures and at low relative humidity. Many of the procedural steps in ISH, including the denaturing and the hybridization steps are typically done in a humidity chamber. The humidity chamber is a closed or semi closed container in which the slides can be processed and heated. It should be understood that the processing temperature as well as the temperature ramp time—that is, the change of temperature per time unit, is important for both the overall protocol length and the subsequent visualized result. Furthermore, it has been observed that the staining result depends strongly on the humidity during the sample treatment. Also, the morphology can suffer from drying out during the treatment. For example, chromosome spreads are easily ruined due to drying out conditions. During the changes of temperatures the air above the slides will expand or contract. The reduction in pressure during lowering of the temperature will draw in air from the outside, which may be less saturated with water compared to the air above the slide. During heating, air will be pressed out of the space between the slide and the lid. This air will contain moisture, which will escape from the system. Consequently, due to the plurality of fast and repeated changes in temperature, high temperatures for prolonged time and the small space between the slides and the lid, moisture can escape either quickly, or over time, from the system, resulting in a change in the concentration of the reagents applied to the biological sample and thus a change in the protocol, or even drying out of the biological sample.
The absolute humidity is defined as the amount of water in a given volume of gas. The relative humidity is the ratio between the amount of water and the maximum amount of water possible at the given temperature and pressure. The maximum amount of water per volume, and consequently the relative humidity, depends strongly on the temperature, as described by the Clausius-Clapeyron equation. For example, without addition of water in a closed system, 100% relative humidity at 25° C. will correspond to 16.3% at 60° C. and 3.7% at 95° C., indicating the strong dependence of temperature. Even a small change of temperature will change the relative humidity dramatically. For example, a relative humidity of 100% at 80° C. will correspond to only 66.7% at 90° C. in a closed system without addition of moisture.
From the discussion above, it should be clear that precise control of humidity, heating and cooling is essential for obtaining, for example, consistent ISH results. Therefore, without an efficient humidifying system, heating of the slides can result in fast drying out of the reagents or sample.
DESCRIPTION OF PRIOR ART
In order to prevent drying out or loss of “reagents” of the slides, several different closed humidifying systems are known to be used in the cytogenetic, pathology and research laboratories during for example the critical steps of denaturation and hybridization.
U.S. Pat. No. 6,555,361 discloses a hybridization chamber that contains a built-in mechanism for saturating the air within the chamber when sealed thereby preventing drying of the liquid sample. The hybridization chamber is defined by matching top and bottom clam-shell like halves that, when brought together, are sealed by an o-ring and clamping device. The chamber is equipped with a liquid reservoir, the liquid from which will serve to saturate the volume of air sealed within the hybridization chamber. A saturated atmosphere within the chamber prevents evaporation of the sample. This patent illustrates an interior chamber sized to receive a glass microscope slide and suggests positioning a well within the chamber to retain liquid separately from the region for holding a liquid sample. Further, it is suggested to dispose a microporous membrane material in the chamber and specifically in the well. The control of temperature and humidity inside the chamber during rapid warm-up or cool-down periods is not discussed in this patent document.
Humid boxes or humidified chambers are typically plastic containers with a lid. Water-soaked paper towels are placed in the bottom of the box and excess water decanted away. Slides in racks can be placed horizontally or vertically in the box during for example overnight hybridization. Typical “home-made” humid box laboratory equipment includes standard Tupperware™ or Rubbermaid™ boxes or standard cake pans with a tight closing lid. Wet paper tissue is placed in the bottom. A frame or grid is placed over the tissues and the slides placed on the frame or grid before the lid is closed. The humid box is placed in a conventional or microwave oven or on top of a heating plate during for example the denaturation or hybridization steps. To further control the humidity and temperature profile, the humid box can be isolated to limit heat loss and thereby hold the temperature for longer periods.
An insulated box like e.g. the HybBox™ (InSitus BioTechnologies, Albuquerque, N. Mex., USA) made of expanded polystyrene with a base and a lid is an attempt to further control the humidity and temperature during for example hybridization. After denaturation of the biological sample on slides in an oven, the slides are transferred to the HybBox™, which is tightly closed. After hybridization, the box is opened and the slides further treated.
To further control the temperature profile during general slide processing, several temperature-controlled chambers are commercially available. One example is the Boekel Slide Moat™ (Boekel Scientific, Feasterville, Pa., USA) consisting of a temperature controlled heating block. Up to 30 standard microscope slides can be placed horizontally on the heating block. A glass lid with seals closes over the heating block and the slides. Placing wet towels on the heating block together with the slides can give high humidity.
The HYBrite™ Denaturation/Hybridization System (Vysis, Abbott Laboratories, Downers Grove, Ill., USA) is another temperature controlled humid chamber widely used in, especially, ISH laboratories. It consists of a programmable heating plate on which up to 12 microscope slides can be placed. A lid comes down over the heating plate and slides and closes the system. On each side of the slide heating plate, wells or channels can hold water or wet tissues or towels. Humidity is thereby sought controlled by the use of wet tissues or towels. Once the slides are placed in the instrument and the lid is closed, sequential denaturation and hybridization steps can be performed automatically without the intervention of the user.
In an attempt to further control the temperature and avoid small temperature fluctuations, the TruTemp heating system (Matrix, Hudson, N.H., USA) uses a heated lid in addition to the heated slide block. The instrument consists of a programmable heating block on which the slides are placed. The lid is further heated. Humidification is provided by water added to wells integrated into the heating block on which the slides rest.
Typically, the user can program the various commercially available temperature controlled humid systems with many time-temperature protocols from 0 to more than 24 hours and from ambient temperature to 100° C.
In yet another attempt to automate the temperature and humidity during processing, automated instruments using so called liquid coverslip systems (Ventana Medical Systems, Tucson, Ariz.) have been introduced. The limiting of drying out of slide-mounted specimens has been sought by covering the reagents and sample with an immiscible oil. The system only limits the evaporation, resulting in loss of a significant part of the reagent volume and is not practical for hybridization in more than 12 hours at elevated temperatures.
The instruments eliminate a number of steps and reduce hands-on time required during conventional ISH procedures performed by cytogenetic, pathology and research laboratories. Nonetheless, the manual systems using ovens and various plastic containers, in general, still give the best results with regard to both preserved morphology and staining efficiency. The semi or fully automated humid boxes or chambers have the advantage of e.g. less hands-on work and ease of use. However, none of the semi or fully automatic humid boxes or chambers has succeeded in providing a performance equivalent to or exceeding the manual methods, with respect to preserved morphology and staining efficiency. The humidity control is closely connected to the temperature, as discussed previously, but is not easily controlled. Also, no known system has truly addressed the problem of having both controllable uniform temperature and uniform and high humidity over the slides for prolonged time.
In light of the above discussion, there is a need in the art for an improved treatment device for treating biological samples. In summary, the improved sample treatment device should ideally include: programmable temperature control; precise control of heating and cooling; fast change of temperature; independence of the number of slides treated; high humidity at any relevant temperature; constant humidity for prolonged periods; and uniform temperature and humidity over the slides. The present invention addresses such a need.
SUMMARY OF THE INVENTION
The present invention provides an apparatus for processing biological samples, the apparatus comprising means for processing at least one biological sample accommodated on at least one carrier member, characterised in that at least one reservoir able to accommodate a fluid is arranged on a surface adjacent to and/or facing a substantial part of the at least one biological sample. The proximity of the fluid reservoir and the sample is important in order to ensure that vapor from the reservoir can be generated at a rate able to maintain a constant high relative humidity in the chamber formed around the sample by the inner surfaces of the apparatus during a heating period with raising temperature.
In a preferred embodiment, the reservoir is arranged above the at least one sample on the at least one carrier member.
In a preferred embodiment, the apparatus comprises a bottom member arranged to support at least one carrier member carrying at least one biological sample and characterised by further comprising a lid including at least one fluid reservoir. The preferred position of the fluid reservoir is on the lower surface of the lid. This ensures the optimal proximity to the samples.
In a preferred embodiment, the lid member is provided with holding means, such as a grid, slots and/or fingers (not shown), supporting the at least one fluid reservoir, arranged to be located above the biological samples when the lid is closed, thereby covering the bottom member.
In a preferred embodiment, an apparatus according to the invention is characterized in that the reservoir is placed less than 5 cm from the carrier member, and, preferably, less than 1.0 cm from the carrier member, and, yet more preferably, less than 0.50 cm from the carrier member.
Preferably, an apparatus according to the invention is characterized in that the macroscopic surface area of the reservoir adjacent to and/or facing the sample on the carrier member is more than 10% of the total carrier member area, and, preferably, more than 30% of the total carrier member area and, even more preferably, more than 60%. The extension of the reservoir plays an important role in the same way as the proximity by improving the rate by which the relative humidity may be changed as well as the ability to maintain a prescribed high relative humidity during a rapid heating period with raising temperature.
Preferably, an apparatus according to the invention is characterized by comprising heating means for heating the sample on the carrier member. Preferably, the heating means are incorporated in the apparatus.
Preferably, the apparatus is characterized by comprising temperature controlling means controlling the temperature of the carrier member and, thereby, the temperature of the biological sample on the carrier member. Preferably, the apparatus includes temperature-controlling means enabling an automatic heating of the sample according to instructions prescribed in a protocol defining the desired processing of the sample.
Preferably, the apparatus is characterized by comprising at least one temperature sensor connected to the temperature controlling means.
In a preferred embodiment the heating means are heating wires. Alternatively, the heating means may be inductive heating.
Preferably, the temperature controlling means comprises cooling means for cooling the sample on the carrier member. The prescribed processing of a biological sample typically involves cooling after a period of heating. In a preferred embodiment the cooling means are Peltier elements and/or at least one fan.
In a preferred embodiment, the apparatus may comprise heating means for heating the reservoir, and the temperature controlling means may enable control of humidity in the chamber by changing the temperature of the reservoir and/or sample by activating the heating means or the cooling means in the bottom member of the apparatus and/or in the lid.
In a preferred embodiment of the apparatus, the heating means for heating the sample on the carrier member and the heating means for heating the reservoir are controlled separately, and may be heated to different temperatures, so that the reservoir may become warmer than the sample or vice versa. In this manner, the control of the relative humidity within the chamber around the sample may be highly improved as a high humidity may be generated fast by raising the temperature of the reservoir, thereby releasing vapor molecules into the atmosphere in the chamber and thereby around the sample. Dependent on the temperature of the sample and the reagents on the sample—and such temperature can be controlled by heating or cooling the support of the sample—the vapor may stay in a balance with the reagents and the sample or may concentrate on the sample and in the solution comprising the reagents.
Alternatively, if a lower humidity is desired, this may be obtained by lowering the temperature of the reservoir so vapor tends to concentrate on the reservoir and become absorbed by the reservoir so vapor can be extracted from the atmosphere around the sample in case a drying out of the sample should be desired.
It is an essential advantage of the new apparatus according to the invention that a complete control of temperature and humidity in the atmosphere around the biological sample is made possible.
In a preferred embodiment of the apparatus, the reservoir is shaped as a substantially flat sheet. Preferably, the thickness of the reservoir is less than 1/10 of the length, so that the external surface—also called the macroscopic surface—is large compared to the volume. It is essential that the reservoir can contain a sufficient volume of water, but it is even more essential that the surface enabling an exchange of vapor in and out of the reservoir is large enough to enable a rapid release or absorption of vapor.
In a preferred embodiment of the apparatus, the reservoir is attached to a lid, which, in a closed position, covers the at least one biological sample on the carrier member lying on a temperature-controlled plate. In another preferred embodiment of the apparatus, the reservoir is the lid, which, in a closed position, covers individual slides with individual temperature controlled plates. In yet another preferred embodiment of the apparatus, the reservoir is the lid, which, in a closed position covers several slides lying on a number of temperature-controlled plates.
Preferably, in the apparatus according to the invention, the reservoir may have a curved surface structure and uneven surfaces, such as a corrugated surface.
Preferably, the fluid in the reservoir is a liquid and the reservoir comprises a medium able to adsorb and/or absorb and desorb and/or release the liquid. Preferably, the fluid is substantially pure water. Alternatively, the fluid may be water including additives, such as an anti-microbial agent.
The fluid may comprise formamide, aqueous buffers, alcohols, dimethylformamide, dimethylsulfoxid, N-methyl-pyrolidone, non-aqueous buffers or complex mixtures containing inorganic salts, detergents, pH buffers, organic solvents, glycerol, oil and/or water, or mixtures thereof.
Preferably, the reservoir is a device made of a material having a very high internal surface area, such as artificial and natural sponges, comprising a plurality of cavities able to accommodate a fluid. Preferably at least a substantial portion of the surface(s) is hydrophilic.
Preferably, the reservoir is made of a material from the group comprising polymeric fiber composites and blends, glass fiber materials, expanded porous polymers, porous ceramics, Rockwool™, wood pulp, cardboard, leather or celluloses based materials.
Preferably, the reservoir is made of a material comprising any of the compositions from the group comprising polyethylene, polypropylene, polyurethanes, polysulfones, polyvinyl, polyamide, polyisobutylene, siloxane polymers, polyacrylic compositions, ethylene Vinyl Acetate, viscose rayon, polystyrene, macroreticular polystyrene, aliphatic, or phenol-formaldehyde condensate polymers, epoxy, cotton, polysaccharide, modified polysaccharides, wood pulp, calcium carbonate, silica gels, glass fiber, bentonite, perlite and zeolite.
Preferably, the reservoir is made of a material from the group comprising manmade or synthetic polymeric bonded, non-bonded, woven or knitted fibers, micro fibers, textiles and tufted textiles. Preferably, the reservoir is made of a material from the group comprising bonded polyamide, polyester, polyolefines and cellulose acetate fibers. Preferably, the material is made of non-woven and bonded blends of hydrophilic modified polypropylene and polyethylene micro fibers. Preferably, the material is made of bundles of fibers or other loose material retained by a thin wall of film.
Preferably, the reservoir material has a density from 0.050 to 1.5 gram/cm 3 and, more preferably, from 0.075 to 0.75 gram/cm 3 . Preferably, the reservoir material has the ability to hold at least a predefined minimum volume of liquid per carrier member. Preferably, the reservoir material has the ability to hold at least 10 micro-litres (μl) in total per carrier member, and, more preferably, more than 100 micro-litres (μl) in total per carrier member, such as more than 200 micro-litres (μl) in total per carrier member, and even more than 500 micro-litres (μl) in total per carrier member, and such as more than 1000 micro-litres (μl) in total per carrier member.
Preferably, a further reservoir is arranged on top of the lid for fluid communication with the absorbing and desorbing reservoir opposite to the biological sample. The further reservoir can easily be refilled with water without opening the hybridising chamber, and the further reservoir may be in fluid communication with the reservoir material though thin channels in the lid allowing the water to ooze or flow slowly towards the reservoir material.
The current invention has solved the problem of control of humidity from an ISH or IHC reaction by having a liquid reservoir very close to and adjacent to, preferably facing, the sample on the slide. Furthermore, the reservoir is designed for fast exchange of humidity between the liquid phase in the reservoir and the vapor phase in the space between the slide and the lid.
The invention also relates to a reservoir. The reservoir according to the invention is characterised in that the reservoir comprises a medium capable of adsorbing and/or absorbing and desorbing and/or releasing the liquid.
Preferably, the reservoir may be shaped as a substantially flat sheet or plate, so that the surface of the reservoir facing the sample is large, preferably larger than the surface of the sample. Preferably, the thickness of the reservoir is less than 1/10 of the length, in order to fit into the chamber surrounding the at least one sample. Typically, the sample support and the cover or lid forming the chamber around the sample can be designed to leave only a little free space between the sample and the cover or lid. By minimising the volume of the chamber, it is easier to limit the evaporation from the sample as well as to control the content of the atmosphere in the small chamber.
In one embodiment, the reservoir may have a curved surface structure and uneven surfaces, such as a corrugated surface, in order to increase the surface area.
Preferably, the macroscopic surface area (external surface area) of the reservoir adjacent to and/or facing the sample on the carrier member is more than 10% of the total carrier member area, and, more preferably, more than 30% of the total carrier member area and, even more preferably, more than 60%.
Preferably, the reservoir is a device made of a material having a very high internal surface area, e.g. comprising a plurality of cavities able to accommodate a fluid, or wherein the material is made of bundles of fibers or other loose material retained by a thin wall of film. Preferably, at least a substantial portion of the surface(s) is hydrophilic.
Preferably, the reservoir may be impregnated with an anti microbial agent or other protective agents. Preferably, the type, shape and size of the reservoir material are selected to optimise surface properties to match with the liquid surface tension.
The reservoir is a device that can contain liquids, e.g. water, located above or adjacent to the slides and the heating plate below the slides. The liquid can be contained in the reservoir over the slides despite the gravitational forces.
The reservoir has the ability to fast adsorb and/or absorb as well as desorb and/or release liquids. The reservoir is preferably made of a material with very high surface area.
The reservoir can be made of a number of different materials, non-limiting examples including polymeric fiber composites and blends, glass fiber materials, expanded porous polymers, porous ceramics, Rockwool™, wood pulp, cardboard, leather or celluloses based materials.
Further non-limiting examples of reservoir materials include materials containing polyethylene, polypropylene, polyurethanes, polysulfones, polyvinyl, polyacrylic, ethylene Vinyl Acetate, viscose rayon, polystyrene, macroreticular polystyrene, aliphatic, or phenol-formaldehyde condensate polymers, epoxy, cotton, polysaccharide, modified polysaccharides, wood pulp, calcium carbonate, silica gels, glass fiber, bentonite, perlite or zeolite. Even a grid of thin steel wires may provide a reservoir for a liquid.
Preferable materials include manmade or synthetic polymeric bonded, non-bonded, woven or knitted fibers, micro fibers, textiles or tufted textiles. More preferably, the materials are made of bonded polyamide, polyester, polyolefines or cellulose acetate fibers. Even more preferably, the material is made of non-woven and bonded blends of hydrophilic modified polypropylene and polyethylene micro fibers. Further, it should be understood that the reservoir material could be made of bundles of fibers or other loose material retained by a thin wall of film.
The material can be selected to optimise surface energy to match with the liquid surface tension. The surface properties of the material can be due to the bulk material or from specific chemical, plasma or irradiation surface treatments. Such treatments are well known to the person skilled in the art of polymer chemistry.
The high internal surface areas can adsorb and later desorb a wide variety of different liquids depending on the environment in which they are used. The relative humidity over the sample on the slide is a consequence of the absorption characteristics of the reservoir material and the temperature. Because of the variation options, such as the type, surface properties, shape and size of the reservoir material, the porosity, and the pore size, the broad spectrum of requirements of humidification action can be fulfilled.
The reservoir should be selected from materials having a density from 0.050 to 1.5 gram/cm 3 , and, preferably, from materials having a density from 0.075 to 0.75 gram/cm 3 . Experience has proven that such density of the preferred porous or fibrous materials provides the desired absorbing and desorbing features.
The reservoir should be selected from materials and geometrical shapes having the ability to hold at least a predefined minimum volume of liquid per carrier member or microscope slide. Preferably, the reservoir has the ability to hold at least 10 microliters in total per carrier member, and, more preferably, more than 100 microliters in total per carrier member, and, yet more preferably, more than 200 microliters in total per carrier member, and, even more preferably, more than 500 microliters in total per carrier member, and, most preferably, more than 1000 microliters in total per carrier member.
The ability to hold the water is essential, as any water drops on the sample would deteriorate the staining of the sample. Also, a high amount of water in the reservoir is important to obtain a high rate of exchange of humid air in order to maintain the desired humidity above and within the sample.
Preferably, the reservoirs are in the form of flat sheets or plates. Preferably, they may have a curved surface structure and uneven surfaces such as a corrugated surface to optimise the surface area.
Preferably, the reservoir is sufficiently rigid and stable and self-supporting, and does not creep or bend downward. Also, preferably, the reservoir does not markedly swell or change shape during desorption or adsorption of liquids or due to change in temperature.
Preferably, the reservoir is placed less than 5 cm over the slides. More preferably, the reservoir is placed less than 1.0 cm over the slides, and, yet more preferably, less than 0.50 cm over the slides.
It should be understood that the slides and reservoir could be in a tilted or vertical or horizontal position. It is the position of the reservoir adjacent to or facing the sample on the slide which is essential. Also, the arrangement of slides and reservoir could be turned upside down, so that the reservoir will be located below the slide.
The macroscopic surface area (the external surface) of the reservoirs facing towards the slides should preferably be more than 10% of the total slide area. More preferably, the area should be more than 30% of the total slide area. Even more preferably, the area should be more than 100% of the total slide area. The macroscopic surface area of the reservoirs should be understood as the external area of the reservoirs and not the internal surface area of the fibers or cavities.
In one preferred embodiment, the reservoir is attached to a lid, which comes down over the slides lying on a temperature-controlled plate. Thereby, the slides are enclosed in a closed controllable space, preferably provided with temperature sensors controlling the climate. In another embodiment, the reservoir is placed between slides and the lid, which comes down over the slides lying on a temperature-controlled plate. In yet another embodiment, the reservoir is the lid, which comes down over individual slides with individually temperature-controlled plates, or several slides lying on a temperature controlled plate or plates.
It should be understood that the cover or lid could cover one, two or several slides on the temperature-controlled plate or the individually temperature-controlled plates.
In yet further embodiments, the reservoir as described above may be further temperature controlled by a heating device above the reservoir. Preferably, one or more sensors are arranged for sensing temperature above the slide(s).
If the reservoirs are attached to the lid and are to be changed, it is preferred to have small handles or perforated taps in the material for easy manual manipulation.
Preferably, heating from beneath the slide controls the temperature of the slide and biological sample. However, it should be understood that the reservoir could also be heated. Preferably, this can be done by electrical heating wires embedded in the reservoir material or from a heating plate in the lid. This will further increase the efficiency of the reservoir's ability to humidify the air over the slides, as a pre-warmed reservoir will more easily humidify the space over the slides.
It should further be understood that the reservoir could be connected to external reservoirs by tubing or other means to allow increased capacity. Consequently the reservoir can be easily refilled. Also, different liquids can be added depending on the reaction and the protocol defining the sample processing.
It should be understood that, in some applications, the temperature might be ambient for long periods. That is, the slides may not be heated to above the ambient temperature. This is of relevance for storage of slides overnight before or after staining or for expanded incubations with reagents.
The reservoir can hold water, aqueous buffers, formamide, alcohols, dimethyl-formamide, dimethylsulfoxide, N-methyl-pyrolidone, non-aqueous buffers or complex mixtures containing inorganic salts, detergents, pH buffers, organic solvents, glycerol, oil and/or water as well as mixtures of the above-mentioned liquids.
Further, it should be understood that the composition of the liquid might include an anti microbial agent, an UV or other protective agents.
Further, it should be understood that the composition of the liquid in the reservoir might not be the same as in the vapor phase i.e. the vapor in the atmosphere in the environment between the reservoir material and the biological sample and reagents on a carrier. By adjusting the composition of the liquid in the reservoir, the composition of the vapors over the slides may be controlled. Specifically, through adjustment of the temperature of the liquid components in the reservoir, the content in the environmental vapor phase can be influenced. Experience has proven that, by maintaining a high humidity close to 100% during the relevant processing, the water content in the sample will, by the end of such processing (typically after a heating, and cooling and storing over night) be about the optimum for obtaining a perfect staining of the sample.
Further, it should be understood that the current invention especially relates to semi or fully automated instruments. Especially, computer controlled and programmable automated instruments for handling and processing slides will benefit from this invention.
The humidity above slides positioned individually, or in rack or carrousel arrangements in instruments can be controlled by the current invention. In filet, the invention is not limited to any particular arrangement of the slides on a slide platform. The reservoirs can be positioned in a stationary position adjacent to the slides.
Alternatively, the reservoirs or slides can be moved to be adjacent to each other when humidity is to be controlled. The reservoir can be single use, disposable or more permanently used in a semi or fully automated instrument.
Of particular relevance is the use of a lid made entirely or partly of the reservoir of the invention. The lid may be placed adjacent to and preferably facing the slide, and the lid controls the humidity, i.e. a sufficiently wet lid will provide for almost 100% relative humidity. Preferably, the lid is placed over the slide while the slide is positioned over a heating device. Reagents or other liquids can be added to the slide through one or several holes in the lid.
An automated dispensing device can deliver the reagents. Similarly, liquids can be added to the reservoir by automated dispensing devices in the instrument.
Further, it should be understood that the current invention would also function as a general warmer of microscope slides or other supports, by specifying a constant time and uniform temperature and humidity.
Another application, which will benefit from the current invention, is ISH on arrays. The arrays can contain thousands of spots or dots of sample. For example, the spots or dots could comprise immobilized tissue, genetic material, DNA, cDNA or RNA. The processing and visualization protocols resemble the protocols of more traditional ISH. Similarly, the control of humidity is essential for consistent results.
Applications using flat membranes or gels, like the one used in western and northern blots and treatment of electrophoresis gels will benefit from the highly controlled humidity and temperature of the current invention.
The PCR and LCR technique is only with difficulty performed in situ on samples mounted on slides. One of the problems is the lack of standardization with respect to temperature ramp time and uniform humidity control. The PCR or LCR procedures, which include repeated changes of temperature for long periods could benefit from the current invention.
Another application, which will benefit from the current invention, is the implementation of ISH on arrays. The arrays can contain thousands of spots, dots, sample dots or tissue samples on a single small or large slide or planar support. The uniformity of treatment over the many dots with respect to temperature and humidity is particularly important to ensure reproducible results.
Also, it should be understood that the current invention could reduce the humidity. The ability of the reservoir to efficiently adsorb moisture will create a dehumidifying system. As an example, such ability could be desirable when the temperature of the slide is decreased, which implies that some vapor in the air over the slide will be released as water, and this water has to be removed from the air over the slide. By having the hydrophilic reservoir, such vapor can be adsorbed on the hydrophilic fibers.
For example, by using a dry reservoir, with no or little liquid present, the high area surface removes the liquid between the space of the slides and the reservoir. This will result in fast dehydration of the slides. Furthermore, applying heat to the slides will increase the speed and efficiency of the dehydration process. For example, as described previously, the typical ISH protocol includes a dehydration step after the stringency wash step. The stringency wash is followed by two wash steps, by which the slides are immersed in a series of baths with increasing ethanol concentration and left to air-dry, before addition of mounting medium.
By using a reservoir with the capability to adsorb liquid, the number of steps in the process can be reduced. Heat applied to the slides will further speed up the process. In summary, an efficient dehumidifying system can reduce the steps and reagents needed for dehydration of slides.
The invention further relates to a method of processing biological samples wherein at least one biological sample is arranged on a carrier member, for treatment in order to prepare the sample by staining for a visual analysis of the sample, characterised by maintaining substantially at least 80% relative humidity above the sample through the close presence of a reservoir filled with water. Preferably, the method is characterized by maintaining relative humidity in the atmosphere above the sample of substantially at least 85% and, preferably, at least 90%, and, more preferably, at least 95% relative humidity and, most preferably, 99-100% relative humidity through the close presence of a reservoir, filled with water.
When carrying out the method of processing, it is preferred to supply the reservoir with water after the arrangement of the samples on the carrier members. If the lid with the reservoir material comprising the content of water is left open for a substantial time, the water may ooze downwards flowing out of the reservoir. Preferably, the lid is closed and positioned in its normal, horizontal position when it contains water—and during the processing of the samples.
Finally, the invention relates to the use of a reservoir in an apparatus for executing a method of processing biological samples, wherein at least one biological sample is arranged on a carrier member, for treatment in order to prepare the sample by staining. Experiences have indicated that the invention is particularly useful for hybridising a sample for performing an analysis in which DNA is the target, for HPV, Her-2, Top2A; for hybridising a sample for performing an analysis in which RNA is the target; for HPV; for performing MC analysis; for p16, Her-family including phosphorylated ER/PR, MIB-1, and for hybridising a sample for performing an analysis from the group comprising ISH, HPV, HER 2, HER2 FISH, Topo II, telomers, EGFr, C-Myc, Epstein-Barr virus, Herpes simplex virus and Human cytomegalo virus, Chronic Myelogenous Leukemia (CML), acute myeloid leukemia (AML), Chromosome banding and paints.
BRIEF DESCRIPTION OF THE DRAWINGS
The object and features of the present invention can be more fully understood and better appreciated with reference to the attached drawings, which are schematic representations only and not necessarily drawn to scale, wherein:
FIG. 1 shows a preferred embodiment of an apparatus in accordance with the present invention with the lid open.
FIG. 2 shows the same apparatus as in FIG. 1 with the lid closed.
FIG. 3 shows a schematic view of an arrangement of carrier members on a bottom member of the apparatus of FIG. 1 .
FIG. 4 shows a sectional view of the apparatus of FIG. 3 along the line a-a in FIG. 3 .
FIG. 5 shows a sectional view of the apparatus in FIG. 3 along the line b-b of FIG. 3 .
FIG. 5A shows a sectional view similar to FIG. 5 , but with a heating plate in the lid.
FIG. 6 shows a sectional view similar to FIG. 5 of an embodiment of an apparatus in accordance with the present invention having an external reservoir.
FIG. 7 shows the display and keypad of the apparatus of FIGS. 1 and 2 .
FIG. 8 shows a single tissue slide on a heating plate, covered by a reservoir according to an embodiment in accordance with the invention.
FIGS. 9 and 10 show a manual version of the apparatus of FIGS. 1 and 2 .
FIG. 11 shows a slide locator assisting the location of the slides on the bottom member of an apparatus as shown in FIG. 1 , 2 , 9 , or 10 .
FIG. 12 shows a sample on a slide arranged on a heating plate and covered by a reservoir and a lid according to a method of the present invention.
FIGS. 13 and 14 show an apparatus similar to the apparatus shown in FIGS. 9 and 10 , but designed for only one slide.
FIG. 15 shows a sectional view of the apparatus of FIGS. 13-14 .
FIG. 16 shows an arrangement similar to FIGS. 12-14 , including a robot arm.
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to an improved apparatus and methods for processing biological samples. The following description is presented to enable one of ordinary skill in the art to make and use the invention and is provided in the context of a patent application and its requirements. Various modifications to the preferred embodiment will be readily apparent to those skilled in the art and the generic principles herein may be applied to other embodiments. Although various components are discussed in the context of a particular initial design, it should be understood that the various elements can be altered and even replaced or omitted to permit other designs and functionality as appropriate. Thus, the present 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 described herein. To more particularly appreciate the features and advantages of preferred apparatuses and methods in accordance with the present invention, the reader is referred to the appended FIGS. 1-16 in conjunction with the following discussion. It is to be understood that the drawings are diagrammatic and schematic representations only and are neither limiting of the scope of the present invention nor necessarily drawn to scale.
FIG. 1 illustrates as an example an embodiment of an apparatus 10 according to the present invention. The apparatus comprises a bottom member 12 and a lid member 14 . Preferably, the bottom member 12 and the lid member 14 are connected through a hinge, which is not shown. In the closed position illustrated in FIG. 2 the two members provide a closed or at least semi-closed chamber.
A plurality of biological samples on carrier members 15 may be arranged on the bottom member 12 e.g. as shown in FIGS. 3 and 11 . Typically the samples may be tissue samples on microscope slides 15 . An apparatus of this kind is manufactured and sold by StatSpin, Mass., US and by DakoCytomation, Denmark A/S.
The bottom member 12 includes a temperature controlled heating plate 16 , as illustrated in FIG. 4 . The heating plate 16 can be made from heat conducting material such as a metal, e.g. such as copper. Alternatively it could be a heat-conducting polymer. The heating plate includes heating means (not shown) such as heating wires for electrical heating, as well as sensor means 34 for sensing the temperature. Such temperature regulation is well known and will not be described in further details here. Preferably, also cooling means (e.g. Peltier elements and/or fan(s) blowing air), are provided in order to enable a ramped temperature profile. The final result of the sample treatment may be highly dependent on an exact optimised temperature profile, requiring that the temperature can be changed rapidly according to the requirements defined at a protocol for the treatment of the biological samples presently arranged in the apparatus.
Preferably, the lid member 14 is provided with holding means, such as a grid, slots and/or fingers (not shown), supporting two humidity control strips 18 ( FIGS. 4-6 ), arranged to be located above the biological samples when the lid 14 is closed, thereby covering the bottom member 12 , as indicated in FIG. 2 . The strips 18 act as water reservoirs ensuring a presence of water inside the closed apparatus during the treatment of the biological samples. The strips may be attached by any known kind of attachments or adhering means, or may be integrated into the lid or cover 14 .
In a preferred embodiment, the lid member 14 may be provided with further heating and/or cooling means 16 a ( FIG. 5A ), as well as temperature sensing means. Preferably, a temperature-controlling unit in the apparatus is arranged to allow for setting the temperature of the lid to a value different from the temperature selected for the heating member 16 in the bottom member 12 in order to accelerate a release or absorption of vapor from the chamber. This could be specifically relevant during a rapid heating or cooling phase of the sample processing during which the relative humidity can be difficult to control without this extra heating or cooling of the water reservoir.
In a further embodiment, the lid member 14 may be provided with a further reservoir 28 ( FIG. 6 ) that allows refilling with liquid 28 a during the sample processing.
It is essential that the strips 18 have large internal surfaces compared to their external surfaces as well as to their total volume. The material may be of a kind comprising pores, forming the cavities accommodating the water. It is however presently preferred that the cavities are formed by spaces between randomly located bonded fibers, preferably having hydrophilic properties. The strips or reservoirs 18 can be made of a number of different materials, non-limiting examples include polymeric fiber composites and blends, glass fiber materials, expanded porous polymers, porous ceramics, Rockwool™, wood pulp, cardboard, leather or celluloses based materials.
Non-limiting examples of materials for strips or reservoirs 18 include materials containing polyethylene, polypropylene, polyurethanes, polysulfones, polyvinyl, polyacrylic compositions, ethylene Vinyl Acetate, viscose rayon, polystyrene, macroreticular polystyrene, aliphatic, or phenol-formaldehyde condensate polymers, epoxy, cotton, polysaccharide, modified polysaccharides, wood pulp, calcium carbonate, silica gels, glass fiber, bentonite, perlite or zeolite. Other preferred materials include man-made or synthetic polymeric bonded, non-bonded, woven or knitted fibers, micro fibers, textiles or tufted textiles. More preferably the materials are made of bonded polyamide, polyester, polyolefins or cellulose acetate fibers.
In the presently preferred embodiment, the strips 18 are oblong plates made of non-woven and bonded blends of hydrophilic modified polypropylene and polyethylene micro fibers. Preferably, the material has a density from 0.050 to 1.5 gram/cm 3 , more preferably from 0.075 to 0.75 gram/cm 3 . This composition provides the strips with extremely large internal surfaces. The hydrophilic properties enable the internal surfaces to adhere to tiny little water drops, providing a very large surface of water versus air, thereby enabling and improving a fast exchange and balancing between the liquid phase and the vapor phase of the water.
Preferably, the macroscopic surface area of the strips (reservoir) 18 facing towards the carrier member with the sample is more than 10% of the total carrier member area, and preferably more than 30% of the total carrier member area even more preferably more than 50% of the total carrier member area, and, in the most preferred embodiment, more than 80% of the total carrier member area.
In a presently preferred embodiment, the strips 18 are about 2 mm thick, about 28 mm wide, and about 250 mm long. This structure provides a large surface of the strip facing the surface of the sample within a short distance from the sample. Preferably, the humidity control strip is located close to the sample in order to improve the fast exchange and supply of humid air. Preferably, the strips may hold more than 10 microliters in total per slide, more preferably, more than 200 microliters in total per slide, and yet more preferably, more than 500 microliters in total per slide, and even more preferably, more than 1000 microliters in total per slide.
By mounting the control strips on the inner surface of the lid and preferably directly above the sample carriers the distance from the strips to the sample is minimized. Typically the distance may be 1 or 2 mm or even less, but always greater than zero so a layer of air and vapor separates the strip from the sample. The control strip should not get in touch with the sample.
In a further advantageous embodiment the strips may have a curved surface structure and uneven surfaces, such as a corrugated surface. Thereby the external surface comprising openings into the interior surfaces becomes large improving a rapid exchange of vapors, more specifically air and vapor of water providing almost 100% relative humidity.
In yet a further advantageous embodiment the humidity control strips 18 may have been impregnated with an anti microbial agent, an UV agent or other protective agents.
In the presently preferred embodiment the reservoir 28 is located above the sample on the carrier member so that the water supply is assisted through gravitation.
As explained earlier, a high humidity is essential to the final result of the staining of the biological samples. The presence of water is essential in order to maintain a high humidity. The treatment of the samples including several, possibly rapid temperature changes necessitates a rapid exchange between the liquid phase and the vapor phase of the water in order to ensure maintenance of a high relative humidity in the atmosphere above the samples. Such high relative humidity can be maintained through the use of the apparatus according to the invention incorporating the strips 18 .
In the presently preferred embodiment, the strips are made of materials selected for their hydrophilic properties. However, other fluids might be contemplated, and in such cases the strip material must be chosen to co-operate with such fluid, e.g. a formamide. More specifically the type, shape and size of the reservoir material should be selected to optimise surface properties to match with the liquid surface tension.
In a preferred embodiment, the apparatus comprises data processing means as well a data input and output means 20 , such as a keyboard or keypad and a display means 22 in FIGS. 1 and 7 , or is adapted for communication with a computer, such as a PC. Preferably, the data processing means may receive input from the temperature sensing means, and should be able to provide control signals to the heating and/or cooling means.
The computer may be provided with software and instructions enabling an automatic control of temperature and humidity inside the apparatus according to protocols specifying the conditions, e.g. temperatures and times, for the treatment of the samples.
In a further embodiment, the lid 14 itself is a sheet of hydrophilic material of a type or material as described previously herein for strips 18 .
Heating wires may be embedded in the hydrophilic material. Also, the material may be bi-layered.
The lid 14 may simply be arranged on top of a heating plate carrying the sample carriers (microscope slides).
The following examples show preferred methods of how to use the preferred embodiment of an automatic apparatus:
EXAMPLE A
Unit Power Up
After a user assures that the unit is plugged into an appropriate outlet, the user moves a power switch (not shown) to its “ON” position. The instrument then audibly beeps to announce that the power has been turned on, a cooling fan and heating (not shown) will start and a Main Menu as shown in Table I is displayed on display means 22 , when the heating plate in the instrument has reached a default temperature of 37° C.
TABLE I
Run a PGM
Edit a PGM
Create a PGM
Example B
Denaturation and Hybridization Program
After the Main Menu screen is displayed, a cursor on the menu highlights the “Run a PGM” line of the menu. The user then presses an “Enter” key of the input and output means 20 to accept this menu item.
Subsequently, using the arrow keys, the user scrolls through various program numbers or program names. To accept the selection of a program, the user presses the “Enter” button or key of the input and output means 20 . The display 22 then confirms the PGM number/name and Denaturation and Hybridization times and temperatures, an example of which is shown in Table II. The cursor highlights the “Run. PGM” line. The user then presses the “Enter” button or key to accept this choice.
TABLE II
PGM 01 Her2
82° C :05; 45° C 20:00
Run PGM
Main Menu
The display 22 then prompts the user to “Add Slides and Close Lid” as illustrated in Table III. Before adding slides, the user inserts two Humidity Control Strips 18 into the inside slide lid. After strip insertion, and after adding the slides, the user saturates the strips 18 with distilled water or equivalent (approx. 13 mL for dry strips). The cursor then highlights “Start” line. The user presses the “Enter” button or key to run the program.
TABLE III
PGM 01 Her2
Add Slides - Close Lid
Start
Main Menu
To return to the Main Menu, the user moves the cursor to highlight the “Main Menu” line of the display 22 and presses the “Enter” button or key. The display indicates “heating” and current temperature of the slides. Once the temperature reaches a denaturation set point, the denaturation time will count down from the set time as shown in Table IV.
TABLE IV
PGM 01 Her2
Denat in Process
Denat: 82° C. 02:28
Present Temp: 82° C.
The apparatus will then automatically cool to the hybridization set temperature once denaturation is completed (Table V).
TABLE V
Please Wait
Cooling to Hyb 45° C.
Present Temp: 58° C.
The hybridization time will then count down from the set time once temperature reaches a hybridization set point.
Upon program completion, the unit will audibly beep to alert the user and the display will show “Process Complete” as shown in Table Vi. The hybridization temperature will be maintained until an “End PGM/Main Menu” menu selection is accepted by pressing the “Enter” button of input and output means 20 . Before pressing the “Enter” button, the user may remove slides for further processing. If the “End PGM/Main Menu” selection is not accepted within the first minute of program completion, the hybridization time will start counting the total time at hybridization temperature.
TABLE VI
PGM 01 Her2
PROCESS COMPLETE
Total Hyb Time 21:05
End PGM/Main Menu
Example C
Run a Hybridization Only Program
After the Main Menu screen is displayed, a cursor on the menu highlights the “Run a PGM” line of the menu. The user then presses an “Enter” key of the input and output means 20 to accept this menu item.
Subsequently, using arrow keys, the user scrolls through various program numbers or program names. To accept the selection of a program, the user presses the “Enter” button or key of the input and output means 20 . The user selects a Hybridization Only program and the display 20 then confirms the PGM number/name and times and temperatures for a Hybridization Only protocol, examples of which are shown in Table VII. The cursor highlights the “Run PGM” line.
TABLE VII
PGM 02 EBV
Hyb: 55° C. 01:30
Run PGM
Main Menu
The user then installs two Humidity Control Strips 18 into the inside slide lid. After strip installation, and after adding the slides, the user saturates the strips 18 with distilled water or equivalent (approx. 13 mL for dry strips). The cursor highlights the “Start” line and the user then presses the “Enter” key or button to run the program as shown in Table VIII.
TABLE VIII
PGM 02 EBV
Add Slides - Close Lid
Start
Main Menu
The instrument will heat slides to the hybridization temperature as indicated in Table VIIIa.
TABLE VIIIa
Please Wait
Heating to Hyb 55° C.
Present Temp: 45° C.
Once hybridization temperature is reached the display changes as shown in table VIIIb and the time will count down from the set time.
TABLE VIIIb
PGM 02 EBV
Hyb in Process
Hyb 55° C. 01:30
Present Temp: 55° C.
Upon program completion, the unit audibly beeps to alert the user and the display 22 shows the message “Process Complete” (Table IX). The Hybridization temperature will be maintained until the “End PGM/Main Menu” selection is accepted by pressing the “Enter” button. Before pressing the “Enter” button, the user may remove slides for further processing. If the “End PGM/Main Menu” selection is not accepted within the first minute of program completion, the hybridization time will start counting the total time at hybridization temperature.
TABLE IX
PGM 02 EBV
PROCESS COMPLETE
Total Hyb Time 02:15
End PGM/Main Menu
Example D
Fixed Temperature Program
After the Main Menu screen is displayed, a cursor on the menu highlights the “Run a PGM” line of the menu. The user then presses an “Enter” key of the input and output means 20 to accept this menu item.
Subsequently, using arrow keys, the user scrolls through various program numbers or program names. To accept the selection of a program, the user presses the “Enter” button or key of the input and output means 20 . The user selects a Fixed Temperature program. The display 20 then confirms the PGM number/name and the Fixed Temperature (Table X) and the cursor highlights the “Run PGM” line of the display 22 .
TABLE X
PGM 03 Appl
Fixed: 65° C.
Run PGM
Main Menu
By pressing the “Enter” button or key of input and output means 20 to run the program the instrument will heat to the fixed temperature as indicated in Table XI.
TABLE XI Please Wait Heating to Fxd: 65° C. Present Temp: 30° C.
When the fixed temperature is reached, the display 22 then prompts the user to “Add Slides and Close Lid”. Before adding slides, the user installs two Humidity Control Strips into the inside slide lid. After strip installation, and after adding the slides the user saturates the strips 18 with distilled water or equivalent (approx. 13 mL for dry strips) and closes the lid. The cursor highlights the “Start” line on display 22 (Table XII). The user then presses the “Enter” button of the input and output means 20 to continue the program.
TABLE XII
PGM 03 Appl
Add Slides - Close Lid
Start
Main Menu
To return to the Main Menu, the user moves the cursor to highlight the “Main Menu” line of display 22 and presses the “Enter” button of input and output means 20 . The display 22 then indicates the present temperature of slides as shown in Table XIII and the timer counts elapsed time. (Pressing the “Enter” button by the user will reset the timer to zero).
TABLE XIII
PGM 03 Appl
Fixed Temp: 65° C.
Reset Timer 01:18:10
End PGM/Main Menu
The user may use the Arrow keys of the input and output means 20 to move the highlighted display to the “End PGM/Main Menu” line and then press the “Enter” button to end the program.
As the above examples (Example A through Example D) indicate, the reservoirs 18 which are the humidity control strips may be useful in a hybridizer. However they can be used in many other apparatuses. FIG. 8 and FIGS. 12-16 show a single tissue slide 15 on a heating plate 16 covered by a reservoir 18 according to the present invention. Such arrangement may be incorporated in several types of apparatus for processing samples, such as automatic stainers, both of the carousel type and as well as stainers with robots moving reagents and/or slides.
Also the arrangement shown in FIG. 8 and FIGS. 12-16 may be used in a tilted version. Also the reservoir 18 as shown in FIG. 8 may be incorporated into a lid 14 similar to the embodiment shown in FIG. 1 , but with only one reservoir and one slide 15 . A heating plate 16 a may be attached or embedded in the lid 14 , e.g. as shown in FIG. 5A .
In FIG. 16 a robot arm 30 is shown arranged above the lid 14 . The lid 14 is provided with a hole 24 providing an inlet for fluid to the reservoir 18 and enabling the robot to provide a fluid, such as water or a reagent to the reservoir and/or to the sample. This is in order to emphasize that the apparatus according to the present invention may be part of an automatic sample-processing instrument for processing a plurality of biological samples.
FIGS. 9 and 10 show a manual version of the apparatus, similar to the apparatus in FIGS. 1 and 2 , but without computer assisted control.
FIG. 11 shows a view similar to FIG. 3 , here with a slide locator 32 assisting the arrangement of 12 slides (A-L) on the bottom member of the apparatus in FIGS. 1 and 2 .
The arrangements as shown in the drawings, and, specifically, the provision of a reservoir, in cooperation with the temperature sensors (not shown) and in cooperation with adequate control units, such as a computer, allow for a precise control of the climate around tissue on a slide 15 . Specifically the hydrophilic adsorbent medium of the reservoir enables better staining results than hereto known when using automatic sample processing equipment.
In the following is presented seven examples taken from a validation test of the instrument.
In Example 1, the reservoir material was ordinary filter paper, not the recommended micro fiber material. In all other examples, the tests were carried out using the recommended micro fiber strips called “Hybridizer Humidity Control Strips”. These strips were oblong plates made of non-woven and bonded blends of hydrophilic modified polypropylene and polyethylene micro fibers.
EXAMPLE 1
FISH Validation
This is an example with TOP2A and paper filter strips. The on average acceptance criteria of TOP2A: Scoring 1.5-3 (signal intensity and specificity). A score of at least 2 on average or a deviation score within ±0.5 on average from reference is required. Individual outliers can be excluded due to obvious reasons and if these are reported. The first run with TOP2A on Hybridizer was performed with paper filter strips (Filter strips), Table 1A. The instrument was tested with twelve slides from the same tissue block and resulted in an average score of the TOP2A signal intensities that resemble the signal intensities of the manual reference slides.
The signal intensities of Green signal, Centromer 17 on Hybridizer, score 2.0, did not resemble the intensities of the manual reference, score 3. Centromer signal intensities with a score less than 1.5 were observed for two of the twelve slides. The signal intensity of Centromer 17 was, however, on average 2, Red signal, HER2 did resemble the manual references, and therefore the acceptance criteria were barely fulfilled. The table shows Raw data of TOP2A probes on sections cut from the same formalin-fixed, paraffin embedded breast cancer tissue block; Performed on a hybridizer instrument with paper filter strips as humidity strips.
TABLE 1A
Position in
Run No. 1
Slide
Hybridizer/Manual
Signal Intensity
Signal Intensity
Tissue
No.
test
Red
Green
Structure
1
1
2.5
2.5
3
2
2
2.5
2.5
3
3
3
1.5
1
3
4
4
3
2.5
3
5
5
3
2.5
3
6
6
2.5
2
3
7
7
2.5
3
3
8
8
2.5
1.5
2.5
9
9
2
1.5
2.5
10
10
3
2.5
3
11
11
2
1
2.5
12
12
2
2
3
13
Manual test
2.5
3
2.5
14
Manual test
2
3
2.5
1-12
Mean
2.4
2.0
2.9
Std
0.469
0.656
0.226
13-14
Mean
2.3
3.0
2.5
EXAMPLE 2
Example with TOP2A and DakoCytomation Hybridizer Humidity Control Strips
A run performed on the validation instrument No. 102 confirmed that the acceptance criteria were easily fulfilled if Hybridizer Humidity Control Strips (0.198 g/cm 3 ) were used instead of paper filter strips.
The instrument test run was as good as the manual procedure,
In conclusion, the Hybridizer passed the acceptance criteria for TOP2A. The scores of the slides were, when Hybridizer Humidity Control Strips were used, as good as the manual procedures.
The table (Table 1B) shows Raw data of TOP2A probes on sections cut from the same formalin-fixed, paraffin embedded breast cancer tissue block, performed on hybridizer instrument with Hybridizer Humidity Control Strips (3 mm thick, 0.198 g/cm 3 ). Green signal, Centromer 17; Red signal, HER2.
TABLE 1B
Position in
Run No. 1
Slide
Hybridizer/Manual
Signal Intensity
Signal Intensity
Tissue
No.
test
Red
Green
Structure
1
1
3
2.5
3
2
2
3
2.5
3
3
3
3
3
3
4
4
3
3
2.5
5
5
3
2.5
2.5
6
6
3
3
2.5
7
7
3
3
3
8
8
3
3
3
9
9
3
2.5
3
10
10
3
3
3
11
11
3
3
2.5
12
12
3
3
3
13
Manual test
3
3
3
1, 4
Manual test
3
3
3
1.5
Manual test
3
2.5
3
1-12
Mean
3.0
2.8
2.8
Stdv
0.000
0.246
0.246
13-15
Mean
3.000
2.833
3.000
Stdv
0.0
0.3
0.0
EXAMPLE 3
HER2
The on average acceptance criteria of HER2: Scoring 1.5-3 (signal intensity and specificity). A score of at least 2 on average or a deviation score within ±0.5 on average from reference is required. Individual outliers can be excluded due to obvious reasons and if these are reported. The run with HER2 on Hybridizer was performed with Hybridizer Humidity Control Strips (0.270 g/cm 3 ). The instrument was tested with tissue sections of different thickness (2 μm to 6 μm) from the same formalin-fixed paraffin-embedded tissue block. The run resulted in scores of signal intensities and tissue structures that resembled the manual reference. No score deviation of ±0.5 grade or above on average was observed. In conclusion, the Hybridizer passed the acceptance criteria for HER2. The scores of the slides were as good as the manual procedures. Table 2 shows raw data of the HER2 Probe; performed on hybridizer instrument with Hybridizer Humidity Control Strips (2 mm thick, 0.270 g/cm 3 ). Green signal, Centromer 17; Red signal, HER2
TABLE 2
Run No. 1
Thick-
Position in
Signal
Signal
Tissue
Slide
ness of
Hybridizer/
Intensity
Intensity
struc-
No.
Tissue
Manual test
Red
Green
ture
1
2 μm
1
3
3
2.5
2
2
3
2.5
2.5
3
3
3
3
2
4
Manual test
3
3
2.5
5
Manual test
3
3
2.5
6
4 μm
4
3
2.5
2.5
7
5
2.5
2.5
2.5
8
6
2.5
2.5
2.5
9
Manual test
2
2.5
2.5
10
Manual test
2.5
3
2.5
11
6 μm
7
3
3
3
12
8
2.5
2
3
13
9
3
3
3
14
Manual test
2.5
3
2.5
15
Manual test
2.5
3
3
1, 2, 3
2 μm
Mean
3.0
2.8
2.3
6, 7, 8
4 μm
Mean
2.7
2.5
2.5
11, 12, 13
6 μm
Mean
2.8
2.7
3.0
Manual 4, 5
2 μm
Mean
3.0
3.0
2.5
Manual 9, 10
4 μm
Mean
2.3
2.8
2.5
Manual 14, 15
6 μm
Mean
2.5
3.0
2.8
EXAMPLE 4
MLL and ETV6
The on average acceptance criteria of MLL and ETV6: Scoring 1.5-3 (signal intensity and specificity). Score deviation off ±0.5 on average from reference is allowed. Individual outliers can be excluded due to obvious reasons and if these are reported.
The run on Hybridizer was performed with Hybridizer Humidity Control Strips (0.270 g/cm 3 ). The instrument was tested with sample specimens from the same lot of metaphase spreads. The run resulted in better scores of the MLL and ETV6 signal intensities than observed with the manual references. The structure of the cells resembled the manual references. In conclusion, the Hybridizer passed the acceptance criteria for MLL and ETV6. The scores of the slides were better than the manual procedures. The scores obtained on Hybridizer were, though, for both probes more than 0.5 grade higher in signal than the manual references, These scores are above the deviations described in the acceptance criteria, but still acceptable.
Table 3 shows raw data of translocation probes, MLL and ETV6, on metaphase spreads, performed on hybridizer instrument No. 25 with Hybridizer Humidity Control Strips (2 mm thick, 0.270 g/cm 3 ).
TABLE 3
Run in Hybridizer No. 25
Structure of
Position in
Signal in
Signal in
inter- and
Slide No.
Probe mix
Hybridizer
interphases
metaphases
metaphases
Comments
1
ETV6
4
3
3
2
—
2
8
3
3
2
—
3
3
2.5
2.5
2
—
4
Manual test
2
2
2
—
5
2
2
2
—
6
MLL
5
2.5
3
2
—
7
6
2.5
2.5
2
—
8
1
2.5
2.5
2.5
—
9
Manual test
1
2
2.5
—
10
2
2
2
—
Signal of inter-
Method
and metaphases
Structure
Hybridizer 1-3
2.83 ± 0.26
2 ± 0
Hybridizer 6-8
2.58 ± 0.20
2.2 ± 0.29
Manual 4-5
2.0 ± 0
2
Manual 9-10
1.75 ± 0.5
2.25
EXAMPLE 5
This example relates to CISH validation of HPV on Formalin-fixed paraffin-embedded tissue blocks. The on average acceptance criteria of HPV on cells: 2.5-4 signal; 0 negative control; 0-1 background; ±0.25 grade divergence from manual staining (for individual slides).
The run with HPV probes on Hybridizer was performed with Hybridizer Humidity Control Strips. The signal intensities fully resembled those of the manual references. No score deviation was observed. The background levels appeared to be lower with Hybridizer than with the manual method.
In conclusion, the scores of signal intensities of the slides were as good as the manual procedure, when the hybridisation was performed with the humidity control strips
Table 4 Raw data of HPV Probe on Tissue.
The test ran on a Hybridizer with Hybridizer Humidity Control Strips.
TABLE 4
Method
Slide number
Block No.
Signal
Background
Hybridizer
1
236
3
0.25
Hybridizer
2
340
3
0.25-0.5
Hybridizer
6
340
3
0.25
Hybridizer
7
236
3
0.5
Hybridizer
11
236
3
0.5
Hybridizer
12
340
3
0.75
Manual
13
236
3
0.25
Manual
14
236
3
1
Manual
15
340
3
0.75
Manual
16
340
3
0.5
Method
Signal
Background
Hybridizer
3 ± 0
0.42-0.46 ± 0.19-0.20
Slide 1, 2, 6, 7, 11, 12
Manual
3 ± 0
0.63 ± 0.32
Slide 13-16
EXAMPLE 6
Telomere
The on average acceptance criteria of Telomere: Scoring 1.5-3 (signal intensity and specificity). Score deviation of ±0.5 on average from reference is allowed. Individual outliers can be excluded due to obvious reasons and if these are reported.
The run on Hybridizer was performed with Hybridizer Humidity Control Strips (0.22-25 g/cm 3 ). The validation instrument was tested with sample specimens from two different lots of metaphase spreads. The run resulted in scores of signal intensities and tissue structures that resembled the manual reference for both FISH (K 5325) and Cy3 (K 5326) labelled Telomere probes. No score deviation above ±0.5 grade on average was observed. The structure of the cells resembled the manual references.
In conclusion, the Hybridizer passed the acceptance criteria for Telomere. The scores of the slides were as good as the manual procedures.
Table 5: Raw data of Telomere probes, on two different metaphase spreads.
Performed on hybridizer instrument with Hybridizer Humidity Control Strips (0.22-0.25 g/cm 3 ).
TABLE 5
Average
Average
Metaphase
Position in
Signal
signal
signal
Slide No.
preparation
Probe
Hybridizer
intensity
Background
intensity
background
1
080903-
Telomere/
1
3
0
3 ± 0
0 ± 0
2
MEM
FITC
2
3
0
3
3
3
0
4
Manual
3
0
3
0
5
test
3
0
6
221203-
4
3
0.5
2.67 ± 0.29
0.5 ± 0
7
MEM
5
2.5
0.5
8
6
2.5
0.5
9
Manual
3
0
3
0
10
test
3
0
11
080903-
Telomere/
7
3
0
3 ± 0
0 ± 0
12
MEM
Cy3
8
3
0
13
9
3
0
14
Manual
3
0
3
0
15
test
3
0
16
221203-
10
3
0
3 ± 0
0 ± 0
17
MEM
11
3
0
18
12
3
0
19
Manual
3
0
3
0
20
test
3
0
EXAMPLE 7
EBER (EBV)
The on average acceptance criteria of EBER: Scoring 1.5-3 (signal intensity and specificity). Score deviation of ±0.5 on average from reference is allowed. Individual outliers can be excluded due to obvious reasons and if these are reported.
The run on Hybridizer was performed with Hybridizer Humidity Control Strips (0.22-25 g/cm 3 ). The run resulted in scores of signal intensities that resembled the manual reference. No score deviation of ±0.5 grade or above on average was observed. The background appeared to be lower with Hybridizer than with the manual method.
In conclusion, the Hybridizer passed the acceptance criteria for EBER. The scores of the slides were as good as the manual procedures.
Table 6: Raw data of EBER probes on two EBV-positive tissue.
Performed on Hybridizer instrument with Hybridizer Humidity Control Strips (0.22-0.25 g/cm 3 ).
TABLE 6
Slide
Position in
Signal
No.
Tissue
Hybridizer
Probe mix
intensity
Background
1A
A
1
EBER Y5200
2
0
1B
Neg. control
0
0
2A
2
EBER Y5200
2.5
0.5
2B
Neg. control
0
0
3A
B
3
EBER Y5200
2
0.5
3B
Neg. control
0
0
4Λ
4
EBER Y5200
2
0
4B
Neg. control
0
0
5A
A
Manual test
EBER Y5200
2.5
0.5
5B
Neg. control
0
0
6A
EBER Y5200
2.5
1
6B
Neg. control
0
0.5
7A
B
EBER Y5200
2.5
0.1
7B
Neg. control
0
0.5
8A
EBER Y5200
2
0
8B
Neg. control
0
0.5
Method
Signal intensity
Background
Hybridizer EBER 1A-4A
2.13 ± 0.25
0.25 ± 0.28
Hybridizer neg. control 1B-4B
0 ± 0
0 ± 0
Manual EBER 5A-8A
2.38 ± 0.25
0.4 ± 0.45
Manual neg. control 5B-8B
0 ± 0
0.38 ± 0.25
LIST OF REFERENCE NUMBERS
The following is a list of reference numbers used in the accompanying drawings and referred to in this specification: 10 —apparatus, Hybridizer; 12 —bottom member; 14 —lid member; 15 —carrier members, which may be microscope slides; 16 —temperature-controlled heating plate; 16 a —heating plate in lid 14 ; 18 —humidity control strips or reservoir; 20 —data input and output means including a display and key pad; 22 —display; 24 —hole; 28 —further reservoir for refilling the reservoir 18 ; 28 a —liquid within reservoir 28 ; 30 —robot arm; 32 —slide sorter.
An improved apparatus and methods for processing biological samples and a reservoir therefore have been disclosed. Although the present invention has been described in accordance with the embodiments shown and discussed, one of ordinary skill in the art will readily recognize that there could be variations to the embodiments and those variations would be within the spirit and scope of the present invention. For instance, although the preferred embodiment of the present invention is described in the context of a Hybridizer for 12 slides, it will be appreciated that the teachings of the present invention are applicable to any number of slides that are processed in any number of chambers equipped with any system for controlling temperature and humidity, e.g., in automated sample processing equipment comprising a plurality of heater plates, each of them being arranged to carry a single microscope slide with tissue. Also, even though all figures show the reservoir above the slide on the heater plate in the bottom part, it must be understood that the chamber might be turned upside down so that the reservoir would be arranged below the slide. Accordingly, many modifications may be made by one of ordinary skill in the art without departing from the spirit and scope of the invention, which is defined by the appended claims. | An apparatus for processing at least one biological sample accommodated on at least one carrier member ( 15 ) in a chamber includes, at least one reservoir ( 18 ) able to accommodate a fluid on a surface inside the chamber adjacent to and/or facing a substantial part of the at least one biological sample. The apparatus may comprise a bottom member ( 12 ) arranged to support at least one carrier member ( 15 ) carrying at least one biological sample and a lid ( 14 ) including at least one fluid reservoir ( 18 ). The reservoir filled with water provides humidity to the chamber and impedes drying out of the sample. | 8 |
TECHNICAL FIELD
[0001] The invention relates to moisture-crosslinking hotmelt adhesives.
PRIOR ART
[0002] Hotmelt adhesives (hotmelts) are polymer compositions which are solid at room temperature and which for the purpose of application are melted and applied while hot to the substrates where bonding is to take place, these substrates being joined immediately thereafter. Following its application, the hotmelt adhesive, usually applied as a thin film, undergoes rapid cooling, with the bond very rapidly developing strength as a result.
[0003] Conventional hotmelt adhesives are chemically unreactive and remain thermoplastic after application. As a consequence of this they are unsuitable for bonds exposed to elevated temperature. Moreover, they often also exhibit creep (cold flow) at temperatures far below the softening point.
[0004] These disadvantages have been largely eliminated with what are called reactive hotmelt adhesives, comprising reactive groups which lead to the crosslinking of the adhesive polymers by means of moisture. As a result of the cooling, the early strength typical of hotmelt adhesives is developed first of all, following by crosslinking of the polymers through chemical reaction, which takes place typically at room temperature and may take a number of hours to several days. Following crosslinking, the bond can be heated without the adhesive melting. The chemical crosslinking of the adhesive means that the cold flow is prevented as well.
[0005] Polyurethane hotmelt adhesives, especially those containing isocyanate groups are widely used. A disadvantage of these systems is that they tend to form blisters on crosslinking, particularly in the case of amorphous polymers and in conditions of increased moisture or temperature. The blisters may severely detract from the aesthetic and mechanical quality and also from the stability of the bond. A further disadvantage is the presence therein of airway-irritant monomeric isocyanates, which may outgas during application and may necessitate protective measures. This results in a higher hazard classification for the products, thereby restricting their usefulness.
[0006] Instead of systems containing isocyanate groups, it is possible to use silane group-containing systems (“STP hotmelt adhesives”). These adhesives crosslink by way of the condensation reaction of silanol groups, which form from the silane groups by hydrolysis, and allow a low hazard classification because of the low monomeric isocyanate content. The silane groups are most easily introduced by reaction of an isocyanate group-containing polyurethane hotmelt adhesive with an aminosilane or a mercaptosilane, as described for example in EP 0 202 491 and EP 1 801 138. These systems known from the prior art, however, have disadvantages. On prolonged heating during application, STP hotmelt adhesives prepared by way of aminosilanes may abruptly thicken up severely and so become impossible to apply. This is a great disadvantage especially for applications in industrial manufacture where the adhesive spends a certain time in the melted state at the application temperature. While STP hotmelt adhesives prepared by way of mercaptosilanes do not thicken up in the melted state, they do have the disadvantage that the attachment of the silane group, especially at elevated temperature, is reversible and hence on application there is release of intensely odorous mercapto compounds, a highly undesirable phenomenon. EP 0 354 472 describes STP hotmelt adhesives obtained using isocyanatosilanes. The isocyanatosilanes used are obtained from mercapto- or aminosilanes by reaction with diisocyanates and dialcohols. In this process the silane groups are likewise bonded to the polymer via urea and/or thiourethane groups, meaning that the difficulties identified above continue to exist.
DESCRIPTION OF THE INVENTION
[0007] It is an object of the present invention, therefore, to provide a method for producing a silane group-containing hotmelt adhesive that permits a low hazard classification and exhibits high thermal stability in the melted state, in other words exhibiting no tendency toward premature thickening and giving off no unpleasant odors.
[0008] Surprisingly it has been found that the method of claim 1 achieves this object. It involves reacting a hydroxysilane which is free from urea groups and from thiourethane groups with an isocyanate group-containing polyurethane polymer which is solid at room temperature. The silane group-containing hotmelt adhesive obtainable by the method of the invention permits a low hazard classification since, depending on the stoichiometry deployed, it has a low or zero monomeric isocyanate content. Even on sustained heating, during the duration of the application procedure, it exhibits high thermal stability and shows no tendency toward premature thickening; as a result, it is easy to apply, without causing any emissions, since the silane groups are attached largely irreversibly. Lastly, it undergoes blister-free crosslinking at room temperature under the influence of moisture, and results in an optically and mechanically high-grade and robust adhesively bonded assembly.
[0009] The preparation and handling of hydroxysilanes carries the difficulty that the silanes tend toward self-condensation, owing to a rapid reaction of the hydroxyl group with the silane group, and are therefore frequently highly impure and/or of low storage stability. In particular, however, the preferred hydroxysilanes having a secondary hydroxyl group are surprisingly stable enough to enable access thereby to silane group-containing hotmelt adhesives with high strength.
[0010] Further aspects of the invention are subjects of further independent claims. Particularly preferred embodiments of the invention are subjects of the dependent claims.
Ways of Implementing the Invention
[0011] A subject of the invention is a method for producing a silane group-containing hotmelt adhesive by reacting at least one isocyanate group-containing polyurethane polymer which is solid at room temperature with at least one hydroxysilane which is free from urea groups and from thiourethane groups.
[0012] In the present document, the term “silane” or “organosilane” refers to silicon compounds which on the one hand have at least one, customarily two or three, hydrolyzable substituents bonded directly to the silicon atom via Si—O bonds, and on the other hand have at least one organic radical bonded directly to the silicon atom via an Si—C bond. The hydrolyzable substituents here represent, in particular, alkoxy, acetoxy, ketoximato, amido, or enoxy radicals.
[0013] A “silane group” is the silicon-containing group bonded to the organic radical of a silane.
[0014] A “hydroxysilane”, “aminosilane”, “isocyanatosilane”, and the like are organosilanes which have a corresponding functional group on the organic radical, i.e., a hydroxyl group, amino group, or isocyanate group.
[0015] Substance names beginning with “poly”, such as polyol or polyisocyanate, denote substances which in formal terms include two or more per molecule of the functional groups that occur in their name.
[0016] The term “polyurethane polymer” encompasses all polymers which are prepared by the diisocyanate polyaddition process. The term “polyurethane polymer” also encompasses polyurethane polymers containing isocyanate groups, of the kind which are obtainable from the reaction of polyisocyanates and polyols and which themselves constitute polyisocyanates and are often also called prepolymers.
[0017] “Active hydrogen” refers to the hydrogen atoms of hydroxyl, mercapto, and primary and secondary amino groups.
[0018] “Molecular weight” is understood in the present document to be the molar mass (in grams per mole) of a molecule. “Average molecular weight” means the number average M n of an oligomeric or polymeric mixture of molecules, and is customarily determined by GPC using polystyrene as a standard.
[0019] A dashed line in the formulae in this document represents in each case the bond between a substituent and the associated remainder of the molecule.
[0020] A “primary hydroxyl group” is an OH group which is bonded to a C atom having two hydrogens; a “secondary hydroxyl group” is an OH group which is bonded to a C atom with one hydrogen.
[0021] The term “storage-stable” denotes the capacity of a substance or of a composition to be storable at room temperature in a suitable container for a number of weeks up to 6 months or more, without changing in its application or service properties to an extent relevant for its use, as a result of such storage. “Room temperature” refers to a temperature of about 23° C.
[0022] The reaction of the isocyanate group-containing polyurethane polymer which is solid at room temperature with the hydroxysilane is carried out advantageously with exclusion of moisture and at an elevated temperature, more particularly at a temperature at which the polyurethane polymer is in liquid form. The reaction is accomplished preferably by the isocyanate group-containing polyurethane polymer and the hydroxysilane being reacted at a temperature in the range from 60 to 180° C., more particularly 80 to 160° C., with hydroxyl groups of the hydroxysilane undergoing reaction with isocyanate groups present to form urethane groups. As a result, the silane groups are bonded covalently to the polyurethane polymer. A catalyst can be used here, more particularly a bismuth(III), zinc(II), zirconium(IV), or tin(II) compound or an organotin(IV) compound.
[0023] The attachment of the silane groups via urethane groups has the great advantage here that the hotmelt adhesive obtained exhibits very good thermal stability both in the noncrosslinked state and in the crosslinked state. This thermal stability on the part of the noncrosslinked adhesive is important for its good applicability. Hotmelt adhesives whose silane groups are bonded to the polymer via urea groups or thiourethane groups exhibit weaknesses in this respect. The thiourethane group in particular is easily splittable by heat, releasing sulfur-containing substances which lead to instances of odor pollution. In the case of urea groups as well, an instability is observed which leads—presumably as a result of catalytic processes—to severe thickening or even gelling of the adhesive in the melted state.
[0024] One embodiment of the invention uses the polyurethane polymer and the hydroxysilane in an amount such that the OH groups of the hydroxysilane are present substoichiometrically in relation to the isocyanate groups of the polyurethane polymer, meaning that the OH/NCO ratio is less than 1. This reaction produces a silane group-containing hotmelt adhesive which additionally has isocyanate groups. In a hotmelt adhesive of this kind, both the silane groups and the isocyanate groups contribute to crosslinking under the influence of moisture. A hotmelt adhesive of this kind has a significantly reduced monomeric isocyanate content by comparison with the isocyanate group-containing polyurethane polymer used for the method described. An OH/NCO ratio in the range from 0.1 to 0.9 is preferred, 0.2 to 0.8 particularly preferred, and 0.3 to 0.7 more particularly. A hotmelt adhesive of this kind has in particular a monomeric isocyanate content of <2 weight %, more particularly <1 weight %. Because of labeling regulations, a hotmelt adhesive of this kind has, in particular, a monomeric MDI content of <1 weight %, or a monomeric IPDI content of <2 weight %, more particularly <0.5 weight %, with the abbreviation “MDI” representing “4,4′-, 2,4′- and/or 2,2′-diphenylmethane diisocyanate and any desired mixtures of these isomers” and the abbreviation “IPDI” representing “isophorone diisocyanate”.
[0025] A preferred embodiment of the invention uses the polyurethane polymer and the hydroxysilane in an amount such that the OH groups of the hydroxysilane are present at least stoichiometrically in relation to the isocyanate groups of the polyurethane polymer, meaning that the OH/NCO ratio is at least 1. This reaction produces a silane group-containing hotmelt adhesive which is free from isocyanate groups. An isocyanate group-free hotmelt adhesive of this kind is particularly advantageous from a toxicological standpoint. An isocyanate group-free hotmelt adhesive, correspondingly, is also free from monomeric isocyanates. A preferred OH/NCO ratio is in the range from 1 to 2, more preferably 1 to 1.8, more particularly 1 to 1.5.
[0026] The method described uses at least one isocyanate group-containing polyurethane polymer which is solid at room temperature. At room temperature it may be crystalline, semicrystalline, or amorphous. For a semicrystalline or amorphous polyurethane polymer the rule is that it has only little or no fluidity at room temperature. This means in particular that its viscosity at 20° C. is more than 5000 Pa·s.
[0027] The isocyanate group-containing polyurethane polymer preferably has an average molecular weight M n in the range from 2000 to 20 000 g/mol, preferably 2000 to 15 000 g/mol, more particularly 2000 to 10 000 g/mol.
[0028] The isocyanate group-containing polyurethane polymer preferably has 1 to 3, more preferably 2, isocyanate groups per molecule.
[0029] A polyurethane polymer of this kind permits a suitable processing viscosity and good mechanical properties in the crosslinked state.
[0030] A suitable isocyanate group-containing polyurethane polymer which is solid at room temperature is obtained in particular through the reaction of at least one polyol with at least one diisocyanate, the diisocyanate being present in a stoichiometric excess.
[0031] A preferred ratio between isocyanate groups and hydroxyl groups is in the range from 1.5 to 5, more preferably 1.8 to 4, more particularly 2 to 3.
[0032] The reaction is carried out advantageously at elevated temperature, more particularly at a temperature at which the polyols and diisocyanates used and the polyurethane polymer formed are in liquid form. A suitable catalyst is optionally present.
[0033] In the reaction of polyols with diisocyanates to give an isocyanate group-containing polyurethane polymer, the statistical distribution of the possible reaction products means that a residual amount of unreacted monomeric diisocyanates remains in the polymer formed. These monomeric diisocyanates, also called “monomeric isocyanates” for short, are volatile compounds and may be harmful to health on account of their irritant, allergenic and/or toxic effect.
[0034] Suitable polyol comprises, in particular, polyols which are solid at room temperature.
[0035] Particularly suitable are polyols which are amorphous or semicrystalline or crystalline at room temperature, more particularly polyester polyols and polycarbonate polyols.
[0036] Especially suitable polyester polyols are those prepared from di- to trihydric, preferably dihydric, alcohols, such as, in particular, 1,2-ethanediol, diethylene glycol, 1,2-propanediol, dipropylene glycol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, neopentyl glycol, glycerol, 1,1,1-trimethylolpropane, or mixtures of the aforesaid alcohols, with organic dicarboxylic acids or anhydrides or esters thereof, such as, in particular, succinic acid, glutaric acid, adipic acid, suberic acid, sebacic acid, dodecanedicarboxylic acid, maleic acid, fumaric acid, phthalic acid, isophthalic acid, terephthalic acid, and hexahydrophthalic acid, or mixtures of the aforesaid acids, and also polyester polyols from lactones such as, for example, from ε-caprolactone.
[0037] Particularly suitable polyester polyols are polyester polyols formed from adipic acid, sebacic acid, or dodecanedicarboxylic acid as dicarboxylic acid and from hexanediol or neopentyl glycol as dihydric alcohol. The polyester polyols preferably have an average molecular weight M n in the range from 1500 to 15 000 g/mol, preferably 1500 to 8000 g/mol, more particularly 2000 to 5500 g/mol.
[0038] Particularly suitable crystalline or semicrystalline polyester polyols are adipic acid/hexanediol polyesters and dodecanedicarboxylic acid/hexanediol polyesters.
[0039] Suitable polycarbonate polyols are those as obtainable in particular through reaction of the abovementioned alcohols—those used to synthesize the polyester polyols—with dialkyl carbonates, diaryl carbonates, or phosgene.
[0040] Preferred as polyol is a mixture of at least one amorphous polyester diol and at least one further polyester diol.
[0041] Particularly preferred as polyol are mixtures of amorphous and/or crystalline and/or semicrystalline polyester diols. With more particular preference the polyol is a mixture of an amorphous polyester diol and a polyester diol which is liquid at room temperature. In this way it is possible, for example, to produce transparent adhesives.
[0042] Likewise preferably the polyol is a crystalline or a semicrystalline polyester diol. Suitable diisocyanate comprises, in particular, commercially available aliphatic, cycloaliphatic, arylaliphatic, and aromatic, preferably cycloaliphatic and aromatic, diisocyanates.
[0043] Preferred diisocyanates are 1,6-hexamethylene diisocyanate (HDI), 2,2,4- and 2,4,4-trimethyl-1,6-hexamethylene diisocyanate (TMDI), cyclohexane-1,3- and 1,4-diisocyanate and any desired mixtures of these isomers, 1-isocyanato-3,3,5-trimethyl-5-isocyanatomethylcyclohexane (i.e., isophorone diisocyanate or IPDI), perhydro-2,4′- and -4,4′-diphenylmethane diisocyanate (HMDI), m- and p-xylylene diisocyanate (m- and p-XDI), m- and p-tetramethyl-1,3- and -1,4-xylylene diisocyanate (m- and p-TMXDI), 2,4- and 2,6-tolylene diisocyanate (TDI) and any desired mixtures of these isomers, and 4,4′-, 2,4′-, and 2,2′-diphenylmethane diisocyanate and any desired mixtures of these isomers (MDI).
[0044] More preferably the diisocyanate is selected from the group consisting of IPDI, MDI, and TDI. These diisocyanates are particularly easily obtainable.
[0045] Preferred among these is MDI. Hotmelt adhesives based thereon have particularly good mechanical properties and rapid crosslinking.
[0046] Further preferred among these is IPDI. Hotmelt adhesives based thereon have particularly good light stability and stability with respect to discoloration. This is advantageous especially for the bonding of transparent substrates.
[0047] The method described also uses at least one hydroxysilane which is free from urea groups and from thiourethane groups.
[0048] The difficulty in preparing and storing hydroxysilanes is basically that a hydroxyl group can react with a silane group and, in so doing, release a hydrolyzable group (“self-condensation”). In principle this is possible both intra- and inter-molecularly, with either cyclic silanes or more highly condensed or oligomeric silane compounds having a plurality of silicon atoms being formed. Such impurities may form even during the preparation of hydroxysilanes, or during storage.
[0049] The hydroxysilane preferably has two or three hydrolyzable substituents on the silicon atom, preferably two or three alkoxy groups, more particularly ethoxy or methoxy groups. With particular preference the hydroxysilane has two or three, more particularly three, ethoxy groups. Hydroxysilanes having ethoxy groups are particularly stable with respect to self-condensation.
[0050] The hydroxysilane is preferably a hydroxysilane which comprises a secondary hydroxyl group. These hydroxysilanes, surprisingly, are sufficiently stable to produce silane group-containing hotmelt adhesives with high strength.
[0051] The method of the invention uses more particularly a hydroxysilane of the formula (I),
[0000]
[0000] where
A either is a divalent aliphatic or cycloaliphatic hydrocarbon radical having 2 to 30 C atoms, optionally with aromatic fractions and optionally with one or more heteroatoms, which is free from active hydrogen,
or together with B—CH is a divalent cycloaliphatic hydrocarbon radical having 6 to 20 C atoms, optionally with aromatic fractions and optionally with one or more heteroatoms, which is free from active hydrogen;
B is a monovalent aliphatic or cycloaliphatic hydrocarbon radical having 1 to 12 C atoms, optionally with one or more heteroatoms, which is free from active hydrogen,
or together with CH-A is a divalent cycloaliphatic hydrocarbon radical having 6 to 20 C atoms, optionally with one or more heteroatoms, which is free from active hydrogen;
R 4 is an alkyl group having 1 to 8 C atoms; R 5 is an alkyl group having 1 to 10 C atoms, optionally with one or more ether oxygens; and x is 0 or 1 or 2.
[0059] The hydroxysilane of the formula (I) has a secondary hydroxyl group and is particularly advantageous in the use according to the invention, since it is preparable in high purity and exhibits high storage stability, and so permits very neat functionalization of the isocyanate group-containing polyurethane polymer with silane groups,—consequently, a silane group-containing hotmelt adhesive with high strength is obtainable.
[0060] Preferably, A either is a divalent aliphatic or cycloaliphatic hydrocarbon radical having 4 to 30 C atoms, which optionally comprises ether oxygen, a tertiary amino group, an amido group, or a urethane group, or together with B—CH is a divalent cycloaliphatic hydrocarbon radical having 6 to 20 C atoms, which optionally comprises ether groups and/or tertiary amino groups.
[0061] Preferably, B is an alkyl group having 1 to 12 C atoms, which optionally comprises ether groups and/or tertiary amino groups, or together with CH-A is a divalent cycloaliphatic hydrocarbon radical having 6 to 20 C atoms, which optionally comprises ether groups and/or tertiary amino groups.
[0062] R 4 is preferably an alkyl group having 1 to 4 C atoms, more particularly methyl.
[0063] R 5 is preferably an alkyl group having 1 to 4 C atoms, more particularly methyl or ethyl.
[0064] Hydroxysilanes with these preferred radicals A, B, R 4 , and R 5 are particularly readily available.
[0065] R 5 more particularly is a methyl group. Accordingly, silane group-containing hotmelt adhesives exhibiting particularly rapid moisture crosslinking are obtainable.
[0066] R 5 , moreover, is in particular an ethyl group. Obtainable accordingly are silane group-containing hotmelt adhesives which do not give off methanol on moisture crosslinking, something which is advantageous on grounds of toxicology. Preferably, x is 1 or 0, more particularly. With these hydroxysilanes, hotmelt adhesives are obtainable which crosslink particularly quickly on contact with moisture and exhibit particularly good mechanical properties.
[0067] The hydroxysilane of the formula (I) is preferably a hydroxysilane which has not been obtained from the addition reaction of an amino silane with a methyl-substituted cyclic carbonate, such as propylene carbonate in particular. This addition reaction is not very selective, meaning that as well as the hydroxysilane with secondary OH group, the reaction product includes a relatively high level of hydroxysilane with primary OH group. As a result, laborious purification of the reaction product is necessary and/or the storage stability and purity of the silane are greatly reduced, meaning that the strength of the resulting hotmelt adhesive in the crosslinked state is no more than moderate.
[0068] A suitable hydroxysilane of the formula (I) is a hydroxysilane which has a tertiary amino group. Hydroxysilanes of this kind are obtainable in particular from the reaction of at least one epoxy silane with at least one secondary amine. A hydroxysilane having a tertiary amino group is especially suitable for reaction with a polyurethane polymer based on aliphatic isocyanates, more particularly IPDI. Hotmelt adhesives derived therefrom exhibit high thermal stability in the noncrosslinked state, and good light stability.
[0069] A preferred hydroxysilane with a tertiary amino group is a hydroxysilane of the formula (I a),
[0000]
[0000] where
either R′ is a radical of the formula (II) and R″ is hydrogen
or R′ is hydrogen and R″ is a radical of the formula (II);
[0000]
R 1a and R 2a either individually are each an alkyl radical having 1 to 12 C atoms, which optionally has heteroatoms in the form of ether oxygen, thioether sulfur, or tertiary amine nitrogen, or together are an alkylene radical having 2 to 12 C atoms which optionally has heteroatoms in the form of ether oxygen, thioether sulfur, or tertiary amine nitrogen;
R 3a is a linear or branched alkylene or cycloalkylene radical having 1 to 20 C atoms, optionally with aromatic fractions, and optionally with one or more heteroatoms;
and R 4 , R 5 , and x have the definitions already stated.
[0073] The hydroxysilane of the formula (I a) corresponds either to the formula (I a′) or to the formula (I a″).
[0000]
[0074] In the formulae (I a′) and (I a″), R 1a , R 2a , R 3a , R 4 , R 5 , ad x have the definitions already stated.
[0075] The formulae (I a′) and (I a″) encompass all diastereomers possible for the structure in question.
[0000] R 1a and R 2a preferably
either individually are each an alkyl radical having 3 to 10 C atoms which optionally has one or two ether oxygens, or together are an alkylene radical having 4 to 8 C atoms which in particular has a heteroatom in the form of ether oxygen, thioether sulfur, or tertiary amine nitrogen and with inclusion of the nitrogen atom form a 5- or 6- or 7-membered ring, more particularly a 5- or 6-membered ring.
R 1a and R 2a more preferably
either individually are 2-methoxyethyl, 2-ethoxyethyl, 3-methoxypropyl, 3-ethoxypropyl, 2-(2-methoxyethoxy)ethyl, 2-octyloxyethyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, 2-ethylhexyl, or N,N-dimethylamino-propyl, or together, with inclusion of the nitrogen atom, are an optionally substituted pyrrolidine, piperidine, hexamethyleneimine, morpholine, thiomorpholine, or 4-methylpiperazine ring.
[0080] Very preferably R 1a and R 2a are each individually 2-methoxyethyl, butyl, or isopropyl, or together, with inclusion of the nitrogen atom, are morpholine, 2,6-dimethylmorpholine, thiomorpholine, pyrrolidine, or 4-methylpiperazine.
[0081] Most preferably R 1a and R 2a with inclusion of the nitrogen atom are morpholine or pyrrolidine.
[0082] These hydroxysilanes can be prepared in a particularly pure quality, and are particularly storage-stable. They enable silane group-containing hotmelt adhesives of high strength.
[0083] R 3a is preferably a linear or branched alkylene radical having 1 to 6 C atoms, more preferably a 1,2-ethylene radical.
[0084] A preferred hydroxysilane of the formula (I a) is in particular selected from the group consisting of 2-bis(2-methoxyethyl)amino-4-(2-triethoxysilylethyl)cyclohexan-1-ol, 2-dibutylamino-4-(2-triethoxysilylethyl)cyclohexan-1-ol, 2-diisopropylamino-4-(2-triethoxysilylethyl)cyclohexan-1-ol, 2-morpholino-4-(2-triethoxysilylethyl)cyclohexan-1-ol, 2-(2,6-dimethylmorpholino)-4-(2-triethoxy-silylethyl)cyclohexan-1-ol, 2-thiomorpholino-4-(2-triethoxysilylethyl)cyclohexan-1-ol, 2-pyrrolidino-4-(2-triethoxysilylethyl)cyclohexan-1-ol, 2-(4-methylpiperazino)-4-(2-triethoxysilylethyl)cyclohexa-1-ol, and the corresponding compounds in which the silane radical is in position 5 rather than in position 4, and the corresponding compounds with methoxy groups instead of ethoxy groups on the silane.
[0085] Preferred among these are 2-morpholino-4-(2-trimethoxysilylethyl)cyclohexan-1-ol, 2-morpholino-4-(2-triethoxysilylethyl)cyclohexan-1-ol, 2-pyrrolidino-4-(2-trimethoxysilylethyl)cyclohexan-1-ol, 2-pyrrolidino-4-(2-triethoxysilylethyl)cyclohexan-1-ol, and the corresponding compounds in which the silane radical is in position 5 rather than in position 4.
[0086] With these hydroxysilanes, silane group-containing hotmelt adhesives are obtained that have good processing viscosity and good storage stability, and which cure rapidly with moisture to form crosslinked adhesives of high strength. Particularly preferred in each case is a mixture of the two molecules in which the silane radical is present in positions 4 and 5. Such mixtures are also represented by the notation “4(5)”.
[0087] A hydroxysilane of the formula (I a) is preferably reacted with a polyurethane polymer having aliphatic isocyanate groups. The hotmelt adhesives obtained accordingly exhibit high thermal stability in the noncrosslinked state, and good light stability.
[0088] A further preferred hydroxysilane with a tertiary amino group is a hydroxysilane of the formula (I b),
[0000]
[0000] where
R 1b and R 2b either individually are each an alkyl radical having 1 to 12 C atoms, which optionally has heteroatoms in the form of ether oxygen, thioether sulfur, or tertiary amine nitrogen, or together are an alkylene radical having 2 to 12 C atoms which optionally has heteroatoms in the form of ether oxygen, thioether sulfur, or tertiary amine nitrogen; R 3b is a linear or branched alkylene or cycloalkylene radical having 1 to 20 C atoms, optionally with aromatic fractions, and optionally with one or more heteroatoms; and R 4 , R 5 , and x have the definitions already stated.
R 1b and R 2b preferably
either individually are each an alkyl radical having 3 to 10 C atoms which optionally has one or two ether oxygens, or together are an alkylene radical having 4 to 8 C atoms which in particular has a heteroatom in the form of ether oxygen, thioether sulfur, or tertiary amine nitrogen and with inclusion of the nitrogen atom form a 5- or 6- or 7-membered ring, more particularly a 5- or 6-membered ring.
R 1b and R 2b more preferably
either individually are 2-methoxyethyl, 2-ethoxyethyl, 3-methoxypropyl, 3-ethoxypropyl, 2-(2-methoxyethoxy)ethyl, 2-octyloxyethyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, 2-ethylhexyl, or N,N-dimethylamino-propyl, or together, with inclusion of the nitrogen atom, are an optionally substituted pyrrolidine, piperidine, hexamethyleneimine, morpholine, thiomorpholine, or 4-methylpiperazine ring.
[0096] Very preferably R 1b and R 2b are each individually 2-methoxyethyl, butyl, or isopropyl, or together, with inclusion of the nitrogen atom, are morpholine, 2,6-dimethylmorpholine, thiomorpholine, pyrrolidine, or 4-methylpiperazine.
[0097] Most preferably R 1b and R 2b With inclusion of the nitrogen atom are morpholine or pyrrolidine.
[0098] These hydroxysilanes can be prepared in a particularly pure quality, and are particularly storage-stable. They enable silane group-containing hotmelt adhesives of high strength.
[0099] R 3b is preferably a linear or branched alkylene radical having 1 to 6 C atoms, more particularly a 1,3-propylene radical. These hydroxysilanes are particularly readily available.
[0100] A preferred hydroxysilane of the formula (I b) is, in particular, selected from the group consisting of 1-morpholino-3-(3-(triethoxysilyl)propoxy)propan-2-ol, 1-(2,6-dimethylmorpholino)-3-(3-(triethoxysilyl)propoxy)propan-2-ol, bis(2-methoxyethyl)amino-3-(3-(triethoxysilyl)propoxy)propan-2-ol, 1-pyrrolidino-3-(3-(triethoxysilyl)propoxy)propan-2-ol, 1-piperidino-3-(3-(triethoxysilyl)propoxy) propan-2-ol, 1-(2-methylpiperidino)-3-(3-(triethoxysilyl)propoxy)propan-2-ol, dibutylamino-3-(3-(triethoxysilyl)propoxy)propan-2-ol, diisopropylamino-3-(3-(triethoxysilyl)propoxy)propan-2-ol, and the corresponding compounds with methoxy groups instead of ethoxy groups on the silane.
[0101] Preferred among these is 1-morpholino-3-(3-(triethoxysilyl)propoxy)propan-2-ol.
[0102] With these hydroxysilanes, silane group-containing hotmelt adhesives are obtained that have good processing viscosity and good storage stability, and which cure rapidly with moisture to form crosslinked adhesives having good mechanical properties.
[0103] A hydroxysilane of the formula (I b) is preferably reacted with a polyurethane polymer having aliphatic isocyanate groups. The hotmelt adhesives obtained accordingly exhibit high thermal stability in the noncrosslinked state, and good light stability.
[0104] A further suitable hydroxysilane of the formula (I) is a hydroxysilane which is free from tertiary amino groups. These hydroxysilanes are particularly suitable for reaction with a polyurethane polymer based on highly reactive aromatic isocyanates, especially MDI. Hotmelt adhesives derived therefrom exhibit high thermal stability in the noncrosslinked state, and particularly good mechanical properties.
[0105] In one embodiment, a hydroxysilane of this kind is a hydroxysilane with a urethane group. Such a hydroxysilane is obtained in particular from the reaction of at least one isocyanatosilane with at least one diol, more particularly a diol having at least one secondary hydroxyl group. Particularly suitable are reaction products of isocyanatosilanes such as 3-isocyanatopropyl-triethoxysilane and diols such as 1,2- or 1,3-butanediol, 1,2-pentanediol, 1,2-hexanediol, 1,2-octanediol, 2-ethyl-1,3-hexanediol, or 2,2,4-trimethyl-1,3-pentanediol, in a molar ratio of approximately 1:1.
[0106] A suitable hydroxysilane of the formula (I) which is free from tertiary amino groups is, moreover, a hydroxysilane with an amido group. A hydroxysilane of this kind is obtained in particular from the reaction of at least one aminosilane with at least one lactone, more particularly with a lactone substituted in alpha-position to the ring oxygen.
[0107] A preferred hydroxysilane with an amido group is a hydroxysilane of the formula (I c),
[0000]
[0000] where
R 1c is an alkyl group having 1 to 12 C atoms; R 2c is a hydrogen atom or is an alkyl group having 1 to 12 C atoms which optionally has ether oxygen or amine nitrogen; R 3c is a linear or branched alkylene or cycloalkylene radical having 1 to 20 C atoms, optionally with aromatic fractions, and optionally with one or more heteroatoms; and n is 2 or 3 or 4; and R 4 , R 5 , and x have the definitions already stated.
[0113] R 1c is preferably a linear alkyl group having 1 to 8 C atoms, more particularly methyl, n-butyl, n-pentyl, n-hexyl, n-heptyl, or n-octyl.
[0114] R 2c is preferably a hydrogen atom.
[0115] Preferably n is 2 or 3, more particularly 2.
[0116] These hydroxysilanes are preparable in particularly pure quality and are particularly storage-stable. They permit silane group-containing hotmelt adhesives of high strength with particularly high thermal stability in the noncrosslinked state, including, in particular, those based on aromatic isocyanates such as especially MDI.
[0117] R 3c is preferably a linear or branched alkylene radical having 1 to 6 C atoms, more particularly a radical selected from the group consisting of 1,3-propylene, 2-methyl-1,3-propylene, 1,4-butylene, 3-methyl-1,4-butylene, and 3,3-dimethyl-1,4-butylene, preferably 1,3-propylene and 3,3-dimethyl-1,4-butylene, more particularly 1,3-propylene. These hydroxysilanes are particularly readily available.
[0118] A preferred hydroxysilane of the formula (I c) is, in particular, selected from the group consisting of N-(3-triethoxysilylpropyl)-4-hydroxypentanamide, N-(3-triethoxysilylpropyl)-4-hydroxyoctanamide, N-(3-triethoxysilylpropyl)-4-hydroxynonanamide, N-(3-triethoxysilylpropyl)-4-hydroxydecanamide, N-(3-triethoxysilylpropyl)-4-hydroxyundecanamide, N-(3-triethoxysilylpropyl)-4-hydroxydodecanamide, N-(3-triethoxysilylpropyl)-5-hydroxyhexanamide, N-(3-triethoxysilylpropyl)-5-hydroxynonanamide, N-(3-triethoxysilylpropyl)-5-hydroxydecan amide, N-(3-triethoxysilylpropyl)-5-hydroxyundecanamide, N-(3-triethoxysilylpropyl)-5-hydroxydodecanamide, and the corresponding compounds having methoxy groups instead of ethoxy groups on the silane.
[0119] Preferred among these are N-(3-triethoxysilylpropyl)-4-hydroxypentanamide and N-(3-triethoxysilylpropyl)-4-hydroxyoctanamide.
[0120] With these hydroxysilanes, silane group-containing hotmelt adhesives with good storage stability are obtained which exhibit high thermal stability in the noncrosslinked state—even in the case of hotmelt adhesives based on aromatic isocyanates—and which cure rapidly with moisture to form crosslinked adhesives, and which exhibit good mechanical properties.
[0121] Particularly preferred in the method described are the hydroxysilanes of the formula (I a). These hydroxysilanes are particularly storage-stable, thereby simplifying their handling in the method described.
[0122] Most preferred in the method described are the hydroxysilanes of the formula (I c). They permit silane group-containing hotmelt adhesives based on aromatic isocyanates and having good thermal stability in the noncrosslinked state.
[0123] The silane group-containing hotmelt adhesive obtained by the method described may comprise further constituents, especially the following auxiliaries and adjuvants:
further crosslinkable polymers, especially polymers having silane groups and/or having isocyanate groups; nonreactive thermoplastic polymers, especially homo- or copolymers of unsaturated monomers, more particularly from the group encompassing ethylene, propylene, butyl, isobutylene, isoprene, vinyl acetate, and alkyl (meth)acrylate, more particularly polyethylene (PE), polypropylene (PP), polyisobutylene, ethylene-vinyl acetate copolymers (EVA), and atactic poly-α-olefins (APAO); additionally polyesters, polyacrylates, polymethacrylates, polyacrylamides, polyacrylonitriles, polyimides, polyamides, polyvinyl chlorides, polysiloxanes, polyurethanes, polystyrenes, and combinations thereof, especially polyetheramide copolymers, styrene-butadiene-styrene copolymers, styrene-isoprene-styrene copolymers, styrene-ethylene-butylene-styrene copolymers, styrene-ethylene-propylene-styrene copolymers; and also, furthermore, butyl rubber, polyisobutylene, and combinations thereof, and also asphalt, bitumen, crude rubber, fluorinated rubber, and cellulose resins; tackifier resins, especially a hydrocarbon resin such as, in particular, coumarone-indene resins, terpene resins, phenol-modified terpene resins, natural, optionally modified resins such as, in particular, rosin, tung resin or tall oil resin, and also α-methyl-styrene resins and polymeric lactic acid; plasticizers, especially carboxylic esters such as phthalates or adipates, polyols, organic phosphoric and sulfonic esters, or polybutenes; catalysts for the crosslinking reactions, especially metal catalysts and/or nitrogen-containing compounds, more particularly organotin compounds, organotitanates, amines, amidines, guanidines, and imidazoles; stabilizers to counter oxidation, heat, hydrolysis, light, and UV radiation, biocides, fungicides, and flame retardants; drying agents, especially tetraethoxysilane, vinyltrimethoxy- or vinyltriethoxy-silane, and organoalkoxysilanes, having a functional group in α-position to the silane group, more particularly N-(methyldimethoxysilylmethyl)-O-methyl carbamate, (methacryloyloxymethyl)silanes, methoxymethylsilanes, orthoformic esters, and also calcium oxide or molecular sieves; adhesion promoters and/or crosslinkers, especially silanes such as aminosilanes, mercaptosilanes, epoxysilanes, (meth)acrylosilanes, anhydridosilanes, carbamatosilanes, alkylsilanes, and iminosilanes; inorganic and organic fillers, especially mineral fillers, molecular sieves, silicas including finely divided silicas from pyrolysis processes, industrially manufactured carbon blacks, graphite, metal powders, PVC powders, or hollow beads; dyes;
and also further substances in common use in reactive hotmelt adhesives.
[0134] It may be advisable to carry out chemical or physical drying of certain constituents before adding them.
[0135] Such auxiliaries and adjuvants may be present even before the method described is carried out, especially as a constituent of the isocyanate group-containing polyurethane polymer which is solid at room temperature. Alternatively, such auxiliaries and adjuvants may not be added to the resulting silane group-containing hotmelt adhesive until after the method described has been carried out.
[0136] The method described results in a silane group-containing hotmelt adhesive. The silane group-containing hotmelt adhesive preferably comprises silane group-containing polyurethane polymer solid at room temperature in an amount in the range from 5 to 100 weight %, more particularly 15 to 95 weight %, very preferably 30 to 90 weight %, most preferably 50 to 80 weight %.
[0137] The silane group-containing hotmelt adhesive preferably comprises at least one further polymer selected from the group consisting of nonreactive thermoplastic polymers and tackifier resins.
[0138] The amount of polymers in the silane group-containing hotmelt adhesive, including the silane group-containing polyurethane polymer which is solid at room temperature, is preferably in the range from 70 to 100 weight %, more preferably 80 to 100 weight %, more particularly 90 to 100 weight %.
[0139] In one preferred embodiment, the silane group-containing hotmelt adhesive is free from organotin compounds. This may be advantageous on environmental and/or toxicological grounds.
[0140] In a further preferred embodiment, the silane group-containing hotmelt adhesive releases no methanol in the course of its crosslinking. This may be advantageous on environmental and/or toxicological grounds.
[0141] Where the method described has been carried out with a substoichiometric amount of hydroxysilane, the silane group-containing hotmelt adhesive comprises a polyurethane polymer containing both isocyanate groups and silane groups. A hotmelt adhesive of this kind comprises a significantly reduced level of monomeric isocyanates in comparison to before the method described is carried out. This is advantageous on toxicological grounds.
[0142] Where the method described has been carried out with an at least stoichiometric amount of hydroxysilane, the silane group-containing hotmelt adhesive is ultimately free from isocyanates. A hotmelt adhesive of this kind is particularly advantageous on toxicological grounds.
[0143] With exclusion of moisture, the silane group-containing hotmelt adhesive is very storage-stable. Before being used, it can be kept in a suitable pack or contrivance over a period ranging from several months up to a year or more. On contact with moisture, the silane groups undergo hydrolysis, leading ultimately to crosslinking of the adhesive. In this process, silanol groups may undergo condensation with, for example, hydroxyl groups of the substrate on which the adhesive is applied, and as a result of this, in the course of crosslinking, there may be additional improvement of the adhesion of the adhesive on the substrate. Where the hotmelt adhesive comprises isocyanate groups as well as the silane groups, the isocyanate groups likewise react with moisture, making an additional contribution to the crosslinking of the adhesive. The moisture needed for crosslinking may either come from the air (atmospheric humidity), or the adhesive may be contacted with a water-comprising component, by being coated or sprayed with such a component, for example.
[0144] On being employed, the silane group-containing hotmelt adhesive is applied in the liquid state to at least one substrate. For this purpose, the adhesive is initially heated at least to an extent that it is in liquid form. The adhesive is applied typically at a temperature in the range from 80 to 200° C., more particularly 100 to 180° C.
[0145] During processing, the noncrosslinked adhesive exhibits high thermal stability. This is evident from the fact that the adhesive can be left in the hot liquid state for a time sufficient for proper application, more particularly of up to several hours, without any undue increase in its viscosity, more particularly without gelling occurring, and without instances of odor pollution arising.
[0146] The applied adhesive is advantageously joined to a second substrate to give an adhesive bond, before it has excessively solidified as a result of cooling. Alternatively, it can solidify in the applied state and at a later point in time be melted again and joined to a second substrate to form an adhesive bond. In that case it is necessary to ensure that the renewed melting of the adhesive takes place before the crosslinking of its reactive groups disrupts the melting process. For this purpose it may be advantageous to protect the applied adhesive from ingress of moisture prior to solidification, in particular by covering it with a protective film.
[0147] The solidification of the adhesive as a result of cooling brings about a very rapid development of strength and a high initial strength of adhesion of the bond. In addition to this physical adhesive curing, there is also crosslinking via silane groups and optionally isocyanate groups by moisture in the adhesive, after the solidification, as described earlier. This chemical crosslinking leads ultimately to a fully cured, crosslinked adhesive, which cannot be melted again by reheating to the application temperature.
[0148] Preferred substrates which can be bonded using the silane group-containing hotmelt adhesive from the method described are
glass, glass-ceramic, concrete, mortar, brick, tile, plaster, and natural stone such as granite or marble; metals and alloys, such as aluminum, iron, steel, and nonferrous metals, and also surface-enhanced metals and alloys, such as galvanized or chromed metals; leather, textile, paper, wood, woodbase materials bonded with resins, such as with phenolic, melamine or epoxy resins, resin-textile composites, and other so-called polymer composites; plastics, such as polyvinyl chloride (rigid and flexible PVC), acrylonitrile-butadiene-styrene copolymers (ABS), polycarbonate (PC), polyamide (PA), polyesters, poly(methyl methacrylate) (PMMA), epoxy resins, polyurethanes (PU), polyoxymethylene (POM), polyolefins (PO), polyethylene (PE) or polypropylene (PP), ethylene/propylene copolymers (EPM) and ethylene/propylene/diene terpolymers (EPDM), and also fiber-reinforced plastics such as carbon fiber-reinforced plastics (CRP), glass fiber-reinforced plastics (GRP), and sheet molding compounds (SMC), it being possible for the plastics to have been surface-treated preferably by means of plasma, corona, or flaming; coated substrates, such as powder-coated metals or alloys; paints and coatings, more particularly automotive topcoats.
[0155] Particularly preferred among these are plastics, textiles, leather, wood, woodbase materials, polymer composites, paper, metals, paints and coatings. The substrates may be pretreated before the adhesive is applied, by means for example of physical and/or chemical cleaning, or by the application of an adhesion promoter, an adhesion promoter solution, or a primer.
[0156] Bonding may be between two similar substrates or two different substrates. Either the adhesive is applied to one of the two substrates and joined to the other to form a bond, or it may be applied to both of the substrates to be bonded.
[0157] Preference is given to the bonding of two different substrates.
[0158] The silane group-containing hotmelt adhesive from the method described can be used in particular for construction and industrial applications, more particularly as laminating adhesive, laminate adhesive, packaging adhesive, textile adhesive, or wood adhesive. It is particularly suitable for bonds in which the bonding location is visible, more particularly for the bonding of glass, in vehicle and window construction, for example, and also for the bonding of transparent packaging.
[0159] The use of the silane group-containing hotmelt adhesive from the method described results in an article.
[0160] Preferred articles are automotive interior equipment components such as, in particular, roof linings, sun visors, instrument panels, door side parts, parcel shelves, and the like, wood fiber materials from the bath and shower sector, decorative furniture foils, membrane films with textiles such as, in particular, cotton, polyester films in the clothing sector, composites of textiles and foams for automotive equipment, and transparent packaging.
[0161] The silane group-containing hotmelt adhesive obtained from the method described has a series of advantages.
[0162] It permits a low hazard classification, since depending on the stoichiometry employed it contains little or no monomeric isocyanates. Before being used, it can be stored in a suitable moisture tight container over a period ranging from several months to a year, without detraction from its good application facility. On heating to a temperature in the range from 80 to 200° C., more particularly 100 to 180° C., it has a viscosity at which it is easily applied, and in the hot liquid state it is highly stable, in contrast to aminosilane-based and mercaptosilane-based, silane group-containing hotmelt adhesives from the prior art, which tend toward severe increases in viscosity to the point of gelling, or to instances of odor nuisance.
[0163] At room temperature under the influence of moisture, the adhesive crosslinks without blisters and leads to an optically and mechanically high-grade adhesively bonded assembly with excellent adhesion and high resistance to environmental influences.
EXAMPLES
[0164] Set out below are working examples which are intended to elucidate the above-described invention in more detail. The invention is of course not confined to these working examples described.
[0165] “Standard conditions” refers to a temperature of 23±1° C. and a relative atmospheric humidity of 50±5%.
[0166] Viscosities were determined on a thermostated plate/plate viscometer, Rheotec RC30 (plate diameter 25 mm, distance 1 mm, shear rate 10 s −1 ) at a temperature of 160° C.
1. Preparation of Polyurethane Polymer Containing Isocyanate Groups
Polymer P1
[0167] A mixture of 1200.0 g of amorphous polyester diol solid at room temperature (Dynacoll® 7150 from Evonik; OH number 43 mg KOH/g) and 1200.0 g of polyester diol liquid at room temperature (Dynacoll® 7250 from Evonik; OH number 22 mg KOH/g) was dried and degassed under reduced pressure at 120° C. for 2 hours, then admixed with 348.4 g of 4,4′-methylenediphenyl diisocyanate (Desmodur® 44 MC L from Bayer), stirred under reduced pressure at 130° C. for 2 hours, and subsequently cooled and stored in the absence of moisture. The resulting polyurethane polymer was solid at room temperature and had a free isocyanate group content of 2.15 weight %.
2. Preparation of Hydroxysilane
[0168] Hydroxysilane S-1: N-(3-Triethoxysilylpropyl)-4-hydroxypentanamide In a round-bottom flask, 100.0 g (452 mmol) of 3-aminopropyltriethoxysilane and 54.3 g (542 mmol) of γ-valerolactone were stirred under a nitrogen atmosphere at 140° C. for about 8 hours until progress of reaction was no longer ascertained using IR. The crude product was aftertreated at 80° C. and about 2 mbar for 30 minutes. This gave a liquid product having a theoretical OH equivalent weight of 321.5 g.
3. Reaction of the Polyurethane Polymer Containing Isocyanate Groups
Example 1
Hotmelt Adhesive K-1
[0169] A mixture of 200.0 g (about 102.4 mmol NCO) of melted polymer P1 and 36.2 g (about 112.6 mmol) of hydroxysilane S-1 was stirred under nitrogen at 120° C. for 2 hours until isocyanate was no longer detectable by IR spectroscopy. Then 40 mg of dibutyltin dilaurate were added and the resulting polymer containing silane groups was cooled and stored in the absence of moisture.
[0170] The hotmelt adhesive K-1 is free from isocyanate groups.
Example 2
Hotmelt Adhesive K-2
[0171] A mixture of 200.0 g (about 102.4 mmol NCO) of melted polymer P1 and 16.45 g (about 51.2 mmol) of hydroxysilane S-1 was stirred under nitrogen at 120° C. for 2 hours until the isocyanate band showed no further decrease by IR spectroscopy. Then 40 mg of dibutyltin dilaurate were added and the resulting polymer containing silane groups was cooled and stored in the absence of moisture.
[0172] The hotmelt adhesive K-2 comprises isocyanate groups as well as the silane groups.
Comparative Example 1
Hotmelt Adhesive Ref-1
[0173] A mixture of 200.0 g (about 102.4 mmol NCO) of melted polymer P1 and 26.85 g (about 112.6 mmol) of 3-mercaptopropyltriethoxysilane were stirred under nitrogen at 120° C. for 2 hours until the isocyanate band no longer showed any further decrease by IR spectroscopy. Then 40 mg of dibutyltin dilaurate were added and the resulting polymer containing silane groups was cooled and stored in the absence of moisture.
[0174] The silane group-containing hotmelt adhesive Ref-1 was obtained from comparative example 1. It was observed that this adhesive smells only slightly of mercaptosilane at room temperature and is free from isocyanate groups according to IR spectroscopy. In the melted state at 120° C., a very strong odor of mercaptosilane is perceptible, and IR spectroscopy indicates that isocyanate groups are present again. This is an indication that the thermal stability of the thiourethane bond is so low that some of the mercaptosilane is released under the hot conditions.
Comparative Example 2
Hotmelt Adhesive Ref-2
[0175] 200.0 g (about 102.4 mmol NCO) of melted polymer P1 were admixed at 120° C. with 25.0 g (about 112.9 mmol) of 3-aminopropyltriethoxysilane (Dynasylan® AMEO from Evonik) and the mixture was stirred under nitrogen. The mixture gelled during the preparation.
4. Properties of the Resulting Hotmelt Adhesives
Monomeric 4,4′-methylenediphenyl diisocyanate content
[0176] The monomeric isocyanate content was determined by HPLC.
[0177] The polymer P1 contained 2.60 weight % of 4,4′-methylenediphenyl diisocyanate.
[0178] The hotmelt adhesive K-2 contained 0.63 weight % of 4,4′-methylenediphenyl diisocyanate, in other words a significantly reduced amount.
Thermal Stability in the Noncrosslinked State:
[0179] A number of aluminum tubes were filled with freshly prepared, melted hotmelt adhesive and sealed and then stored in a forced air oven at 160° C. The viscosity was determined in each case on the fresh material (“0 h”) and after 2 h, 4 h, and 6 h of storage at 160° C. The results are reported in table 1.
[0000]
TABLE 1
Viscosity of inventive hotmelt adhesives K-1
and K-2 and of comparative adhesive Ref-1.
Hotmelt adhesive
K-1
K-2
Ref-1
Viscosity
after 0 h
99
84
19.5
(160° C.)
after 2 h
97
106
16.7
after 4 h
139
303
17.3
after 6 h
148
gelled
17.3
Odor
none
none
severe
Mechanical Properties:
[0180] For the determination of the mechanical properties, the respective hotmelt adhesive was pressed to a film with a thickness of 1 mm between two PTFE-coated sheets in a heatable press, and the film was cooled, the PTFE-coated sheets were removed, and dumbbell-shaped test specimens with a length of 75 mm, a crosspiece length of 30 mm and a crosspiece width of 4 mm were punched from the film. For each hotmelt adhesive, three test specimens were measured 3 h after manufacture (identified as “fresh” in table 2), and three further specimens were measured after storage under standard conditions for 10 days (identified in the table as “10d SC”). Determinations were made of tensile strength (force at break), elongation at break, and elasticity modulus (within the stated elongation range) in accordance with DIN EN 53504 at a tensioning speed of 200 mm/min. The results are reported in table 2.
[0000]
TABLE 2
Mechanical properties of inventive hotmelt
adhesives K-1 and K-2 and of polymer P1.
Hotmelt adhesive
K-1
K-2
Polymer P1
fresh:
tensile strength [MPa]
1.44
2.21
0.11
elongation at break [%]
1960
1040
60
elast. modulus (0.5-5%) [MPa]
2.74
3.19
0.82
elast. modulus (0.5-25%) [MPa]
1.15
1.41
0.20
elast. modulus (0.5-50%) [MPa]
0.63
0.81
0.04
appearance
clear
clear
clear
10 d
tensile strength [MPa]
5.64
9.56
10.40
SC:
elongation at break [%]
960
580
460
elast. modulus (0.5-5%) [MPa]
3.00
4.92
6.90
elast. modulus (0.5-25%) [MPa]
1.42
2.57
3.55
elast. modulus (0.5-50%) [MPa]
0.87
1.70
2.37
appearance
no
few
few
blisters
small
large
blisters
blisters | A method for producing a hot melt adhesive containing silane groups, in which at least one polyurethane polymer which contains isocyanate groups and is solid at room temperature is reacted with at least one hydroxysilane that is devoid of urea and thiourethane groups. The hot melt adhesive containing silane groups obtained from the method allows a low hazard classification, has a good degree of thermal resistance when melted such that, even upon application under prolonged heating, it does not tend towards premature thickening, releases no unpleasant odours, and crosslinks at room temperature without bubbles under the influence of moisture, resulting in an optically and mechanically high-quality and resistant adhesive connection. | 2 |
TECHNICAL FIELD
[0001] The present invention relates in general to notebook size computers and in particular to the physical and signal interface of removable input/output (I/O) devices to a notebook computer.
BACKGROUND INFORMATION
[0002] Notebook computers have wide usage and are usually selected for their small size. Sometimes an application for a notebook computer does not require the smallest size but rather requires portability and the ability to add options when needed. Notebook computers typically require cabling to add some optional devices (e.g., printers and larger displays) which plug into ports that have the appropriate connector for the particular option. Other optional devices may be self contained (e.g. auxiliary storage units) and plug into a compatible connector and reside inside the notebook computer. One of the limitations of notebook computers is their small display screen size and small keyboard size. To remedy this problem some notebook computers have been made with means to expand the keyboard from a smaller stored form factor and many notebook computers have external display ports for optionally using an external display either concurrent with or instead of the attached display.
[0003] Traditionally, the keyboard area of a notebook has been reserved for devices that have an input only function, such as a keypad, track ball or other type of pointing device. There have also been notebook computers with printer ports and ports for connecting to a larger display, however, these devices are usually not portable and the I/O connections are generally in the back of the keyboard base. Recently digital devices have been introduced that have functionality when not connected to computer (e.g., digital cameras). However, these devices may have information that may be loaded into a computer for further processing or storage and may also receive output data from a computer. While these devices may have a standardized electrical interfaces (e.g., USB serial bus) their physical and electrical interface are not necessarily designed to make these I/O devices conveniently operate as part of the notebook computer.
[0004] Therefore, there is a need for a notebook computer with I/O device connectivity in combination with a widened display screen where the traditional features of the notebook are enhanced with the ability to connect new and existing I/O devices with a new display form factor.
SUMMARY OF THE INVENTION
[0005] A notebook computer is disclosed with a keyboard base containing a keyboard and an attached display. The keyboard base is widened to create a widened I/O area. The display is also widened corresponding to the widened keyboard base. In one embodiment, a recessed area is provided within the widened I/O area which has an I/O connector adapted for a number of removable I/O devices. Each of the I/O devices is operable to electrically connect to the I/O connector. While the I/O devices may vary in functionality, they are all adapted to physically and electrically connect to the I/O connector. I/O devices may also have software drivers, necessary to interface to the notebook computer, either resident in the I/O device or in the notebook computer. Connection of an I/O device may automatically cause the I/O device drivers to be loaded into the notebook computer from the I/O device or the device drivers may be stored and activated from within the notebook computer itself. The widened display may use the extended display space to either display multiple windows for normal notebook operation or to display a window associated only with the operation of a particular I/O device installed in the recessed area in the widened keyboard base and connected to the I/O connector. Selected I/O devices may have functionality wholly separate from any communication or connection with the notebook computer.
[0006] 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.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] 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:
[0008] [0008]FIG. 1 illustrates a notebook computer with a widened display screen and how an I/O device may connect to an I/O connector in a widened keyboard base;
[0009] [0009]FIG. 2 illustrates a notebook computer with a widened display screen and an I/O device installed in the widened I/O area where the widened screen is used to display multiple windows side by side for a notebook computer application program;
[0010] [0010]FIG. 3 illustrates a notebook computer with a widened display screen and an I/O device installed in the widened I/O area where an I/O device window is show displayed in a widened portion of the notebook computer display;
[0011] [0011]FIG. 4 illustrates logic units and embodiments of the present invention useable in a notebook computer; and
[0012] [0012]FIG. 5 illustrates a flow diagram of method steps used in embodiments of the present invention.
DETAILED DESCRIPTION
[0013] In the following description, numerous specific details are set forth to provide a thorough understanding of the present invention. However, it will be obvious to those skilled in the art that the present invention may be practiced without such specific details. In other instances, well-known circuits have been shown in block diagram form in order not to obscure the present invention in unnecessary detail. For the most part, details concerning timing considerations and the like may have been omitted in as much as such details are not necessary to obtain a complete understanding of the present invention and are within the skills of persons of ordinary skill in the relevant art.
[0014] Refer now to the drawings wherein depicted elements are not necessarily shown to scale and wherein like or similar elements are designated by the same reference numeral through the several views. In the following description, the term I/O device will be synonymous with a “removable I/O device” as the invention is drawn to I/O devices that are removable from a notebook computer.
[0015] [0015]FIG. 4 is a block diagram of logic units within a motherboard 400 of a notebook computer (not shown in FIG. 4) useable with embodiments of the present invention. The central processing unit (CPU), read only memory (ROM) and random access memory (RAM) make up the majority of the processing function of the notebook computer. Bus 412 is one communication path used to communicate between the logic units and external devices. A user interface adapter 422 (including a keyboard controller) is used to couple signals from devices such as a keyboard 101 , a mouse 426 , a track ball 432 and an audio speaker 428 . Keyboard 101 may have a widened keyboard base 107 with an widened I/O device area 108 according to embodiments of the present invention. A display adapter 436 is used to couple signals to a display 102 . Display 102 may also have an widened display area 103 corresponding to a widened keyboard base 107 according to embodiments of the present invention. Bus 412 may also be used to couple signals from I/O adapter 418 and communication adapter 443 . Adapters 418 is used, according to embodiments of the present invention, to couple signals from an I/O device 449 to motherboard 400 via I/O connection means 434 . In one embodiment of the present invention, I/O device 449 has a connector 450 that is operable to mate with a corresponding connector 448 on I/O connection means 434 . In another embodiment of the present invention, where connectors 448 and 450 are not matched, an interposer 444 is inserted between these two connectors to enable signal connection. Interposer 444 would have a connector features compatible with connector 450 on the I/O device 449 side and a connector feature compatible with connector 448 on the I/O connection means 434 side. The signals wires (not shown) within the interposer 444 would make the required corresponding signal connections to ensure operation of I/O device 449 . An interposer 444 may also be used, in embodiments of the present invention, when the physical form of the connector on an I/O device 449 or a physical feature of the I/O device 449 itself does not allow connection of the I/O device 449 directly to the motherboard 400 via connector 448 . Other communication signals from other devices (not shown) may be coupled to bus 412 via communication adapter 443 .
[0016] Once CPU 410 recognizes a device by its identifying signals it may also have programs with instructions to retrieve, from RAM 414 , ROM 416 , or from the I/O device 449 itself, data specific to the operation of the identified I/O device 449 . This data may include device driver instructions or other pertinent operational information. CPU 410 may also activate software routines that have instructions used to communicate with display adapter 436 to present, on an I/O device display window 111 , data specific to the operation of a specific connected I/O device 449 . This I/O device display window 111 may be wholly separate and not overlay any other operation windows (e.g., 109 ) on a display 102 . An I/O device 449 with specific I/O device display window 111 may be used to indicate, to a user, operation status of I/O device 449 . For example, I/O device display window 111 may indicate; whether a communication link has been established, any additional instructions to the user concerning actions to be taken, or it may be used to display I/O data in various forms. The I/O device display may also contain data which has been received from or is to be transmitted to I/O device 449 .
[0017] I/O device display window 111 may be used without interrupting other notebook computer display window information. Other embodiments of the present invention allow an widened display 102 (with a widened area 103 ) to be used by the CPU 410 to display windows (e.g., 109 and 110 in FIG. 2) of a notebook computer application program if no I/O device 449 is present an using the widened display area 103 . An I/O device 449 may be self contained and be wholly operable as a stand alone device when not communicating with notebook computer devices via a motherboard 400 . The I/O connection means 434 allows newly developed devices to be easily adapted to an existing notebook computer containing embodiments of the present invention.
[0018] An I/O device 449 may be supplied with an interposer 444 to allow required signals to be coupled via an I/O adapter 418 and bus 412 to a CPU 410 . Even though the new I/O device 449 was previously unknown, it may still be adaptable to load, into CPU 410 , software that would fully enable synergistic operation of the I/O device 449 and a notebook computer with CPU 410 . The downloaded software may have instructions operable for later identification of the I/O device 449 with display functions for the widened display area 103 (see FIG. 3).
[0019] [0019]FIG. 1 is an illustration of a notebook computer comprising embodiments of the present invention. Notebook computer 100 has a keyboard 101 and display screen 102 . Embodiments of the present invention widen the base 107 creating an widened area 108 . Widened area 108 has a recessed I/O area 105 which contains I/O connection means 104 . Recessed I/O area 105 is operable to accept one of a group of universal I/O devices 106 . I/O devices 106 may be sized to fit into the I/O area 105 (or adapted possibly using an interposer) to mate with I/O connection means 104 . Notebook computer 100 also has, as the result of extension of the base 107 , an widened I/O display area 103 . I/O display area 103 makes the display 102 more useable either by enabling a single very wide window, two or more smaller windows side-by side, or optionally an inserted window supporting an added I/O device installed or connected in recessed I/O area 105 . I/O connection means 104 may contain sensing means to indicate to the central processing unit (CPU) of the notebook computer 100 the identity of an added I/O device 106 , if necessary. The CPU (not shown, e.g., 410 ) may reside on a mother board (e.g., 400 ) which also contains necessary electronic circuits for the notebook computer 100 . The CPU is operable to automatically load drivers and software necessary to support an added I/O device 106 . The sensing means in the I/O connection means 104 , in one embodiment of the present invention, may be a selected number of connector pins that receive encoded logic signals from the added I/O device and couple these signals to the CPU. In another embodiment of the present invention, an added I/O device 106 sends a serial set of bits defining its identity on a specific connector pin of the I/O connection means 104 . Other sensing means, for determining an I/O device identity, may include applying a logic signal to a selected single pin which is coupled to the CPU which the CPU has been programmed to associate with a particular I/O device 106 .
[0020] Many different I/O devices are possible using embodiments of the present invention. A list of possible I/O devices includes, but is not limited to, a numeric keypad, a trackpad/digitizer, a track pad with integrated display, a Work Pad or other personal digital assistant (PDA), a digital camera pad, a MP3 Pad, a Fingerprint sensor, Control Pad, a Phone Pad, a Cellular Pad, and a SmartCard reader/recorder. A “pad” in this context is a term used to define an I/O unit which has the features necessary to provide the particular I/O function (e.g., buttons, keys, audio input/output, display, etc.). A keypad may be a simple input device for inputting key data where the keypad has a particular keypad layout or specific user characters. A trackpad/digitizer may be a device that is used over a drawing where a reference may be established and data inputted by moving over figures and inputting coordinates of points. Some devices like a PDA or a digital camera pad may have a complete functionality wholly separate from communication to the notebook computer. A Phone Pad or Cellular Pad contain the functionality to make phone calls using either the standard telephone protocol or wireless via a cellular connection. The notebook may use the functionality of the Phone Pad or Cellular Pad to make either voice or data connections. For example a user may want to use the Cellular Pad in conjunction with the notebook computer to make a voice connection and talk while accessing and displaying data or operating an application program. Other devices like the Fingerprint sensor may be used for a variety of security protocol applications (e.g., granting access to certain local or remote files). A Smartcard reader/recorder is a device used to read and write specially formatted cards that may contain data storage either magnetically, optically or by accessing embedded memory chips within the Smartcard.
[0021] In one embodiment of the present invention, plugging in an I/O device 106 into I/O connection means 104 would trigger the enhanced notebook computer 100 to present a display window (e.g., 111 ) indicating which supported I/O device drivers are installed. The user would then select, from the options, the particular I/O device 106 . In another embodiment of the present invention, the notebook computer automatically loads the appropriate I/O device driver by sensing the particular I/O device 106 connected. Yet in another embodiment of the present invention, the I/O device 106 stores its required I/O driver in internal ROM. The I/O driver may be automatically loaded into the notebook computer when the I/O device 106 is coupled to I/O connection means 104 . Other embodiments of the present invention also bring up a supporting display window (e.g., 111 ) in the extended display area 103 for use with the I/O device 106 . The extended display area 103 would also be available for notebook computer application program use whether or not an I/O device 106 is connected. This would be very useful for displaying two pages side by side during an editing or review process.
[0022] [0022]FIG. 2 illustrates an embodiment of the present invention of a notebook 100 with an installed I/O device 106 . Widened keyboard base 107 contains a keyboard 101 . Display 102 has an extended display area 103 . In this illustration, two display windows 109 and 110 are shown displayed side by side where display window 110 extends into extended display area 103 .
[0023] [0023]FIG. 3 illustrates an embodiment of the present invention where a notebook computer 100 has a I/O device 106 installed. Widened keyboard base 107 contains a keyboard 101 . Display 102 has a widened display area 103 . In this illustration, display windows 109 and 112 are in display 101 . An I/O display window 111 , associated with I/O device 106 , is displayed in the widened display area 103 .
[0024] [0024]FIG. 5 is a flow diagram of method steps in embodiments of the present invention. In step 501 , a test is executed to determine if a I/O device 106 is coupled to the universal connection means is sending communication requests. If the result of the test in 501 is NO, then a test is done in step 502 to determine if a notebook application program has a requirement that may use the widened display area 103 . If the result of the test in step 502 is YES, then the widened display area 103 may be used for the notebook application program. If the result of the test in step 502 is NO, then a branch is executed to step 501 awaiting an I/O device 106 connection or a requirement by an notebook application program that may use of the widened display 103 . If the result of the test in step 501 is YES, then communication requests of an activated and installed I/O device 106 are acknowledged in step 504 . In step 505 , communication software within the notebook computer 100 requests I/O device 106 identification. In step 506 , the particular I/O device driver program is either downloaded to or activated within the notebook computer 100 . In step 507 , the I/O display window program is activated in the notebook or downloaded from the I/O device 106 . In step 508 , the notebook computer 100 and the I/O device 106 are operated together under user commands entered via the keyboard 101 of notebook computer 100 or via the I/O device 106 . In step 509 , a test is executed to determine if operation the I/O device 106 active or terminated. If the result of the test in step 509 is YES, a branch is executed back to step 508 continuing operation. If the result of the test in step 509 is NO, then a branch to step 501 is executed in step 510 awaiting communication requests from an I/O device.
[0025] Although the present invention and its advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims. | A notebook computer with an extended keyboard base and widened display. The extended keyboard base region adjacent to the keyboard has a recessed area which contains a universal I/O connector. The recessed area is designed to fit a set of I/O devices which are designed to electrically connect to the universal I/O connector. When a I/O device is plugged into the universal I/O connector, it may be automatically sensed by circuitry internal to the notebook computer and software drivers are loaded that enables the particular I/O device to be used. The widened display gives added display capability wherein multiple pages of a document may be placed side by side for editing or viewing. I/O devices include, but are not limited to, a numeric keypad, a trackpad/digitizer, a track pad with integrated display, a WorkPad, a digital camera pad, a MP3Pad, a Fingerprint sensor, Control Pad, a PhonePad, a Cellular Pad, and a SmartCard reader/recorder. | 6 |
CROSS REFERENCE
This application is a continuation of U.S. patent application Ser. No. 10/718,876 filed Nov. 21, 2003 now U.S. Pat. No. 6,849,531, and entitled, “Phosphoric Acid Free Process for Polysilicon Gate Definition,” which is hereby incorporated by reference in its entirety.
BACKGROUND
The present invention relates to methods used to fabricate semiconductor devices, and in some embodiments, to a method used to define a polysilicon gate structure for a metal oxide semiconductor field effect transistor (MOSFET) device.
Micro-miniaturization, or the ability to fabricate semiconductor devices with sub-micron features, has allowed the performance of the sub-micron device to be increased while the fabrication cost of the same sub-micron semiconductor device has been decreased. The smaller device features result in decreases in performance degrading parasitic capacitances in addition to allowing a greater number of smaller semiconductor chips, still comprised with device densities comparable to larger semiconductor chips, to be obtained from a specific size starting wafer thus reducing the process cost of each individual semiconductor chip. One critical dimension of sub-micron semiconductor or MOSFET devices, is the width of the conductive gate structure, or the channel length of the MOSFET device. This dimension is critical in determining MOSFET device performance. Conductive gate structures defined in polysilicon layers via photoresist masking and dry etching procedures, have been used to define narrow width conductive gate structures. However to control this critical dimension, anti-reflective coatings (ARC) layers are employed underlying the masking photoresist shape to optimize photoresist exposure and thus optimize the definition of the polysilicon gate structure using the narrow photoresist shape as an etch mask. To further insure critical dimension control of the masking photoresist shape, a dual ARC strategy is used. The dual ARC technology comprises a bottom anti-reflective coating (BARC) layer underlying the pre-exposed photoresist layer and a dielectric anti-reflective coating (DARC) layer underlying the BARC layer, with the DARC layer sometimes comprised of silicon nitride or silicon oxynitride. After definition of the conductive gate structure removal of the DARC layer is accomplished using a hot phosphoric acid solution capitalizing on the high selectivity between the fast etching silicon nitride or silicon oxynitride DARC layer and underlying non-silicon oxide materials. However the hot phosphoric wet etch tanks if not frequently maintained can be loaded with unwanted particles as a result of previous applications. After DARC removal, particles from the contaminated hot phosphoric acid wet etch tank can deposit on critical regions of the in-process MOSFET device resulting in yield loss.
The present disclosure will describe a procedure for defining a MOSFET device conductive gate structure, wherein a dual ARC technology is used. However, several embodiments of the present invention will include removal of a DARC layer without employment of hot phosphoric acid, thus avoiding the contamination and possible yield detractors resulting from unwanted particles in the hot phosphoric acid.
BRIEF DESCRIPTION OF THE DRAWINGS
The object and other advantages of this invention are best described in the preferred embodiments with reference to the attached drawings that include:
FIGS. 1-6 , which schematically in cross-sectional style, describe key stages used to define a MOSFET polysilicon gate structure wherein a dual ARC coating, used to enhance dimension control of the polysilicon gate structure, is removed without the use of hot phosphoric acid.
DETAILED DESCRIPTION
A method of defining a polysilicon gate structure for a MOSFET device wherein a dual ARC coating is employed as a component of the defining photolithographic procedure, and wherein the dual ARC coating is removed without the use of hot phosphoric acid, will now be described in detail. Semiconductor substrate 1 , comprised of P type single crystalline silicon featuring a <100> crystallographic orientation, is used and schematically shown in FIG. 1 . Gate insulator 2 , comprised of a gate dielectric layer such as thermally grown silicon oxide, silicon oxynitride, nitrogen doped silicon oxide or a high dielectric constant (high k) layer, is formed to a thickness between about 6 to 80 Angstroms on semiconductor substrate 1 . The silicon dioxide or nitrogen doped silicon oxide gate dielectric candidates are formed at a thickness between about 6 to 20 Angstroms, while silicon oxynitride or other high k gate dielectric alternatives are formed to a thickness between about 20 to 80 Angstroms.
Conductive layer 3 , a layer such as polysilicon, is next formed to a thickness between about 400 to 1800 Angstroms. The polysilicon layer can be in situ doped during deposition via the addition of arsine or phosphine to a silane or disilane ambient, or the polysilicon layer can be deposited intrinsically then implanted with arsenic or phosphorous ions. If desired, a metal silicide layer such as tungsten silicide, cobalt silicide, or nickel silicide, can be used as conductive layer 3 . Silicon oxide layer 4 is next formed, to be used as a capping oxide layer for the subsequent polysilicon gate definition procedure. Capping silicon oxide layer 4 is obtained at a thickness between about 100 to 400 Angstroms via LPCVD or via plasma enhanced chemical vapor deposition (PECVD) procedures.
To improve the ability to define the critical dimension in polysilicon needed for gate width control, anti-coating reflective (ARC), layers can be included as underlying or overlying component layers in a photoresist stack. The ARC layers minimize unwanted spreading phenomena that can occur during photoresist exposure procedures thus increasing the ability to obtain sharper images of the photoresist stack used as the mask for the polysilicon gate structure definition. Organic, bottom ARC (BARC) layers have been used to accomplish this objective, however to further optimize the critical polysilicon width dimension, dual ARC coatings comprised of both an underlying dielectric ARC (DARC) layer and the overlying organic BARC layer can also be used as components of the photolithographic procedure. The DARC layer can be a silicon oxynitride (SiON) layer or a silicon nitride layer. Dielectric layer 5 , employed in this current embodiment is a SiON layer obtained at a thickness between about 200 to 600 Angstroms, via PECVD procedures. Organic bottom anti-reflective coating (BARC) layer 6 , is next applied at a thickness between about 500 to 1200 Angstroms. The result of these depositions and applications are schematically shown in FIG. 1 .
Photoresist shape 7 , is next formed via application of a photoresist layer, exposure of the photoresist layer and development or removal of exposed regions of the photoresist layer via alkaline developer solutions. The presence of the dual ARC layers, organic BARC layer 6 and DARC layer 5 , reduces unwanted scatter during the exposure cycle resulting in a desired image of photoresist shape 7 , between about 1500 to 4000 Angstroms, after the development cycle. The exposed portions of BARC layer 6 , are next removed via an anisotropic dry etching procedure such as a RIE procedure, using a chemistry comprised with either CF 4 , HBR, O 2 , CHF 3 , or CH 2 F 2 as an etchant for organic BARC layer 6 . The anisotropic RIE procedure is continued to remove or trim exposed portions of DARC layer 5 , using a fluorine based chemistry such as CHF 3 , CF 4 , CH 3 F, or CH 2 F 2 as an etchant, resulting in a stack comprised of photoresist shape 7 , organic BARC shape 6 , and dielectric DARC shape 5 , overlying capping silicon oxide layer 4 . This is schematically shown in FIG. 2 .
Trimming of silicon oxide layer capping layer 4 , is next addressed via continuation of the anisotropic RIE procedure, again using either CHF 3 , CF 4 , CH 3 F, or CH 2 F 2 as a selective etchant for silicon oxide, using photoresist shape as the etch mask. This is shown schematically in FIG. 3 .
Transfer of the critical dimension in photoresist shape 7 , to underlying DARC layer 5 , allows removal of photoresist shape to now be performed. This is accomplished via plasma oxygen ashing and follow-up wet strip procedures for removal of photoresist shape 7 . The process used to remove photoresist shape 7 also results in removal of organic BARC layer 6 , resulting in an etch mask stack now comprised of DARC shape 5 , and underlying silicon oxide capping shape 4 , on blanket polysilicon layer 3 . The result of the photoresist and organic BARC removal procedure is schematically displayed in FIG. 4 . The present stack, comprised with the identical critical dimension previously defined in photoresist layer 7 , will be used as an etch mask to pattern or define the desired narrow width, MOSFET polysilicon gate structure.
Another anisotropic RIE procedure using a chemistry comprised of Cl 2 , CF 4 , HBr, and O 2 as etchants for polysilicon layer 3 , is next performed resulting in polysilicon gate structure 3 . The anisotropic RIE procedure also results in the removal of dielectric DARC shape 5 , with the selectivity, or the high etch rate ratio of DARC or polysilicon to silicon oxide, allowing the RIE procedure to terminate at the appearance of the top surface of silicon dioxide gate insulator layer 2 , as well as terminating at the appearance of capping silicon oxide shape 4 , allowing capping silicon oxide shape 4 to perform as an etch mask to transfer the critical dimension in the polysilicon layer. This is schematically shown in FIG. 5 . The employment of a dry etch procedure for removal of DARC shape 5 can be used to limit the use of a hot phosphoric acid for DARC removal. The cleaner dry etch procedure avoids the particles encountered in hot phosphoric acid procedures and thus eliminates possible MOSFET yield loss resulting from particle contamination.
A hydrofluoric acid type procedure, either a dilute hydrofluoric (DHF) or a buffered hydrofluoric (BHF) wet procedure, is then applied to remove portions of silicon dioxide gate insulator layer not covered by polysilicon gate structure 3 . Capping silicon oxide shape 4 is also selectively removed during this procedure resulting in polysilicon gate structure 3 on underlying silicon dioxide gate insulator layer 2 , with the desired critical dimension for the polysilicon gate structure successfully transferred via use of a dielectric DARC layer. The DARC layer can be removed via an integrated transfer procedure accomplished without the use of a contaminating hot phosphoric acid bath. This is schematically shown in FIG. 6
Other embodiments of this invention feature definition of a stack comprised of photoresist shape 7 , BARC shape 6 , and DARC shape 5 , followed by an oxygen ashing procedure removing both photoresist shape 7 and organic BARC shape 6 , leaving DARC shape 5 as an etch mask for anisotropic etching or trimming of capping silicon oxide layer 4 . The definition of polysilicon gate structure 3 is again accomplished via dry etching procedures wherein DARC shape 5 is again removed during the dry etch procedure, again avoiding the use of hot phosphoric acid.
While this invention has been particularly shown and described with reference to the preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made without departing from the spirit and scope of this invention. | A method of defining a patterned, conductive gate structure for a MOSFET device on a semiconductor substrate includes forming a conductive layer over the semiconductor substrate and forming a capping insulator layer over the conductive layer. An anti-reflective coating (ARC) layer is formed over the capping insulator layer and a patterned photoresist shape is formed on the ARC layer. A first etch procedure using the photoresist shape as an etch mask defines a stack comprised of an ARC shape and a capping insulator shape. A second etch procedure using the stack as an etch mask defines the patterned, conductive gate structure in the conductive layer. | 7 |
FIELD OF THE INVENTION
The invention relates to steam irons, and more in particular to the control of steaming functions of such irons.
BACKGROUND
A domestic steam iron has the capability to generate steam and to subsequently release this steam through outlet openings provided in the soleplate of the iron. The steam, which is applied directly to a garment being ironed, helps to diminish the ironing effort and to improve the ironing result.
To store the water that is to be released as steam, a steam iron is commonly fitted with a water reservoir. From there, a water channel guides the water either to a special steam chamber or directly to the soleplate of the iron, where it is heated and converted into steam. Thereafter, it may be released through the outlet openings in the soleplate. Normally, the generation and release of steam is desired only when the iron is in contact with a garment that is being ironed. Several arrangements to ensure such safe and energy-efficient steam iron behaviour have been disclosed in the art. In some of them, an iron is provided with a handle that can be used to control a valve that is disposed in the water channel leading from the water reservoir to the outlet openings in the soleplate of the iron. The handle is preferably operated intuitively, such that it is automatically forced into a position that corresponds to an open position of the valve when a user grips the iron in a manner that indicates an actual ironing activity. Intuitively operated handles commonly rely on the downward force that is exerted by a user's hand on the handle as the user steers the iron across the garment. When a user lifts the iron off of the garment, or when the iron is parked on an iron rest, no downward force is present, indicating that no actual ironing activity takes place. In the absence of a downward force, a biasing mechanism will push the handle into its stationary position, thereby ensuring closure of the valve such that no steam is released.
Research has shown that the forces exerted on a handle by ironing users range from less than 100 gf (0.98 N) to about 4 kgf (39 N). In addition, individual users do not display consistent force-exertion behaviour during a single ironing session either. Users of an iron with an intuitively operated handle may therefore not, or not at all times, automatically apply sufficient force to the handle to open the valve in order to effect the release of steam. From a user point of view, this corresponds to inconsistent iron behaviour: at the one moment the iron may release steam while at the other it doesn't, without a conscious choice being made by the user in between. Furthermore, any temporary or structural disruption of the steam supply due to a variable or consistently insufficient force may increase the ironing effort and worsen the ironing result.
SUMMARY
It is an object of the present invention to provide for a steam iron that overcomes or mitigates one or more of the above-described effects of applying a variable and/or small force to the handle that operates the valve.
According to an aspect of the present invention, a steam iron is provided that includes a housing; a water reservoir; a soleplate that is connected to the housing, and in which at least one outlet opening is provided for the release of steam; and a water channel leading from the water reservoir to the at least one outlet opening in the soleplate. The steam iron further includes a handle, the handle being connected to the housing such that the handle is moveable between a first position and a second position, whereby a biasing mechanism is provided to bias the handle into the first position. The steam iron also includes a valve, disposed in the water channel and operably connected to the handle, such that the valve is in a closed position when the handle is in the first position, and such that the valve is in an open position when the handle is in the second position. The steam iron is further provided with a by-pass around the handle-operated valve for delivering water from the water reservoir to an outlet opening in the soleplate.
According to another aspect of the present invention, a method for steam ironing using a steam iron is provided. The method includes providing a fluid including water (H 2 O), and transporting a first fluid stream to a selectively operable valve that is intuitively operable by a handle. The method also includes transporting a second stream of fluid, by-passing the valve, to steam outlet openings in a soleplate of the iron. The method further includes transporting the first fluid stream that has passed the valve to steam outlet openings in the soleplate of the iron.
A steam iron according to the present invention aims to provide a minimum steam rate, independent of the force that the user applies to the handle of the iron. To this end, it features a by-pass around the handle-operated valve: a water path, leading from the water reservoir to one or more outlet openings in the soleplate, wherein the valve is not included. The result is that even when no or an insufficient force is exerted on the handle, in which case the valve remains in its closed position, water is allowed to flow from the water reservoir to outlet openings in the soleplate. A minimum flow of steam may thus be released from the soleplate even when the valve is in its closed position, ensuring a minimum of steam ironing comfort and steam ironing results. A steam iron according the present invention may be used to practise the method according to the present invention.
Thus, in summary: steam irons with a steam valve that is controlled by an intuitively operated, usually pivotable handle may not provide consistent steam ironing behaviour due to the fact that the force exerted on the handle by the user may change over time. To overcome or mitigate the problem, the present invention provides a steam iron, comprising a by-pass around the handle-operated valve. The by-pass allows a relatively small but continuous water stream to be transported from a water reservoir to steam outlet openings in the soleplate of the iron. Consequently, subject to an ample supply of water, the steam iron provides a minimum of steam ironing comfort throughout a steam ironing session.
These and other features and advantages of the invention will be more fully understood from the following detailed description of certain embodiments of the invention, taken together with the accompanying drawings, which are meant to illustrate and not to limit the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic illustration of an embodiment of a steam iron according to the present invention; and
FIG. 2 schematically shows a number of possible arrangements of a handle-operated valve plus by-pass, a drip-stop and a metering device in the water channel.
DETAILED DESCRIPTION
FIG. 1 schematically shows an embodiment of a steam iron 1 according to the present invention. It will be appreciated that several components of the iron which are well known and have no particular relevance to the present invention are omitted for reasons of clarity.
Steam iron 1 comprises a housing 2 that is fitted with an intuitively operated handle 3 . Handle 3 is pivotable between a first, elevated position and a second, lower position around a hinge 4 that connects the handle 3 to the housing 2 . In FIG. 1 , handle 3 is hinged near its front end, though in other embodiments it may be hinged at other points, such as its middle or its back end. Due to the action of a biasing mechanism 14 , handle 3 resides in its first position when no external, downward force is applied thereto. A biasing mechanism may, for example, be integrated in hinge 4 in the form of a spring hinge. Handle 3 is operably connected to a valve 7 via a link mechanism 5 , such that valve 7 is in a closed position when handle 3 is in its first position and in an open position when the handle 3 is in its second position. Valve 7 is disposed in a water channel 13 that leads from a refillable water reservoir 6 to outlet openings 12 in the heated soleplate 11 . When valve 7 is in an open position, water is allowed to flow from reservoir 6 , through valve 7 and through an optional metering/dripstop-assembly 8 —to be discussed hereafter—to a heated steam chamber 10 . In steam chamber 10 , the water is converted from its liquid form into steam, after which it is released through outlet openings 12 in soleplate 11 .
Without the presence of a by-pass 9 , the only way for water from the water reservoir 6 to reach the outlet openings 12 would be through valve 7 . Naturally, a closed valve 7 would correspond to no release of steam, whereas an open valve 7 would allow the supply of water to steam chamber 10 for steam generation and the subsequent release thereof. As the natural force applied to handle 3 during ironing may differ from user to user, and may be variable over time for a single user, the position of handle 3 , and thus the position of the valve 7 during ironing is not fully predictable. Accordingly, the steaming behaviour of iron 1 would be unpredictable as well. To mitigate this erratic conduct, and to provide the user with a minimum of steam ironing comfort at all times, by-pass 9 is provided. By-pass 9 ensures a minimum of steam release during ironing, which steam release is boosted when handle 3 is pressed into its second position.
A by-pass may take many shapes. It may, for example, be formed as a water conducting conduit that branches off from the water channel upstream of the valve and that returns thereto downstream of the valve, so as to provide a path parallel to a water channel section comprising the valve (as shown in FIG. 1 ). Likewise, a by-pass may be implemented as a systematically leaking valve, or as a hole or passage next to the valve in a channel wall, which wall is provided in the water channel as a flow blockage (see FIG. 2B ). In these cases, the by-pass may be said to have been provided in the water channel, in the sense that the flow of water through the by-pass may be subject to the same controls as the flow of water through the valve, such as for example a drip-stop control or a metering device (see infra the discussion of FIG. 2 ). Alternatively, a by-pass may constitute a second, independent water channel that leads from the water reservoir (or another, second water reservoir) to a steam chamber, or even directly to one or more outlet openings in the soleplate. It is noted that in the latter embodiment, the outlet openings that are configured to release the by-pass steam do not necessarily have to be the same as those in which the (first) water channel discharges itself.—In general, any path that delivers water, steam or liquid, to the outlet openings in the soleplate of the iron, other than through the handle-operated valve, may be considered a by-pass.
The minimum steam rate that the by-pass should warrant need not be very high. Typically, a steam rate of around 12-24 g/min will suffice to achieve an agreeable steam ironing effect, while higher minimum steam rates may result in unnecessarily high energy losses due to steam release when no ironing takes place. The precise minimum steam rate provided for by the by-pass may be made user-adjustable. To this end, the by-pass may for example be fitted with a by-pass valve that allows the effective cross-sectional area of the by-pass to be controlled, whereby the by-pass valve itself may be operated by a dial provided on the outside of the housing of the iron. As a base steam rate of 12-24 g/min is relatively small compared to the overall steam rate that may be applied during ironing, which is typically around 25-95 g/min, the by-pass and the by-passed section of the water channel may be dimensioned such that—in use, and given the same flow-driving pressure—a flow rate of water through the by-pass is smaller than a flow rate of water through the section of the water channel with the valve in its (fully) open position.
Although FIG. 1 depicts a steam iron with an integrated water reservoir 6 , i.e. a water reservoir integrated into the housing 2 that is purposefully moveable by the user during ironing, it is noted that in another embodiment of the steam iron the water reservoir may be arranged external to said housing 2 in a stationary body. This arrangement is common in so called steam iron systems, which, as a rule, feature a relatively large water reservoir and a pressurized steam chamber upstream of the handle-operated valve. In contrast to the embodiment of FIG. 1 , in which the valve 7 controls a flow of liquid water, the valve in these steam iron systems may control a flow of steam. This is a result of the fact that heating of the water in the former embodiment tends to be taken care of downstream of the valve 7 , near the soleplate 11 of the iron 1 , while in the latter embodiment heating is provided for in the aforementioned external, pressurized steam chamber.
Though the above-described handle-operated valve 7 and the by-pass 9 around it improve the consistency of the iron's behaviour, control over the steam rate of iron 1 may be further improved. An iron 1 fitted with said features will normally produce a relatively small, constant base steam rate during an entire ironing session (i.e. during the time the iron 1 is energized), and discharge additional steam in proportion to the displacement of handle 3 from its first position. ‘In proportion’ because of the mechanical nature of the link mechanism 5 by means of which the handle 3 is connected to the valve 7 . As set forth above, valve 7 may be operated between a first and a second position. These two extreme valve positions, and any position therebetween, may correspond to different flow rates through the water channel 13 , and thus to different steam rates of iron 1 . An intermediate valve position corresponds to a handle position between the first and second handle position. A specific intermediate handle position, however, is not easily selectable by a user during ironing, which causes the control over the valve 7 by means of the handle 3 to be somewhat inaccurate. This problem may be solved by enhancing the binary character of the handle-operated valve 7 . To this end, handle 3 may be operably connected to valve 7 by means of a mechanical linkage amplification mechanism 5 that provides a mechanical advantage. A mechanical linkage amplification mechanism 5 may be provided in the form of a lever system, a rack and pinion system, a gear system or any other type of amplification system known in the art. The mechanical advantage can be in the form of a larger output displacement or a higher output force. Through the use of an amplification mechanism 5 , small user inputs—e.g. a small handle displacement or a small force applied to the handle—can be amplified to narrow the input displacement/force interval that corresponds to an intermediate position of the valve. The input force interval that corresponds to an intermediate position of the valve valve may for example be narrowed to 100-500 gf (0.98-4.9 N), or even smaller. Advantageously, the amplification mechanism may also take care of any play due to the tolerance stack-up in the design of the handle-operated valve.
The handle-operated valve including a mechanical linkage amplification mechanism 5 thus provides a substantially on/off-switch functionality that—purposefully—does not allow the user to select a specific, desired steam rate. A user, however, may desire to control the steam rate of the iron 1 in such a way that he or she can adjust the steam rate between zero (dry ironing) and a certain user-defined maximum. To this end, the iron 1 may be fitted with a conventional metering device, which will be described in some detail with reference to FIG. 2 .
FIG. 2 schematically illustrates how a handle-operated valve 7 , a by-pass, and a conventional metering system may be coherently arranged in a water channel 13 . In addition, a drip-stop 23 is shown as well. The assemblies shown in FIG. 2 may be thought of as implementations of the components located in the area demarcated by a dashed line 20 in FIG. 1 . To define the flow direction in FIG. 2 , an upstream point of the water channel 13 is marked 21 , and a downstream point in water channel 13 is marked with 29 .
Referring to FIG. 2A now. Going downstream from the point marked 21 , the first component disposed in the water channel 13 is drip-stop 23 . A drip-stop may be provided in the water channel to stop the flow of water from the water reservoir (not shown in FIG. 2 ) to the soleplate of the iron (not shown in FIG. 2 ) in case the temperature of the soleplate is lower than a preset value. A simple yet effective drip-stop 23 may be made from a bimetallic strip or disc 24 that is exposed to the heated soleplate, and that converts a sufficiently high temperature of the soleplate into a mechanical displacement of the valve head 25 , so as to push it from the valve seat 26 in order to unblock water channel 13 . Downstream of drip-stop 23 the handle-operated valve 7 is disposed. The by-pass provided around valve 7 is denoted with two reference signs: and ⊕. The first sign , labelled 9 a , marks an upstream point of the by-pass, e.g. a point where a by-pass conduit branches off from water channel 13 , whereas the second sign ⊕, labelled 9 b , marks a downstream point of the by-pass, e.g. a point where the by-pass conduit returns to water channel 13 . Even more downstream in water channel 13 , the metering device 22 is located. It comprises a suitably shaped pin 27 that is moveable relative to an aperture 28 , such that the higher it is raised the more water passes by the tapered end and through the aperture 28 . The vertical position of pin 27 may be controlled by means of a user-operable control, such as a knob, dial or slider, which is accessibly disposed on the outside of the housing 2 of the iron 1 .
In principle, valve 7 plus the bypass, drip-stop 23 and metering device 22 may be disposed in water channel 13 in arbitrary order, giving rise to six alternative arrangements. Two of them however, namely the ones in which drip-stop 23 is the most downstream element, are somewhat less advantageous than the other four. This is because water may accumulate in the section of water channel 13 between drip-stop 23 on the one side, and metering device 22 or valve 7 plus by-pass 9 on the other. Such accumulation will occur in particular when a user opens valve 7 or sets metering device 22 to an open position before soleplate 11 of the iron is well-heated. Once drip-stop 23 opens to unblock the water channel 13 , a relatively large amount of accumulated water may flow uncontrolled towards outlet openings 12 in soleplate 11 , which may cause a sudden boost of steam. FIG. 2B-D therefore schematically show only three favourable alternative arrangements relative to the arrangement shown in FIG. 2A . The reference numerals in FIG. 2B-D refer to the same or similar components as those depicted in FIG. 2A . In FIG. 2B , the by-pass 9 is formed as a passage in a channel wall, next to the valve 7 . It may be worth noting that, seen in a downstream direction, FIG. 2B depicts the components in the order: valve 7 plus by-pass 9 , drip-stop 23 and metering device 22 , FIG. 2C depicts them in the order: drip-stop 23 , metering-device 22 , valve 7 plus by-pass, and FIG. 2D depicts them in the order: metering device 22 , drip-stop 23 , valve 7 plus by-pass.
Together, the components depicted in FIG. 2 constitute a relatively simple and efficient system for controlling the flow rate of water through channel 13 , and thus the steam rate of the iron in which it is implemented. In short, a system according to any of the FIG. 2A-D allows a user to select a dry-ironing or steam-ironing mode of the iron, and, in case the later mode is chosen, to determine the maximum steam rate desired. Subject to the provisions that the steam-ironing mode is selected and that the soleplate 11 is sufficiently heated, such that drip-stop 23 does not block water channel 13 , water is allowed to flow from water reservoir 6 to outlet openings provided in the soleplate 11 of iron 1 . A relatively small flow of water is allowed to flow through the by-pass 9 continuously, to provide for a minimum of steam ironing comfort independent of the position of valve 7 . When the valve 7 is moved into its second, open position by means of the intuitive handle 3 , indicating an actual ironing activity, the flow of water through channel 13 is maximised.
It is noted that FIG. 2 illustrates an advantage of providing a by-pass in water channel 13 , as opposed to providing a by-pass separate therefrom. A by-pass provided in water channel 13 is automatically subjected to any flow restriction that the drip-stop and/or the metering system 22 may impose on the flow of water through the channel, whereas in a second, separate channel these restrictions may have to be imposed separately as well.
Although illustrative embodiments of the present invention have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to these embodiments. Various changes or modifications may be effected by one skilled in the art without departing from the scope or the spirit of the invention as defined in the claims. Accordingly, reference throughout this specification to “one embodiment” or “an embodiment” means that a particular feature, structure or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention. Thus, the appearances of the phrases “in one embodiment” or “in an embodiment” in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, it is noted that the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. | Steam irons with a steam valve that is controlled by an intuitively operated, usually pivotable handle may not provide consistent steam ironing behavior due to the fact that the force exerted on the handle by the user may change over time. To overcome or mitigate the problem, the present invention provides a steam iron ( 1 ), comprising a by-pass ( 9 ) around the handle-operated valve ( 7 ). The by-pass allows a relatively small but continuous water stream to be transported from a water reservoir ( 6 ) to steam outlet openings ( 12 ) in the soleplate ( 11 ) of the iron. Consequently, subject to an ample supply of water, the steam iron provides a minimum of steam ironing comfort throughout a steam ironing session. | 3 |
RELATED APPLICATIONS
This case is a continuation-in-part of U.S. Ser. No. 599,612, filed July 28, 1975, now abandoned.
The present invention relates to novel chemical compounds which are derivatives of imidazole. More particularly, the present invention relates to compounds of the formula ##STR3## wherein:
ONE OF R 1 and R 2 is alkyl or the group ##STR4## IN WHICH N IS 0 TO 3, AND THE OTHER OF R 1 and R 2 is benzyl, substituted benzyl, phenyl or substituted phenyl, said substituted benzyl and substituted phenyl substituted on the phenyl ring with one or more substituents independently selected from the group consisting of halo, lower alkyl and trifluoromethyl;
X and Y are independently oxygen or sulfur with the proviso that Y is not oxygen when R 2 is phenyl or substituted phenyl; and the antimicrobial acid addition salts thereof.
The term "alkyl" as used in the specification and appended claims refers to a saturated, unbranched or branched acyclic hydrocarbon group containing 1 to 12 carbon atoms such as methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, tert-butyl, n-pentyl, n-hexyl, n-heptyl, n-octyl, n-nonyl, n-decyl, n-undecyl, n-dodecyl and the like. The term "lower alkyl" refers to an alkyl group as previously defined having 1 to 4 carbon atoms. The term "halo" refers to bromo, chloro and fluoro. The term "antimicrobial acid addition salts" refers to salts of the subject compounds which possess the desired activity and which are neither biologically nor otherwise undesirable. These salts are formed with inorganic acids such as hydrochloric acid, hydrobromic acid, sulfuric acid, nitric acid, phosphoric acid and the like, or organic acids such as acetic acid, propionic acid, glycolic acid, pyruvic acid, oxalic acid, malic acid, malonic acid, succinic acid, maleic acid, fumaric acid, tartaric acid, citric acid, benzoic acid, cinnamic acid, mandelic acid, methanesulfonic acid, ethanesulfonic acid, p-toluenesulfonic acid and the like.
All compounds of Formula (I) possess at least one chiral center, i.e., the carbon atom to which are attached the R 1 XCH 2 , R 2 Y, H and ##STR5## moieties. Accordingly, the compounds of the present invention may be prepared in either optically active form, or as a racemic mixture. Unless otherwise specified, the compounds described herein are all in the racemic form. However, the scope of the subject invention herein is not to be considered limited to the racemic form, but to encompass the individual optical isomers of the subject compounds.
If desired, racemic intermediates or final products prepared herein may be resolved into their optical antipodes by conventional resolution means known per se, for example, by the separation (e.g., fractional crystallization) of the diastereomeric salts formed by reaction of, e.g., racemic compounds of Formula (I) or the alcohol precursors of Formulas (1), (3) and (6) with an optically active acid, or by separation of the diastereomeric esters formed by reaction of the racemic alcohol precursors of compounds of Formula (I) with an optically active acid. Exemplary of such optically active acids are the optically active forms of camphor-10-sulfonic acid, α-bromo-camphor-π-sulfonic acid, camphoric acid, menthoxy-acetic acid, tartaric acid, malic acid, diacetyltartaric acid, pyrrolidone-5-carboxylic acid and the like. The separated pure diastereomeric salts or esters may then be cleaved by standard means to afford the respective optical isomers of the compounds of Formula (I) or the precursor alcohols.
Alternatively, the subject compounds may be prepared in optically active form from optically active compounds of the formula ##STR6## wherein Z is oxygen or sulfur.
The above compounds (15) are obtained from optically active forms of glycerol acetonide (2,2-dimethyl-1,3-dioxolane-4-methanol) by methods known in the art, e.g. J. Med. Chem. 1973, 16, pp. 168-169.
The subject compounds embraced by generic Formula (I) can be represented subgenerically as: ##STR7## wherein:
one of R 1 and R 2 is alkyl or the group ##STR8## in which n is 0 to 3, and the other of R 1 and R 2 is benzyl, substituted benzyl, phenyl or substituted phenyl, said substituted benzyl and substituted phenyl substituted on the phenyl ring with one or more substituents independently selected from the group consisting of halo, lower alkyl and trifluoromethyl;
X and Y are independently oxygen or sulfur with the proviso that Y is not oxygen when R 2 is phenyl or substituted phenyl; and the antimicrobial acid addition salts thereof.
Preferred compounds embraced by the above subgeneric Formulas are:
1. Compounds of Formulas (IA), (IB), (IC) and (ID) wherein R 1 is halo substituted benzyl or halo substituted phenyl and R 2 is alkyl;
2. Compounds of Formulas (IA) and (IB) wherein R 1 is alkyl and R 2 is halo substituted benzyl; and
3. Compounds of Formulas (IC) and (ID) wherein R 1 is is alkyl and R 2 is halo substituted benzyl or halo substituted phenyl.
Particularly preferred compounds within the group described in the previous paragraph are those wherein the halo substituted benzyl and halo substituted phenyl groups are 4-, 2,4-di- and 3,4-dichloro substituted benzyl and 4-, 2,4-di, 3,4-di, 2,4,5-tri, 2,4,6-tri and 2,3,4,5,6 - pentachloro substituted phenyl and the alkyl group is a straight chain alkyl.
Especially preferred compounds within the group described in the previous paragraph are those having a 4-, 2,4-di- or 3,4-dichlorophenyl or a 4-, 2,4-di- or 3,4-dichlorobenzyl in combination with a straight chain alkyl having 3 to 8 carbon atoms.
The subject compounds of Formula (I) exhibit antifungal, antibacterial and antiprotozoal activity. For example, compounds of the present invention exhibit antifungal activity against human and animal pathogens such as
Microsporum audouini,
Microsporum gypseum,
Microsporum gypseum - canis,
Epidermophyton floccosum,
Trichophyton mentagrophytes
Trichophyton rubrum,
Trichophyton tonsurans,
Candida albicans and
Cryptococcus neoformans.
The compounds of the present invention also exhibit antifungal activity against fungi of primarily agricultural importance such as
Aspergillus flavus,
Cladosporium herbarum,
Fusarium graminearum,
Penicillium notatum,
Aspergillus niger,
Penicillium oxalicum,
Penicillium spinulosum and
Pithomyces chartarum.
In addition, the compounds of the present invention exhibit antibacterial activity against human and animal pathogens, such as mercaptan
Staphylococcus aureus,
Streptococcus faecalis,
Corynebacterium acnes,
Erysipelothrix insidiosa,
Escherichia coli,
Proteus vulgaris,
Salmonella choleraesuis,
Pasteurella multocida and
Pseudomonas aeruginosa.
Moreover, the compounds of the present invention exhibit antiprotozoal activity against protozoa such as Trichomonas vaginalis.
In view of the aforementioned activities, the subject compounds are found to be useful antimicrobials, having not only pharmaceutical but also agricultural and industrial application.
Accordingly, a further aspect of the present invention relates to compositions for pharmaceutical, agricultural and industrial use, which compositions comprise the subject compounds of Formula (I) in combination with a suitable carrier. A still further aspect of the present invention relates to methods of inhibiting the growth of fungi, bacteria and protozoa by applying to a host object containing, or subject to attack by, fungi, bacteria or protozoa an effective amount of a compound of the present invention or a suitable composition containing same.
In pharmaceutical applications, compositions may be solid, semi-solid or liquid in form such as tablets, capsules, powders, suppositories, liquid solutions, suspensions, creams, lotions, gels, ointments and the like. Pharmaceutically acceptable non-toxic carriers, or excipients normally employed for solid formulations include tricalcium phosphate, calcium carbonate, kaolin, bentonite, talcum, gelatin, lactose, starch and the like; for semi-solid formulations there may be mentioned, for example, polyalkylene glycols, vaseline and other cream bases; for liquid formulations there may be mentioned, for example, water, oils of vegetable origin and low boiling solvents such as isopropanol, hydrogenated naphthalenes and the like. The pharmaceutical compositions containing the compounds of the present invention may be subjected to conventional pharmaceutical expedients such as sterilization and can contain conventional pharmaceutical excipients such as preservatives, stabilizing agents, emulsifying agents, salts for the adjustment of osmotic pressure and buffers. The compositions may also contain other therapeutically active materials. In pharmaceutical applications, the subject compounds and compositions may be administered to humans and animals by conventional methods, e.g., topically, orally, parenterally and the like. Parenteral administration includes intramuscular as well as subcutaneous and intravenous injection. Intravenous injection of imidazole derivatives for certain systemic conditions has been demonstrated to be effective (see for example, Drugs, 9, 419-420 (1975), which describes the intravenous administration of Miconazole, i.e., 1-[2,4-dichloro-β-(2',4'-dichlorobenzyloxy)phenethyl]imidazole nitrate, to patients with systemic candidiasis).
Topical application is the preferred method of administration in pharmaceutical applications. For such treatment, an area having an existing fungal, bacterial or protozoal growth, or to be protected against attack by fungi, bacteria or protozoa may be treated with the subject compounds or compositions by, for example, dusting, sprinkling, spraying, rinsing, brushing, dipping, smearing, coating, impregnating and the like. Topical compositions containing the compounds of the present invention exhibit antifungal, antibacterial and antiprotozoal activity over a wide range of concentration, for example, from about 0.1 to 10.0% by weight of the composition.
The pharmaceutical compositions hereof typically comprise one or more subject compounds of Formula (I) and a pharmaceutically acceptable, non-toxic carrier, and are preferably formulated in unit dosage form to facilitate administration (unit dosage being the amount of active ingredient administered on one occasion).
In general, for systemic (e.g. oral or parenteral) administration it is expedient to administer the active ingredient in amounts of between about 1 and 100 mg./kg. body weight per day (preferably between about 5 and 50 mg./kg. body weight per day) distributed over several applications (e.g. in 3 individual doses) in order to achieve effective results. For localized (e.g. topical) administration however, proportionately less of the active ingredient is required. The exact regimen for pharmaceutical administration of the compounds and compositions disclosed herein will necessarily be dependent upon the needs of the individual subject being treated, the type of treatment, e.g., whether preventative or curvative, the type of organism involved and, of course, the judgment of the attending practitioner. In any event the compositions to be administered will contain a quantity of the subject compound in an amount effective for relief or prevention of the specific condition being treated.
In agricultural applications, the subject compounds may be applied directly to plants (e.g., seeds, foliage) or to soil. For example, compounds of the present invention may be applied to seeds alone or in admixture with a powdered solid carrier. Typical powdered carriers are the various mineral silicates, e.g., mica, talc, pyrophyllite and clays. The subject compounds may also be applied to the seeds in admixture with a conventional surface-active wetting agent with or without additional solid carrier. Surface-active wetting agents that can be used are any of the conventional anionic, non-anionic or cationic types. As a soil treatment for fungi and the like, the subject compounds can be applied as a dust in admixture with sand, soil or a powdered solid carrier such as a mineral silicate with or without additional surface-active agent, or the subject compounds can be applied as an aqueous spray optionally containing a surface-active dispersing agent and a powdered solid carrier. As a foliage treatment, the subject compounds may be applied to growing plants as an aqueous spray which contains a surface-active dispersing agent with or without a powdered solid carrier and hydrocarbon solvents.
In industrial applications, the subject compounds may be used to control bacteria and fungi by contacting the pathogens with the compounds in any known manner. Materials capable of supporting bacteria and fungi may be protected by contacting, mixing or impregnating these materials with the subject compounds. In order to increase their effectiveness, the subject compounds may be combined with other pesticidal control agents such as fungicides, bactericides, insecticides, miticides and the like. A particularly important industrial/agricultural use for the subject compounds of the present invention is as a food preservative against bacteria and fungi which cause deterioration and spoilage of foods.
DETAILED DESCRIPTION
The present invention in a still further aspect is directed to methods for the preparation of the subject compounds of Formula (I).
Sequence 1
The following reaction sequence, directed to the preparation of compounds of Formulas (IA) and (IB), can be illustrated as follows: ##STR9## wherein R 1 is as previously defined, R 2 is limited to alkyl, ##STR10## in which n is 0 to 3, benzyl or substituted benzyl, Z is oxygen or sulfur, and X' is a conventional leaving group such as a halide (e.g., bromide or chloride), or a sulfonate ester (e.g., methanesulfonate or p-toluenesulfonate).
In the above sequence, the imidazole derivatives of Formulas (IA) and (IB) are prepared by converting a hydroxy compound of Formula (1) to its metal salt by treatment with a strong base, such as sodium hydride and the like, and thereafter contacting the resulting metal salt with a compound of Formula (2). Preparation of the metal salt is effected in an organic solvent such as hexamethylphosphoramide, tetrahydrofuran, dimethylformamide and the like, at a temperature of 0° to 65° C. for a period of 30 minutes to 4 hours. Thereafter, reaction of the metal salt with a compound of Formula (2) is carried out, preferably, in the same solvent at a temperature of 0° to 65° C. for a period of 1 to 24 hours.
Sequence 2
The following reaction sequence, directed to the preparation of compounds of Formula (IC), can be illustrated as follows: ##STR11## wherein R 1 and R 2 are as previously defined and X' is a conventional leaving group such as a halide (e.g., chloride or bromide) or a sulfonate ester (e.g., methanesulfonate or p-toluenesulfonate).
In the above sequence, the imidazole derivatives of Formula (IC) are prepared from compounds of Formula (3) by a two-step sequence involving conversion of the hydroxy group to a suitable leaving group followed by reaction with a metal salt of a thiol of Formula (5).
The conversion of an alcohol of Formula (3) to a compound of Formula (4) is carried out by means well known in the art. For example, the alcohol may be halogenated using a halogenating agent such as thionyl chloride or thionyl bromide, either neat, or in a inert organic solvent such as dichloromethane or chloroform, at a temperature between about 0° to 80° C., preferably between about 20° and 80° C. The halogenation reaction may be carried out in the presence of a molar equivalent of a base (e.g., pyridine) if desired. Alternative halogenation procedures include, for example, the use of triphenylphosphine with either carbon tetrachloride, carbon tetrabromide, or N-chloro (or N-bromo)succinimide. When utilizing thionyl chloride or thionyl bromide without the use of added base, the hydrochloride or hydrobromide salt of the corresponding halo compound is produced. This salt is preferably neutralized (e.g., with potassium carbonate) prior to its use in the thioalkylation step, however the salt may be used directly if excess thiol salt or base is utilized.
Sulfonate esters may be prepared by the standard proedure of treating the alcohol with an excess of, for example, methanesulfonyl chloride or p-toluenesulfonyl chloride, in the presence of a base, for example, pyridine or triethylamine. This reaction is carried out at a temperature from about -20° to +50° C., preferably between about 0° and 20° C.
The thus prepared compounds of Formula (4) are then treated with a metal salt, preferably an alkali metal salt such as the sodium or potassium salt, of a thiol of Formula (5) in the presence of an inert organic solvent at a temperature from about 20° to about 80° C.
The reaction of compounds of Formula (4) with compounds of Formula (5) wherein R 2 in Formula (5) is alkyl, ##STR12## in which n is 0 to 3, benzyl or substituted benzyl is carried out in an inert organic solvent such as tetrahydrofuran, ether, methanol and the like in the presence of a suitable base such as sodium hydride or sodium methoxide at a temperature of 20° to 67° C. for a period of 30 minutes to 24 hours.
The reaction of compounds of Formula (4) with compounds of Formula (5) wherein R 2 in Formula (5) in phenyl or substituted phenyl is carried out in an inert organic solvent such as acetone, methanol and the like in the presence of a suitable base such as potassium carbonate, sodium hydroxide or sodium methoxide at ambient temperature to reflux for a period of 30 minutes to 72 hours.
Sequence 3
The following reaction sequence, directed to the preparation of compounds of Formula (ID), can be illustrated as follows: ##STR13## wherein R 1 and R 2 are as previously defined and X' is a conventional leaving group such as a halide (e.g. chloride or bromide), or a sulfonate ester (e.g. methanesulfonate or p-toluenesulfonate).
In the above sequence, the compounds of Formula (7) are prepared in the same manner previously described for the preparation of compounds of Formula (4) in Sequence 2.
Thereafter the imidazole derivatives of Formula (ID) are prepared by treating a compound of Formula (7) with a metal salt, preferably an alkali metal salt such as the sodium or potassium salt of a thiol of Formula (8) in the presence of an inert organic solvent at a temperature of 20° to 80° C. This particular reaction proceeds via a cyclic intermediate with the net result being attachment of the entering R 1 -S-moiety at the --CH 2 -position and the migration of the original R 2 -S-moiety from this position to the --CH= position.
The reaction of compounds of Formula (7) with compounds of Formula (8) wherein R 1 in Formula (8) is alkyl, ##STR14## in which n is 0 to 3, benzyl or substituted benzyl is carried out as previously described in the preparation of compounds of Formula (IC) in Sequence 2 (see paragraph 6).
The reaction of compounds of Formula (7) with compounds of Formula (8) is phenyl or substituted phenyl, is carried out as previously described in the preparation of compounds of Formula (IC) in Sequence 2 (see paragraph 7).
Sequence 4
The following reaction sequence, directed to a second method for the preparation of compounds of Formula (IC), can be illustrated as follows: ##STR15## wherein R 1 and R 2 are as previously described and X' is a conventional leaving group such as a halide (e.g. chloride or bromide) or a sulfonate ester (e.g. methanesulfonate or p-toluenesulfonate.
In the above sequence, compounds of Formula (10) are prepared in the manner previously described for the preparation of compounds of Formula (4) in Sequence 2.
Thereafter, compounds of Formula (10) are reacted with imidazole in an organic solvent such as acetonitrile, dimethylformamide and the like to obtain the imidazole derivatives of Formula (IC). This reaction is carried out at a temperature of 0° to 100° C. for a period of 1 to 24 hours.
The subject compounds of the instant invention can be isolated as free bases, however, since many of the compounds in base form are oils or gums, it is more convenient to isolate and characterize the compounds as acid addition salts. These salts are prepared in the usual manner, i.e., by reaction of the base compound with a suitable inorganic or organic acid, described above. Salts formed with dibasic acids (e.g. oxalic acid) may contain one or two molecules of base per molecule of acid. All oxalates described herein contain one molecule of oxalic acid per molecule of imidazole base. If desired, the salts can be readily converted to the compounds in base form by treatment with alkali, such as potassium carbonate, sodium carbonate or sodium or potassium hydroxide.
The alcohols required as starting materials for preparation of the subject compounds of the instant invention are either available or can be obtained by known processes.
For example, the alcohols required in Sequences 1-3 can be prepared as follows: ##STR16## wherein R 1 is as previously defined, X' is chloro or bromo and Z is oxygen or sulfur.
In the above depicted sequence, the 2,3-epoxypropyl (thio)ethers of Formula (15 ) are prepared by reaction of a compound of Formula (13) with an epihalohydrin such as epichlorohydrin or epibromohydrin followed by reaction of the resulting 2,3-epoxypropyl (thio)ether with imidazole.
The reaction of compounds of Formula (13) with epihalohydrins, wherein R 1 in Formula (13) is alkyl, ##STR17## in which n is 0 to 3, benzyl or substituted benzyl is carried out in an inert organic solvent such as tetrahydrofuran, ether and the like in the presence of a suitable base such as sodium hydride at a temperature of 0° to 67° C. for a period of 30 minutes to 72 hours.
The reaction of compounds of Formula (13) with epihalohydrins, wherein R 1 in Formula (13) is phenyl or substituted phenyl is carried out in an inert organic solvent such as acetone, methanol and the like in the presence of a suitable base such as potassium carbonate, sodium hydroxide and sodium methoxide at ambient temperature to reflux for a period of 30 minutes to 24 hours.
The thus obtained 2,3-epoxypropyl(thio)ethers of Formula (15) are then reacted with at least one molar equivalent of imidazole (preferably an excess) in an inert organic solvent such as acetonitrile, dimethylformamide, and the like, at a temperature of 0° to 80° C. for a period of 1 to 72 hours to obtain the alcohols of Formula (1).
When R 1 is a small alkyl group such as methyl, ethyl etc., in alcohols of Formula (1), such alcohols tend to be relatively water soluble. In such cases, variations necessary in the reaction and work up procedures will be apparent to those skilled in the art. Such variations may include use of a low boiling organic solvent, non-aqueous work up, chromatographic separation, removal of excess imidazole at a later stage, etc.
The above discussion particularly applies to certain alcohols prepared in Preparations A and B on pages 21 to 24.
Alcohols required in Sequence 4 can be prepared as follows: ##STR18## wherein R 1 and R 2 are as previously defined.
In the above depicted sequence, the alcohols of Formula (9) are prepared by reaction of a 2,3-epoxypropyl ether of Formula (16) with a thiol of Formula (5).
The reaction of a 2,3-epoxypropyl ether (16) with a compound of Formula (5) wherein R 2 in Formula (5) is alkyl, ##STR19## in which n is 0 to 3, benzyl or substituted benzyl is carried out in a solvent such as tetrahydrofuran, ether, methanol and the like in the presence of a suitable base such as sodium hydride or sodium methoxide at ambient temperature to reflux for a period of 30 minutes to 24 hours.
The reaction of 2,3-epoxypropyl ether (16) with a compound of Formula (5) wherein R 2 in Formula (5) is phenyl or substituted phenyl is carried out in an inert organic solvent such as acetone, methanol and the like in the presence of a suitable base such as potassium carbonate, sodium hydroxide and sodium methoxide at ambient temperature to reflux for a period of 30 minutes to 24 hours.
DESCRIPTION OF SPECIFIC EMBODIMENTS
The following specific description is given to enable those skilled in the art to more clearly understand and practice the present invention. It should not be considered as a limitation upon the scope of the invention but merely as being illustrative and representative thereof.
Preparation A
A 56% dispersion of sodium hydride in mineral oil (2.2 g.) is added at room temperature to a solution of 7.95 g. of 4-chlorobenzylmercaptan in 100 ml. of dry tetrahydrofuran. The resulting salt is then treated with 6.9 g. epibromohydrin in 20 ml. tetrahydrofuran and the mixture stirred for 30 minutes and evaporated to dryness. Thereafter, 250 ml. of ether is added to the residue and the ether extract washed with water. The organic phase is dried over magnesium sulfate and evaporated; excess epibromohydrin being removed under vacuum. To the resulting oil is added 17 g. imidazole and 50 ml. dimethylformamide. The mixture is stirred overnight at 60° C. and then poured into water and the aqueous phase extracted with ether. The resulting product is chromatographed on silica gel and eluted with 10% methanol in methylene chloride to yield 12.3 g. of 1-[3'-(4"-chlorobenzylthio)-2'-hydroxypropyl] imidazole as an amber gum.
Similarly, replacing 4-chlorobenzyl mercaptan in the above procedure with equivalent amounts of other suitable thiols or alcohols is productive of the following 1-[3'-R 1 -thio(oxy)-2'-hydroxypropyl]imidazoles:
1-[3'-methylthio-2'-hydroxypropyl] imidazole,
1-[3'-ethylthio-2'-hydroxypropyl] imidazole,
1-[3'-isopropylthio-2'-hydroxypropyl] imidazole,
1-[3'-n-propylthio-2'-hydroxypropyl] imidazole,
1-[3'-n-butylthio-2'-hydroxypropyl] imidazole,
1-[3'-n-hexylthio-2'-hydroxypropyl] imidazole,
1-[3'-n-penthylthio-2'-hydroxypropyl] imidazole,
1-[3'-n-octylthio-2'-hydroxypropyl] imidazole,
1-[3'-n-nonylthio-2'-hydroxypropyl] imidazole,
1-[3'-n-decylthio-2'-hydroxypropyl] imidazole, 1-[3'-n-dodecylthio-2'-hydroxypropyl] imidazole,
1-[3'-cyclohexylthio-2'-hydroxypropyl] imidazole,
1-[3'-cyclohexylmethylthio-2'-hydroxypropyl] imidazole,
1[3'-benzylthio-2'-hydroxypropyl] imidazole,
1-[3'-(3"-bromobenzylthio)-2'-hydroxypropyl] imidazole,
1-[3'-(4"-bromobenzylthio)-2'-hydroxypropyl] imidazole,
1-[3'-(2",4"-dichlorobenzylthio)-2'-hydroxypropyl] imidazole,
1-[3'-(3",4"-dichlorobenzylthio)-2'-hydroxypropyl] imidazole,
1-[3'-(4"-fluorobenzylthio)-2'-hydroxypropyl] imidazole,
1[3'-(3'-methylbenzylthio-2'-hydroxypropyl] imidazole,
1-[3'-(4"-methylbenzylthio)-2'-hydroxypropyl] imidazole,
1-[3'-(2",4",6"-trimethylbenzylthio)-2'-hydroxypropyl] imidazole,
1-[3'-(4"t-butylbenzylthio)-2'-hydroxypropyl] imidazole,
1[3'-(4"-trifluoromethylbenzylthio)-2'-hydroxypropyl] imidazole
1-[3'-methoxy-2'-hydroxypropyl] imidazole,
1[3'-n-propoxy-2'-hydroxypropyl] imidazole,
1[3'-isopropoxy-2'-hydropypropyl] imidazole,
1-[3'-t-butoxy-2'-hydroxypropyl] imidazole,
1-[3'-n-pentyloxy-2'-hydroxypropyl] imidazole,
1-[3'-n-hexyloxy-2'-hydroxypropyl] imidazole,
1-[3'-n-heptyloxy-2'-hydroxypropyl] imidazole,
1-[3'-n-decyloxy-2'-hydroxypropyl] imidazole,
1-[3'-n-dodecyloxy-2'-hydroxypropyl] imidazole,
1-[3'-(3-cyclohexyl-n-propoxy)-2'-hydroxypropyl] imidazole,
1-[3'-benzyloxy-2'-hydroxypropyl] imidazole,
1-[3'-(4"-chlorobenzyloxy)-2'-hydroxypropyl] imidazole,
1-[3'-(4"-bromobenzyloxy)-2'-hydroxypropyl] imidazole,
1-[3'-(4"-fluorobenzyloxy)-2'-hydroxypropyl] imidazole,
1-[3'-(4"-trifluromethylbenzyloxy)-2'-hydroxypropyl] imidazole
1-[3'n-octyloxy-2-hydroxypropyl] imidazole, and
1-[3'-n-nonyloxy-2-hydroxypropyl] imidazole.
Preparation B
A mixture of 3.8 g. of 2,4-dichlorothiophenol, 5.5 g. of epibromohydrin and 5.6 g. of anhydrous potassium carbonate in 100 ml. acetone is stirred at reflux. After 2 hours the mixture is evaporated to dryness and 100 ml. of water is added to the residue. The resultant aqueous mixture is extracted with ether and the ether extract washed with water. The organic phase is dried over magnesium sulfate and evaporated to yield a pale yellow oil.
Without further purification the oil obtained above is added to 7.0 g. of imidazole in 15 ml. dimethylformamide. After stirring for 3 days at 25° C. the reaction mixture is poured into water. The product is extracted with ether and the ether extracts filtered, washed with water, dried over magnesium sulfate and evaporated. The residue is chromatographed on silica gel eluting with 10% methanol in dichloromethane to yield 1-[3'-(2",4"-dichlorophenylthio)-2'-hydroxypropyl]imidazole as a pale yellow gum which solidifies.
Similarly, replacing 2,4-dichlorothiophenol in the above procedure with other thiophenols or phenols is productive of the following 1-[3'-phenylthio (oxy)-2'-hydroxypropyl]imidazoles:
1-[3'-phenylthio-2'-hydroxypropyl]imidazole,
1-[3'-(4"-chlorophenylthio)-2'-hydroxypropyl]imidazole,
1-[3'-(3",4"-dichlorophenylthio)-2'-hydroxypropyl]imidazole,
1-[3'-pentachlorophenylthio-2'-hydroxypropyl]imidazole,
1-[3'-(4"-bromophenylthio)-2'-hydroxypropyl]imidazole,
1-[3'-(3"-bromophenylthio)-2'-hydroxypropyl]imidazole,
1-[3'-(4"-fluorophenylthio)-2'-hydroxypropyl]imidazole,
1-[3'-(4"-trifluoromethylphenylthio)-2'-hydroxypropyl]imidazole,
1-[3'-(3"-methylphenylthio)-2'-hydroxypropyl]imidazole,
1-[3'-(4"-t-butylphenylthio)-2'-hydroxypropyl]imidazole,
1-[3'-phenoxy-2'-hydroxypropyl]imidazole,
1-[3'-(4"-chlorophenoxy)-2'-hydroxypropyl]imidazole, 1-[3'-(2",4"-dichlorophenoxy)-2'-hydroxypropyl]imidazole,
1-[3'-(3",4"-dichlorophenoxy)-2'-hydroxypropyl]imidazole,
1-[3'-pentachlorophenoxy-2'-hydroxypropyl]imidazole,
1-[3'-(4"-bromophenoxy)-2'-hydroxypropyl]imidazole,
1-[3'-(2",4",6"-trimethylphenoxy)-2'-hydroxypropyl]imidazole,
1-[3'-(4"-t-butylphenoxy)-2'-hydroxypropyl]imidazole,
1-[3'-(3"-trifluoromethylphenoxy)-2'-hydroxypropyl]imidazole
1-[3'-(2",4"-dibromophenoxy)-2'-hydroxypropyl]imidazole,
1-[3'-(2",4"-dibromophenylthio-2'-hydroxypropyl]imidazole,
1-[3'-(2",4"-difluorophenoxy)-2'-hydroxypropyl]imidazole, and
1-[3'-(2",4"-difluorophenylthio)-2'-hydroxypropyl]imidazole.
Preparation C
2,4-Dichlorophenyl 2,3-epoxypropyl ether (2.2 g.) in several ml. of dry tetrahydrofuran is added with stirring to a prereacted mixture of 1.5 g. of n-heptylthiol and 50 mg. of sodium hydride (56% dispersion in mineral oil) in 40 ml. tetrahydrofuran. The mixture is then stirred at 55° C. for 6 hours. The solvent is then removed from the reaction mixture and 30 ml. of water is added to the residue. The resulting aqueous mixture is extracted with ether and the ether extracts washed with water, dried over magnesium sulfate and evaporated to yield 3-(2',4'-dichlorophenoxy)-1-(n-heptylthio)-2-propanol.
Similarly, replacing 2,4-dichlorophenyl 2,3-epoxypropyl ether in the above procedure with equivalent amounts of other suitable 2,3-epoxypropyl ethers and/or replacing n-heptylthiol with other suitable thiols is productive of the following 3-(R 1 -oxy)-1-(R 2 -thio)-2-propanols:
3-methoxy-1-(4'-t-butylbenzylthio)-2-propanol,
3-n-butoxy-1-(2',4'-dichlorobenzylthio)-2-propanol,
3-n-pentyloxy-1-(4'-chlorobenzylthio)-2-propanol,
3-n-pentyloxy-1-(2',4'-dichlorobenzylthio)-2-propanol,
3-n-hexyloxy-1-(4'-chlorobenzylthio)-2-propanol,
3-n-hexyloxy-1-(2',4'-dichlorobenzylthio)-2-propanol,
3-n-hexyloxy-1-(3',4'-dichlorobenzylthio)-2-propanol,
3-n-heptyloxy-1-(4'-chlorobenzylthio)-2-propanol,
3-n-heptyloxy-1-(3',4'-dichlorobenzylthio)-2-propanol,
3-n-heptyloxy-1-(2',4'-dichlorobenzylthio)-2-propanol,
3-n-octyloxy-1-(4'-chlorobenzylthio)-2-propanol, 3-n-octyloxy-1-(4'-bromobenzylthio)-2-propanol,
3-n-octyloxy-1-(4'-trifluoromethylbenzylthio)-2-propanol,
3-n-nonyloxy-1-(4'-chlorobenzylthio)-2-propanol,
3-n-decyloxy-1-(pentafluorobenzylthio)-2-propanol,
3-n-dodecyloxy-1-benzylthio-2-propanol,
3-cyclohexylmethoxy-1-(2',4',6'-trimethylbenzylthio)-2-propanol,
3-benzyloxy-1-decylthio-2-propanol,
3-(4'-chlorobenzyloxy)-1-n-octylthio-2-propanol,
3-(4'-chlorobenzyloxy)-1-n-nonylthio-2-propanol,
3-(4'-bromobenzyloxy)-1-n-octylthio-2-propanol,
3-(4'-fluorobenzyloxy)-1-n-nonylthio-2-propanol,
3-pentamethylbenzyloxy-1-n-butylthio-2-propanol,
3-(4'-t-butylbenzyloxy)-1-n-hexylthio-2-propanol,
3-(3'-trifluoromethylbenzyloxy)-1-n-octylthio-2-propanol,
3-phenoxy-1-n-dodecylthio-2-propanol,
3-(4'-chlorophenoxy)-1-n-pentylthio-2-propanol,
3-(4'-chlorophenoxy)-1-n-hexylthio-2-propanol,
3-(4'-chlorophenoxy)-1-n-heptylthio-2-propanol,
3-(4'-chlorophenoxy)-1-n-octylthio-2-propanol,
3-(4'-chlorophenoxy)-1-n-nonylthio-2-propanol,
3-(2',4'-dichlorophenoxy)-1-n-butylthio-2-propanol,
3-(2',4'-dichlorophenoxy)-1-n-pentylthio-2-propanol,
3-(2',4'-dichlorophenoxy)-1-n-hexylthio-2-propanol,
3-(2',4'-dichlorophenoxy)-1-n-octylthio-2-propanol,
3-(3',4'-dichlorophenoxy)-1-n-hexylthio-2-propanol,
3-(3',4'-dichlorophenoxy)-1-n-heptylthio-2-propanol,
3-(3',4'-dichlorophenoxy)-1-n-octylthio-2-propanol,
3-pentachlorophenoxy-1-methylthio-2-propanol,
3-pentachlorophenoxy-1-n-propylthio-2-propanol,
3-pentachlorophenoxy-1-isobutylthio-2-propanol,
3-(4'-chloro-3'-trifluoromethylphenoxy)-1-n-heptylthio-2-propanol,
3-(4'-bromophenoxy)-1-n-octylthio-2-propanol,
3-(2',4',6'-tribromophenoxy)-1-n-pentylthio-2-propanol,
3-(3'-fluorophenoxy)-1-n-dodecylthio-2-propanol,
3-(4'-t-butylphenoxy-1-n-hexylthio-2-propanol,
3-(4'-t-butylphenoxy)-1-cyclohexylthio-2-propanol and
3-(2',6'-dimethyl-4'-t-butylphenoxy)-1-n-butylthio-2-propanol.
Preparation D
2,3-Epoxypropyl isopropyl ether (1.16 g.), 3.2 g. of pentachlorothiophenol and 1.5 g. of potassium carbonate in 50 ml. of acetone are stirred at reflux overnight. The solvent is then removed and water is added to the residue. The resultant aqueous phase is then extracted with ether and the ether extracts washed with water, dried over magnesium sulfate and evaporated to dryness to yield crude 3-isopropoxy-1-pentachlorophenylthio-2-propanol.
EXAMPLE 1
A 56% dispersion of sodium hydride in mineral oil (480 mg.) is added under nitrogen to a solution of 2.52 g. of 1-[3'-(4"-chlorophenoxy)-2'-hydroxypropyl]imidazole in 6 ml. dry hexamethylphosphoramide. After stirring for 1 hours at room temperature, the temperature is increased to 45° C. and stirring is continued for 2 hours. The solution is then cooled in an ice bath and 2.5 g. of 1-bromodecane in 1 ml. of hexamethylphosphoramide is added. Thereafter, the solution is stirred for 2 hours at room temperature and then for 16 hours at 50° C. The reaction mixture is poured into water and the resultant aqueous mixture extracted with ether and the ether extracts washed with water. The organic phase is dried over magnesium sulfate and evaporated. The resulting residue is chromatographed on silica gel. Elution with 20% acetone in dichloromethane yields 1-[3'-(4"-chlorophenoxy)-2'-(n-decyloxy)propyl]imidazole.
An ethereal solution of the above obtained base is acidified with ethereal oxalic acid yielding, after recrystallization of the crude salt from ethyl acetate, 1-[3'-(4"-chlorophenoxy)-2'-(n-decyloxy)propyl]imidazole oxalate.
EXAMPLE 2
Thionyl chloride (5 ml.) and 1.6 g. of 1-[3'-(n-decyloxy)-2'-hydroxypropyl]imidazole are warmed gently for a period of 2 hours and the solution is then evaporated to dryness. The residue is dissolved in dichloromethane and rendered basic with aqueous potassium carbonate solution. The organic layer is separated, dried over magnesium sulfate and evaporated to yield 1-[2'-chloro-3'-(n-decyloxy)propyl]imidazole.
The chloro compound obtained above, i.e., 1-[2'-chloro-3'-(n-decyloxy)propyl]imidazole (1.6 g.) is then stirred and heated under reflux with 1.1 g. of thiophenol and 1.2 g. anhydrous potassium carbonate in 40 ml. of acetone. After stirring for approximately 16 hours the solvent is removed and water is added to the residue. The resultant aqueous phase is then extracted with ether and the ether extracts washed with water, dried over magnesium sulfate and evaporated to yield 1-[3'-(n-decyloxy)-2'-(phenylthio)propyl]imidazole.
An ethereal solution of the above obtained base is acidified with ethereal oxalic acid yielding, after recrystallization of the crude salt from ethyl acetate, 1-[3'-(n-decyloxy)-2'-(phenylthio)propYl]imidazole oxalate.
EXAMPLE 3
1-[3'-(4"-chlorobenzylthio)-2'-hydroxypropyl]imidazole (500 mg.) and 0.5 ml. of thionyl chloride in 20 ml. dichloromethane are warmed gently for 1/2 hour. Thereafter, the reaction mixture is evaporated to yield a gum which is dissolved in 50 ml. dichloromethane and basified with aqueous potassium carbonate solution. The organic phase is separated, dried over magnesium sulfate and evaporated.
The chloro compound obtained above is dissolved in 5 ml. of tetrahydrofuran and added to the salt formed in situ from 600 mg. of n-hexyl mercaptan and 200 mg. of sodium hydride (56% dispersion in mineral oil) in 30 ml. tetrahydrofuran. The mixture is stirred overnight at room temperature and then evaporated to dryness. To the residue is added 30 ml. of water and the resultant aqueous phase is then extracted with 100 ml. of ether.
The ether extract is washed with water, dried over magnesium sulfate and evaporated to dryness. The residue is chromatographed on silica gel. Elution with 5% acetone in dichloromethane yields 1-[2'-(4"-chlorobenzylthio)-3'-(n-hexylthio)]imidazole as a gum.
Acidification of an ethereal solution of the above obtained gum with ethereal oxalic acid yields, after recrystallization from ethyl acetate, 1-[2'-(4"-chlorobenzylthio)-3-(n-hexylthio)propyl]imidazole oxalate, m.p. 130°-131° C.
EXAMPLE 4
1-[3'-n-octylthio-2'-hydroxypropyl]imidazole (2.7 g.) and 3 ml. of thionyl chloride in 50 ml. dichloromethane are warmed gently for 2 hours and the solution is then evaporated to dryness. The resulting residue is dissolved in 150 ml. dichloromethane and rendered basic with aqueous potassium carbonate solution. The organic layer is separated, dried over magnesium sulfate and evaporated.
The chloro compound obtained above is then heated under reflux with 1.75 g. of p-chlorothiophenol and 1.6 g. of potassium carbonate in 100 ml. of acetone. After stirring for approximately 4 hours at reflux the solvent is removed from the reaction mixture and water is added to the residue. The resultant aqueous phase is extracted with ether and the ether extracts washed with water, dried over magnesium sulfate and evaporated. The residue is chromatographed on silica gel. Elution with 10% acetone in dichloromethane yields 1-[3'-(4"-chlorophenylthio)-2'-n-octylthio)propyl]imidazole.
EXAMPLE 5
3-(2",4"-dichlorophenoxy)-1-(n-heptylthio)-2-propanol (3.5 g.) in 30 ml. of dichloromethane and 3 ml. of thionyl chloride are stirred for 2 hours at room temperature. Thereafter the solution is evaporated to dryness and 10 ml. of acetonitrile and 4 g. of imidazole are added to the resulting residue. The reaction mixture is then stirred overnight at room temperature and then at 60° C. for 24 hours. The solvent is removed and 30 ml. of water is added to the resulting residue. The resulting aqueous phase is then extracted with ether and the ether extracts washed with water, dried over magnesium sulfate and evaporated to yield 1-[3'-(2",4"-dichlorophenoxy)-2'-(n-heptylthio)-propyl]imidazole.
An ethereal solution of the above obtained base is acidified with oxalic acid yielding, after recrystallization of the crude salt from ethyl acetate, 1-[3'-(2",4"-dichlorophenoxy)-2-(n-heptylthio)propyl]imidazole, oxalate.
EXAMPLE 6
Crude 3-isopropoxy-1-pentachlorophenylthio-2-propanol, obtained in Preparation D, in 60 ml. of dichloromethane and 5 ml. of thionyl chloride are stirred for 2 hours at room temperature. The solution is then evaporated to dyrness and 5 ml. of acetonitrile and 4 g. of imidazole are added to the resulting residue. The reaction mixture is stirred at 80° C. for 48 hours and then evaporated to dryness. To the resulting residue is added 30 ml. of water. The resultant aqueous phase is extracted with ether and the ether extracts washed with water, dried over magnesium sulfate and evaporated to yield crude 1-[3'-isopropoxy-2'-(pentachlorophenylthio)propyl]imidazole.
An ethereal solution of the above obtained base is acidified with nitric acid yielding, after recrystallization of the crude salt from ethyl acetate, 1-[3'-isopropoxy-2' -(pentachlorophenylthio)propyl]imidazole nitrate, m.p. 126°-129° C. (decomp.).
EXAMPLE 7
Repeating the procedure in paragraph 1 of Example 1 using reactants of Formulas (1) and (2) as dictated by the particular 1-{3'-[R 1 -oxy(thio)]-2'-[R 2 -oxy]propyl}imidazole desired is productive of the following compounds as free bases, which where indicated, are further characterized by conversion to the indicated acid addition salt, by treatment in the conventional manner with the appropriate acid:
1-[2'-(n-decyloxy)-3'-(2",4",6"-trimethylphenoxy)propyl]-imidazole, oxalate salt, m.p. 88°-89° C.,
1-[2'-(n-dodecyloxy)-3'-(phenoxy)propyl]imidazole,
1-[3'-(4"-bromophenoxy)-2'-(n-decyloxy)propyl]imidazole,
1-[2'-(4"-bromobenzyloxy)-3'-(n-decyloxy)propyl]imidazole,
1-[2'-(n-hexyloxy)-3'-(pentachlorophenoxy)propyl]imidazole,
1-[3'-(2",4"-dichlorophenoxy)-2'-(n-nonyloxy)propyl]imidazole,
1-[3'-(3",4"-dichlorophenoxy)-2'-(n-nonyloxy)propyl]imidazole, oxalate salt, m.p. 109.5°-110° C.,
1-[3'-(4"-chlorobenzyloxy)-2'-(n-decyloxy)propyl]imidazole,
1-[2'-(4"-chlorobenzyloxy)-3'-(n-decyloxy)propyl]imidazole,
1-[3'-(methoxy)-2'-(pentamethylbenzyloxy)propyl]imidazole,
1-[2'-(2",4",5"-trichlorobenzyloxy)-3'-(n-heptyloxy)propyl]imidazole,
1-[2'-benzyloxy)-3'-(n-dodecyloxy)propyl]imidazole,
1-[2'-(4"-t-butylbenzyloxy)-3'-(3-cyclohexyl-n-propoxy)-propyl]imidazole,
1-[3'-(benzyloxy)-2'-(n-dodecyloxy)propyl]imidazole,
1-[2'-(n-dodecyloxy)-3'-(4"-fluorobenzyloxy)propyl]imidazole,
1-[2'-(n-decyloxy)-3'-(4"-bromobenzyloxy)propyl]imidazole,
1-[2'-(n-decyloxy)-3'-(4"-trifluoromethylbenzyloxy)propyl]imidazole,
1-[3'-(4"-t-butylphenoxy)-2'-(3-cyclohexyl-n-propoxy)propyl]imidazole,
1-[2'-(n-octyloxy)-3'-(3"-trifluoromethylphenoxy)propyl]imidazole,
1-[3'-(n-decyloxy)-2'-(4" -trifluoromethylbenzyloxy)propyl]imidazole,
1-[2'-(methoxy)-3'-(pentachlorophenoxy)propyl]imidazole,
1-[2'-(n-butoxy)-3'-(pentachlorophenoxy)propyl]imidazole,
1-[2'-(4"-fluorobenzyloxy)-3'-(n-dodecyloxy)propyl]imidazole,
1-[2'-(cyclohexylethoxy)-3'-(2",4"-dichlorophenylthio)propyl]imidazole,
1-[2'-(n-butoxy)-3'-(pentachlorophenylthio)propyl]imidazole,
1-[2'-(3",4"-dichlorobenzyloxy)-3'-(cyclohexylthio) propyl]imidazole,
1-[2'-(benzyloxy)-3'-(n-dodecylthio)propyl]imidazole,
1-[2'-(n-octyloxy)-3'-(2",4"-dichlorophenylthio)propyl]imidazole,
1-[2'-(n-octyloxy)-3'-(3",4"-dichlorophenylthio)propyl]imidazole,
1-[2'-(3",4"-dichlorobenzyloxy)-3'-(n-heptylthio)propyl]imidazole,
1-[3'-(4"-chlorophenylthio)-2'-(n-nonyloxy)propyl]imidazole,
1-[3'-(4"-chlorophenylthio)-2'-(n-decyloxy)propyl]imidazole,
1-[3'-(4"-chlorobenzylthio)-2'-(n-octyloxy)propyl]imidazole,
1-[3'-(4"-chlorobenzylthio)-2'-(n-nonyloxy)propyl]imidazole,
1[2'-(4"-chlorobenzyloxy)-3'-(n-octylthio)propyl]imidazole,
1-[2'-(4"-chlorobenzyloxy)-3'-(n-nonylthio)propyl]imidazole,
1-[3'-(2",4"-dichlorobenzylthio)-2'-(n-heptyloxy)propyl]imidazole,
1-[3'-(3",4"-dichlorobenzylthio)-2'-(n-heptyloxy)propyl]imidazole,
1-[2'-(2",4"-dichlorobenzyloxy)-3'-(n-heptylthio)proply]imidazole,
1-[3'-(methylthio)-2'-(pentamethylbenzyloxy)propyl]imidazole,
1-[3'-(n-butylthio)-2'-(2",4",5"-trichlorobenzyloxy)propyl]imidazole,
1-[3'-(benzylthio)-2'-(n-decyloxy)propyl]imidazole,
1-[3'-(4"-bromobenzylthio)-2'-(n-octyloxy)propyl]imidazole,
1-[3'-(4"-fluorobenzylthio)-2'-(n-decyloxy)propyl]imidazole,
1-[2'-(n-heptyloxy)-3'-(2",4",6"-trimethylbenzylthio)propyl]imidazole,
1-[2'-(n-octyloxy)-3'-(4"-trifluoromethylbenzylthio)propyl]imidazole,
1-[2'-(n-dodecyloxy)-3'-(phenylthio)propyl]imidazole,
1-[3'-(4"-bromophenylthio)-2'-(n-nonyloxy)propyl]imidazole,
1-[3'-(4"-fluorophenylthio)-2'-(n-decyloxy)propyl]imidazole,
1-[2'-(n-nonyloxy)-3'-(4"-trifluoromethylphenylthio)propyl]imidazole,
1-[2'-(methoxy)-3'-(pentachlorophenylthio)propyl]imidazole,
1-[2'-(4"-bromobenzyloxy)-3'-(n-octylthio)propyl]imidazole,
1-[2'-(4"-fluorobenzyloxy)-3'-(n-decylthio)propyl]imidazole,
1-[2'-t-butylbenzyloxy)-3'-(n-hexylthio)propyl]imidazole,
1-[2'-(t-butylbenzyloxy)-3'-(cyclohexylmethylthio)propyl]imidazole,
1-[3'-(2",4"-dichlorophenoxy)-2'-(n-octyloxy)propyl]imidazole,
1-[3'-(2",4"-dichlorophenoxy)-2'-(n-decyloxy)propyl]imidazole,
1-[2'-(3",4"-dichlorobenzyloxy)-3'-(n-octyloxy)propyl]imidazole,
1-[2'-(3",4"-dichlorobenzyloxy)-3'-(n-nonyloxy)propyl]imidazole,
1-[2'-(3",4"-dichlorobenzyloxy)-3'-(n-decyloxy)propyl]imidazole,
1-[2'-(2",4"-dichlorobenzyloxy)-3'-(n-octyloxy)propyl]imidazole,
1-[2'-(2",4"-dichlorobenzyloxy)-3'-(n-nonyloxy)propyl]imidazole,
1-[2'-(2",4"-dichlorobenzyloxy)-3'-(n-decyloxy)propyl]imidazole,
1-[3'-(3",4"-dichlorophenoxy)-2'-(n-octyloxy)propyl]imidazole,
1-[ 3'-(3", 4"-dichlorophenoxy)-2'-(n-nonyloxy)propyl] imidazole,
1-[3'-(3",4"-dichlorophenoxy)-2'-(n-decyloxy)propyl] imidazole,
1-[2'-(4"-chlorobenzyloxy)-3'(n-decyloxy)propyl] imidazole,
1-[3'-(2",4"-dichlorophenylthio)-2'-(n-nonyloxy)propyl] imidazole,
1-[2'-(3", 4"-dichlorobenzyloxy)-3'-(n-octylthio)propyl] imidazole,
1-[2'-(2",4"-dichlorobenzyloxy)-3'-(n-hexylthio)propyl] imidazole,
1-[2'-(2", 4"-dichlorobenzyloxy)-3'-(n-octylthio)propyl] imidazole,
1-[3'-(2",4"-dichlorophenylthio)-2'-(n-hexyloxy)propyl] imidazole,
1-[3'-(3",4"-dichlorophenylthio)-2'-(n-heptyloxy)propyl] imidazole,
1-[3'-(3",4"-dichlorophenylthio)-2'-(n-nonloxy)propyl] imidazole,
1-[3'-(4"-chlorophenylthio)-2'-(n-pentyloxy)propyl] imidazole,
1-[3'-(4"-chlorophenylthio)-2'-n-hexyloxy)propyl] imidazole,
1-[3'-(4"-chlorophenoxy)-2'-(n-hexyloxy)propyl] imidazole,
1-[3'-(4"-chlorophenoxy)-2'-(n-heptyloxy)propyl] imidazole,
1-[3'-(4"-chlorophenoxy)-2'-(n-octyloxy)propyl] imidazole,
1-[3'-(2",4"-dichlorophenoxy)-2'-(n-pentyloxy)piopyl] imidazole,
1-[3'-(2",4"dichlorophenoxy)-2'-(n-hexyloxy)propyl] imidazole,
1-[3'-(2",4"-dichlorophenoxy)-2"-(n-heptyloxy)propyl] imidazole,
1-[3'-(4"-chlorophenylthio)-2'-(n-heptyloxy)-propyl] imidazole,
1-[3'-(2",4"-dichlorophenylthio)-2'-(n-pentyloxy)propyl] imidazole,
1-[3'-(4"-chlorobenzylthio)-2'-(n-pentyloxy)propyl] imidazole,
1-[3'-chlorobenzylthio)-2'-(n-hexyloxy)propyl] imidazole,
1-[3'-(4"-chlorobenzylthio)-2'-(n-heptyloxy)propyl]
1-[3'-(n-butylthio)-2'-(4"-chlorobenzyloxy)propyl] imidazole,
1-[2'-(4"-chlorobenzyloxy)-3'-(n-pentylthio)propyl] imidazole,
1-[2'-(4"-chlorobenzyloxy)-3'-(n-hexylthio)propyl] imidazole,
1-[2'-(4"-chlorobenzyloxy)-3'-(n-pentyloxy)propyl] imidazole,
1-[2'-(4"-chlorobenzyloxy)-3'-(n-hexyloxy)-propyl] imidazole,
1-[2'-(4"-chlorobenzyloxy)-3'-(n-heptyloxy)propyl] imidzole,
1 -[2'-(2",4"-dichlorobenzyloxy)-3'-n-propylthio)propyl] imidazole,
1-[3'-(n-butylthio)-2'-(2",4"-dichlorobenzyloxy)propyl] imidazole,
1-[2'-(2",4"-dichlorobenzyloxy)-3'-(n-pentylthio)propyl] imidazole,
1-[3'-(n-butoxy)-2'-(2",4"-dichlorobenzyloxy)propyl] imidazole,
1[2'-(2",4"-dichlorobenzyloxy)-3'-(n-pentyloxy)propyl] imidazole and
1-[2'-(2",4"-dichlorobenzyloxy)-3'-(n-hexyloxy)propyl] imidazole.
EXAMPLE 8
Repeating the procedure in paragraphs 1 and 2 of Example 2 using reactants of Formulas (3) and (5) as dictated by the particular 1-[3'-(R 1 -oxy)-2'-(R 2 -thio)propyl] imidazole desired is productive of the following compounds as free bases:
1[3'-(n-decyloxy)-2'-(4"-fluorophenylthio)propyl] imidazole,
1-[3'-(n-decyloxy)-2'-(3"-methylphenylthio)propyl] imidazole,
1-[3'-(isopropoxy)-2'-(pentachlorophenylthio)propyl] imidazole,
1-[3'-(n-propoxy)-2'-(pentachlorophenylthio)propyl] imidazole,
1-[3'-(t-butoxy)-2'-(pentachlorophenylthio)propyl] imidazole,
1-[2'-(2",4"-dichlorophenylthio)-3'-(n-heptyloxy)propyl] imidazole,
1-[2'-(3",4"-dichlorophenylthio)-3'-(n-heptyloxy)propyl] imidazole,
1-[2'-(4"-chlorophenylthio)-3'-(n-octyloxy)propyl] imidazole,
1-[2'-(4"-chlorophenylthio)-3'-(n-nonyloxy)propyl] imidazole,
1-[3'-(methoxy)-2'-(pentachlorophenylthio)propyl] imidazole,
1-[3'-(n-dodecyloxy)-2'-(phenylthio)propyl] imidazole,
1-[3'-(3'-cyclohexyl-n-propoxy)-2'-(3",4"-dichlorophenylthio)propyl] imidazole,
1-[2'-(4"-chlorophenylthio)-3'-(n-decyloxy)propyl] imidazole,
1-[2'-(3",4"-dichlorophenylthio)-3'-(n-octyloxy)propyl] imidazole,
1-[2'-(2",4"-dichlorophenylthio)-3'-(n-octyloxy)propyl] imidazole,
1-[2'-(4"-chlorophenylthio)-3'-(n-pentyloxy)propyl] imidazole,
1-[2'-(4"-chlorophenylthio)-3'-(n-hexyloxy)propyl] imidazole,
1-[2'-(4"-chlorophenylthio)-3'-(n-heptyloxy)propyl] imidazole,
1-[3'-(n-butoxy)-2'-(2",4"-dichlorophenylthio)propyl] imidazole,
1-[2'-(2",4"-dichlorophenylthio)-3'-(n-pentyloxy)propyl] imidazole,
1-[2'-(2",4"-dichlorophenylthio)-3'-(n-hexyloxy)propyl] imidazole,
1-[3'-(n-butoxy)-2'-(3",4"-dichlorophenylthio)propyl] imidazole,
1-[2'-(3",4"-dichlorophenylthio)-2'-(n-pentyloxy)propyl] imidazole and
1-[2'-(3",4"-dichlorophenylthio)-2'-(n-hexyloxy)propyl] imidazole.
EXAMPLE 9
Repeating the procedure in paragraphs 1-3 of Example 3 using reactants of Formulas (6) and (8) as dictated by the particular 1-[2'-(R 2 -thio)-3'-(R 1 -thio)propyl]imidazole desired is productive of the following compounds as free bases, which where indicated, are further characterized by conversion to the indicated acid addition salt, by treatment in the conventional manner with the appropriate acid:
1-[3'-(4"-chlorobenzylthio)-2'-(n-heptylthio)propyl]imidazole,
1-[3'-(benzylthio)-2'-(n-octylthio)propyl]imidazole,
1-[3'-(n-octylthio)-2'-(benzylthio)propyl]imidazole,
1-[3'-(methylthio)-2'-(4"-t-butylbenzylthio)propyl]imidazole,
1-[2'-(3",4"-dichlorophenylthio)-3'-(n-hexylthio)propyl]imidazole,
1-[3'-(4"-chlorobenzylthio)-2'-(n-hexylthio)propyl]imidazole,
1-[2'-(2",4"-dichlorophenylthio)-3'-(n-pentylthio)propyl]imidazole,
1-[2'-(3",4" -dichlorophenylthio)-3'-(n-pentylthio)propyl]imidazole,
1-[2'-(4"-chlorobenzylthio)-3'-cyclohexylthio)propyl]imidazole, oxalate salt, m.p. 128.5°-131° C.,
1-[2'-(pentachlorophenylthio)-3'-(ethylthio)propyl]imidazole,
1-[2'-(pentachlorophenylthio)-3'-(isopropylthio)propyl]imidazole,
1-[2'-(2",4"-dichlorophenylthio)-3'-(n-hexylthio)propyl]imidazole, oxalate salt, m.p 91.5°-93° C.,
1-[2'-(4" -chlorophenylthio)-3'-(n-heptylthio)propyl]imidazole,
1-[2'-(4"-chlorophenylthio)-3'-(n-octylthio)propyl]imidazole,
1-[2'-(4"-chlorobenzylthio)-3'-(n-heptylthio)propyl]imidazole,
1-[3'-(n-dodecylthio)-2'-(phenylthio)propyl]imidazole,
1-[3'-(2"-bromobenzylthio)-2'-(cyclohexylmethylthio)propyl]imidazole,
1-[3'-(4"-fluorobenzylthio)-2'-(n-heptylthio)propyl]imidazole,
1-[3'-(2",4",6"-trimethylbenzylthio)-2'-(n-pentylthio)propyl]imidazole,
1-[2'-(n-butylthio)-3'-(4"-t-butylbenzylthio)propyl]imidazole,
1-[2'-(n-hexylthio)-3'-(3"-trifluoromethylbenzylthio)propyl]imidazole,
1-[2'-(4"-bromobenzylthio)-3'-(n-hexylthio)propyl]imidazole,
1-[2'-(4"-fluorobenzylthio)-3'-(n-octylthio)propyl]imidazole,
1-[3'-(n-heptylthio)-2'-(4"-methylbenzylthio)propyl]imidazole,
1-[3'-(n-hexylthio)-2'-(4"-trifluoromethylbenzylthio)propyl]imidazole,
1-[2'-(3"-bromophenylthio)-3'-(n-heptylthio)propyl]imidazole,
1-[2'-(4"-fluorophenylthio)-3'-(n-nonylthio)propyl]imidazole,
1-[2'-(3"-methylphenylthio)-3'-(n-octylthio)propyl]imidazole,
1-[2'-(n-butylthio)-3'-(4"-chlorobenzylthio)propyl]imidazole,
1-[3'-(4"-chlorobenzylthio)-2'-(n-pentylthio)propyl]imidazole,
1-[3'-(n-butylthio)-2'-(4"-chlorophenylthio)propyl]imidazole,
1-[2'-(4"-chlorophenylthio)-3'-(n-pentylthio)propyl]imidazole,
1-[2'-(4"-chlorophenylthio)-3'-(n-hexylthio)propyl]imidazole,
1-[2'-(2",4"-dichlorophenylthio)-3'-(n-propylthio)propyl]imidazole,
1-[3'-(n-butylthio)-2'-(2",4"-dichlorophenylthio)propyl]imidazole,
1-[2'-(3",4"-dichlorophenylthio)-3'-(n-propylthio)propyl]imidazole,
1-[3'-(n-butylthio)-2' -(3",4"-dichlorophenylthio)propyl]imidazole,
1-[3'-(n-butylthio)-2'-(4"-chlorobenzylthio)propyl]imidazole,
1-[2'-(4"-chlorobenzylthio)-3'-(n-pentylthio)propyl]imidazole,
1-[2'-(2",4"-dichlorobenzylthio)-3'-(n-propylthio)propyl]-imidazole,
1-[3'-(n-butylthio(-2'-(2",4"-dichlorobenzylthio)propyl]-imidazole and
1-[2'-(2",4"-dichlorobenzylthio)-3'-(n-pentylthio)propyl]-imidazole.
EXAMPLE 10
Repeating the procedure of Example 4 using reactants of Formulas (6) and (8) as dictated by the particular 1-[2'-(R 2 -thio)-3'-(R 1 -thio)propyl]imidazole desired is productive of the following compounds as free bases:
1-[3'-(4"-chlorophenylthio)-2'-(n-heptylthio)propyl]imidazole,
1-[3'-(pentachlorophenylthio)-2'-(methylthio)propyl]imidazole,
1-[3'-(3",4"-dichlorophenylthio)-2'-(n-hexylthio)propyl]imidazole,
1-[3'-(2",4"-dichlorophenylthio)-2'-(n-pentylthio)propyl]imidazole,
1-[3'-(3",4"-dichlorophenylthio)-2'-(n-pentylthio)propyl]imidazole,
1-[3'-(pentachlorophenylthio)-2'-(ethylthio)propyl]imidazole,
1-[3'-(pentachlorophenylthio)-2'-(isopropylthio)propyl]imidazole,
1-[3'-(2",4"-dichlorophenylthio)-2'-(n-hexylthio)propyl]imidazole,
1-[2'-(n-dodecylthio)-3'-(phenylthio)propyl]imidazole,
1-[3'-(3"-bromophenylthio)-2'-(n-heptylthio)propyl]imidazole,
1-[3'-(4"-fluorophenylthio)-2'-(n-nonylthio)propyl]imidazole,
1-[2'-(n-butylthio)-3'-(4"-t-butyl-2"-methylphenylthio)propyl]imidazole,
1-[3'-(4"-chlorophenylthio)-2'-(n-pentylthio)propyl]imidazole,
1-[3'-(4"-chlorophenylthio)-2'-(n-hexylthio)propyl]imidazole and
1-[2'-(n-butylthio)-3'-(2",4"-dichlorophenylthio)propyl]imidazole.
EXAMPLE 11
Repeating the procedure in paragraph 1 of Example 5 using reactants of Formula (9) as dictated by the particular 1-[3'-(R 1 -oxy)-2'-(R 2 -thio)propyl]imidazole desired is productive of the following compounds as free bases, which where indicated, are further characterized by conversion to the indicated acid addition salt, by treatment in the conventional manner with the appropriate acid:
1-[3'-(4"-chlorobenzyloxy)-2'-(n-nonylthio)propyl]imidazole,
1-[3'-(4"-t-butylphenoxy)-2'-(cyclohexylthio)propyl]imidazole,
1-[3'-(4"-chlorophenoxy)-2'-(n-nonylthio)propyl]imidazole,
1-[3'-(pentachlorohenoxy)-2'-(n-propylthio)propyl]imidazole,
1-[3'-(pentachlorophenoxy)-2'-isobutylthio)propyl]imidazole,
1-[3'-(3",4"-dichlorophenoxy)-2'-(n-heptylthio)propyl]imidazole,
1-[3'-(4"-chlorophenoxy)-2'-(n-octylthio)propyl]imdiazole,
1-[3'-(4"-chlorobenzyloxy)-2'-(n-octylthio)propyl]imidazole,
1-[2'-(4"-chlorobenzylthio)-3'-(n-octyloxy)propyl]imidazole,
1[2'-(4"-chlorobenzylthio-3'-(n-nonyloxy)propyl]imidazole,
1-[2'-(4"-t-butylbenzylthio)-3'-(methoxy)propyl]imidazole,
1-[2'-(3",4"-dichlorobenzylthio)-3'-(n-hexyloxy) propyl]imidazole,
1-[2'-(benzylthio)-3'-(n-dodecyloxy)propyl]imidazole,
1-[3'-(cyclohexylmethoxy)-2'-(2",4",6"-trimethylbenzylthio)propyl]imidazole
1-[3'-(benzyloxy)-2'-(n-decylthio)propyl]imidazole,
1-[3'-(4"-fluorobenzyloxy)-2'-(n-nonylthio)propyl]imidazole,
1-[3'-(4"-bromobenzyloxy)-2'-(n-octylthio)propyl]imidazole,
1-[2'-(n-butylthio-3'-(pentamethylbenzyloxy)propyl]imidazole,
1-[3'-(4"-t-butylbenzyloxy)-2'-(n-hexylthio)propyl]imidazole,
1-[2'-(n-octylthio-3'-(3"-trifluoromethylbenzyloxy)propyl]imidazole,
1-[2'-(n-dodecylthio)-3'-(phenoxy)propyl]imidazole,
1-[3'-(2",4",6"-tribromophenoxy-2-(h-pentylthio)propyl]imidazole,
1-[2'-(n-dodecylthio)-3'-(3"-fluorophenoxy)propyl]imidazole,
1-[2'(n-butylthio)-3'-(2",6"-dimethyl-4"-t-butylphenoxy)propyl]imidazole,
1-[2'-(n-heptylthio)-3'-(4"-chloro-3"-trifluoromethylphenoxy)propyl]imidazole,
1-[2'-(methylthio)-3'-(pentachlorophenoxy)propyl]imidazole,
1-[3'-(n-decyloxy)-2'-(pentafluorobenzylthio)propyl]imidazole,
1-[2'-(4"-bromobenzylthio)-3'-(n-octyloxy)propyl]imidazole,
1-[3'-(n-octyloxy)-2'-(4"-trifluoromethylbenzylthio)propyl]imidazole,
1-[3'-(2",4"-dichlorophenoxy)-2'-(n-hexylthio)propyl]imidazole,
1-[3'-(2",4"-dichlorophenoxy)-2'-(n-heptylthio)propyl]imidazole,
1-[3'-(2",4"-dichlorophenoxy)-2'-(n-octylthio)propyl]imidazole,
1-[2'-(3",4"-dichlorobenzylthio)-3'-(n-heptyloxy)propyl]imidazole,
1-[2'-(2",4"-dichlorobenzylthio)-3'-(n-heptyloxy)propyl]imidazole,
1-[3'-(3",4"-dichlorophenoxy)-2'-(n-hexylthio)propyl]imidazole,
1-[3'-(3",4"-dichlorophenoxy)-2'-(n-octylthio)propyl]imidazole,
1-[3'-(4"-t-butylphenoxy)-2'-(n-hexylthio)propyl]imidazole, oxalate salt, m.p. 106°-107.5° C.,
1-[3'-(4"-bromophenoxy)-2'-(n-octylthio)propyl]imidazole, oxalate salt, m.p. 88.5°-92.5° C.,
1-[3'-(4"-chlorophenoxy)-2'-(n-pentylthio)propyl]imidazole,
1-[3'-(4"-chlorophenoxy)-2'-(n-hexylthio)propyl]imidazole,
1-[3'-(4"-chlorophenoxy)-2'-(n-heptylthio)propyl]imidazole,
1-[2'-(n-butylthio)-3'-(2",4"-dichlorophenoxy)propyl]-imidazole,
1-[3'-(2",4"-dichlorophenoxy)-2'-(n-pentylthio)propyl] imidazole,
1-[2'-(4"-chlorobenzylthio)-3'-(n-pentyloxy)propyl]imidazole,
1-[2'-(4"-chlorobenzylthio)-3'-(n-hexyloxy)propyl]imidazole,
1-[2'-(4"-chlorobenzylthio)-3'-(n-heptyloxy)propyl]imidazole,
1-[3'-(n-butoxy)-2'-(2",4"-dichlorobenzylthio)propyl]imidazole,
1-[2'-(2",4"-dichlorobenzylthio)-3'-(n-pentyloxy)propyl]imidazole and
1-[2'-(2",4"-dichlorobenzylthio)-3'-(n-hexyloxy)propyl]imidazole.
EXAMPLE 12
1-[2'-(4"-chlorobenzylthio)-3'-(n-hexylthio)propyl]imidazole oxalate (2.3 g.) in 100 ml. of dichloromethane is shaken with excess potassium carbonate solution until the salt is completely dissolved. The organic layer is then separated, washed with water, dried over magnesium sulfate and evaporated to yield 1-[2'-(4"-chlorobenzylthio)-3'-(n-hexylthio)propyl]imidazole.
In similar manner, the antimicrobial acid addition salts of all compounds of Formula (I) can be converted to the corresponding compounds in base form.
EXAMPLE 13
Nitric acid (70%; d = 1.42) is added dropwise to a stirred solution of 2.0 g. of 1-[3'-isopropoxy-2'-(pentachlorophenylthio)propyl]imidazole in 30 ml. of anhydrous ether until precipitation was complete. The product was filtered off, washed with ether, air dried, and recrystallized from ethyl acetate to yield 1-[3'-isopropoxy-2'-(pentachlorophenylthio)propyl]imidazole nitrate.
In similar manner, all compounds of Formula (I) in base form can be converted to the antimicrobial acid addition salts by treatment with the appropriate acid, for example, hydrochloric acid, hydrobromic acid, sulfuric acid, nitric acid, phosphoric acid, acetic acid, propionic acid, glycolic acid, lactic acid, pyruvic acid, oxalic acid, malonic acid, succinic acid, malic acid, maleic acid, fumaric acid, tartaric acid, citric acid, benzoic acid, cinnamic acid, mandelic acid, methanesulfonic acid, ethanesulfonic acid or p-toluenesulfonic acid.
EXAMPLE 14
The following example illustrates the preparation of representative formulations containing an active compound, such as a salt of 1-[2'-(4"-chlorobenzylthio)-3-(n-hexylthio)propyl]imidazole which may be used for controlling fungi, bacteria and protozoa.
______________________________________A. Topical Formulation grams______________________________________Active compound 0.2 - 2Span 60 2Tween 60 2Mineral oil 5Petrolatum 10Methyl paraben 0.15Propyl paraben 0.05BHA(butylated hydroxy anisole) 0.01Water qs 100______________________________________
All of the above ingredients, except water, are combined and heated at 60° C. with stirring. A sufficient quantity of water at 60° C. is then added with vigorous stirring to provide 100 g. of the cream formulation which is then cooled to room temperature.
______________________________________B. I.V. Formulation______________________________________Active compound 0.5 g.Propylene glycol 20 g.Polyethylene glycol 400 20 g.Tween 80 1 g.0.9% Saline solution qs 100 ml.______________________________________
The active compound is dissolved in propylene glycol, polyethylene glycol 400 and Tween 80. A sufficient quantity of 0.9% saline solution is then added with stirring to provide 100 ml. of the I.V. solution which is filtered through a 0.2 micron membrane filter and packaged under sterile conditions.
______________________________________C. Oral Formulation parts by weight______________________________________Active compound 200Magnesium stearate 3Starch 30Lactose 116PVP (polyvinylpyrrolidone) 3______________________________________
The above ingredients are combined and granulated using methanol as the solvent. The formulation is then dried and formed into tablets (containing 200 mg. of active compound) with an appropriate tabletting machine. | Compounds of the formula ##STR1## wherein one of R 1 and R 2 is alkyl or the group ##STR2## IN WHICH N IS 0 TO 3 AND THE OTHER OF R 1 and R 2 is benzyl, substituted benzyl, phenyl or substituted phenyl, said substituted benzyl and substituted phenyl substituted on the phenyl ring with one or more substituents independently selected from the group consisting of halo, lower alkyl and trifluoromethyl; X and Y are independently oxygen or sulfur with the proviso that Y is not oxygen when R 2 is phenyl or substituted phenyl; and the antimicrobial acid addition salts thereof are useful as antifungal, antibacterial and antiprotozoal agents. | 2 |
This invention was made with government support under U.S. Department of Agriculture Grant No. 91372056320. The government has certain rights to this invention.
This application is a divisional of U.S. application Ser. No. 07/884,423, filed May 15, 1992, now U.S. Pat. No. 5,340,740, the disclosure of which is herein incorporated by reference in its entirety.
FIELD OF THE INVENTION
The present invention relates to stem cells in general, and particularly relates to avian embryonic stem cells.
BACKGROUND OF THE INVENTION
Embryonic stem cells (ESCs) were first cultured from mouse embryos using a feeder layer of mouse fibroblasts or media conditioned with buffalo rat liver cells. The established ESC lines from mouse embryos have a characteristic phenotype consisting of a large nucleus, a prominent nucleolus, and relatively little cytoplasm. Such cells can be grown relatively indefinitely using the appropriate culture conditions. They can be induced to differentiate in vitro using retinoic acid or spontaneously by removal of the feeder layer or conditioned media. In addition, these cells can be injected into a mouse blastocyst to form a somatic and germ line chimera. This latter property has allowed mouse ESCs to be used for the production of transgenic mice with specific changes to the genome. See M. Evans et al., Nature 292, 154 (1981); G. Martin, Proc. Natl. Acad. Sci. USA 78, 7638 (1981); A. Smith et al., Developmental Biology 121, 1 (1987); T. Doetschman et al., Developmental Biology 127, 224 (1988); A. Handyside et al., Roux's Arch Dev. Biol. 198, 48 (1989).
The active compound that allows the culture of murine embryonic stem cells has been identified as differentiation inhibiting activity (DIA), also known as leukemia inhibitory factor (LIF). See A. Smith, J. Tiss. Cult. Meth. 13, 89 (1991); J. Nichols et al., Development 110, 1341 (1990). Recombinant forms of LIF can be used to obtain ESCs from mouse embryos. See S. Pease et al., Developmental Biology 141, 344 (1990).
Subsequent to the work with mouse embryos, several groups have attempted to develop stem cell lines from sheep, pig and cow. A few reports indicate that a cell line with a stem cell-like appearance has been cultured from porcine embryos using culture conditions similar to that used for the mouse. See M. Evans et al., PCT Application WO90/03432; E. Notarianni et al., J. Reprod. Fert., Suppl. 41, 51 (1990); J. Piedrahita et al., Theriogenology 34, 879 (1990); E. Notarvianni et al., Proceedings of the 4th World Congress on Genetics Applied to Livestock Production, 58 (Edinburgh, July 1990).
Few or no attempts have been made to date regarding the culture of embryonic stem cells from avian embryos. The main reason for this is that it is very difficult to establish a continuous line of chicken cells without viral or chemical transformation, and most primary chicken lines do not survive beyond 2-3 months. The culture of cells from the unincubated embryo has been more difficult, and under reported conditions such cells do not survive beyond two weeks. See E. Mitrani et al., Differentiation 21, 56-61 (1982); E. Sanders et al., Cell Tissue Res. 220, 539 (1981).
SUMMARY OF THE INVENTION
We have developed a process that allows the culture of cells with an embryonic stem cell phenotype from the avian embryo. The development of this process was problematic. First, we attempted to culture chicken embryo cells on a chicken fibroblast feeder layer. This was not successful. Next, we attempted to culture chicken embryo cells on a mouse feeder layer. This was not successful either. We then attempted to culture chicken embryo cells with BRL conditioned media. This also was not successful. Finally, we cultured chicken embryo cells on a mouse feeder layer in the presence of conditioned media and obtained the cultured stem cells described herein.
A first aspect of the present invention is, accordingly, a method of producing undifferentiated avian cells expressing an embryonic stem cell phenotype. The method comprises collecting avian cells from an avian blastoderm prior to formation of the primitive streak, then depositing the avian cells in contact with a mouse fibroblast feeder cell layer, and then growing the avian cells on the mouse fibroblast feeder cell layer in the presence of a media containing leukemia inhibitory factor in a differentiation-inhibiting amount for a time sufficient to produce a sustained avian cell culture. The sustained avian cell culture consists essentially of undifferentiated avian cells having a large nucleus, a prominent nucleolus, and little cytoplasm (an "embryonic stem cell phenotype"). Typically, the undifferentiated avian cells are capable of maintaining the stem cell phenotype when grown on the mouse fibroblast feeder layer in the presence of the aforesaid media for at least three days, and even for 1, 2, 3, or 4 or more weeks.
A second aspect of the present invention is a sustained avian cell culture consisting essentially of undifferentiated avian cells having a large nucleus, a prominent nucleolus, and little cytoplasm (an "embryonic stem cell phenotype"). The cells are produced from ancestor cells isolated from an avian blastoderm prior to formation of the primitive streak.
A third aspect of the present invention is a veterinary pharmaceutical formulation comprising sustained avian cells as described above with respect to sustained avian cultures in a pharmaceutically acceptable carrier.
While applicants do not wish to be bound to any particular theory of operation of the invention, it appears that the use of an avian feeder cell layer, which would appear the logical choice if one wished to obtain avian embryonic stem cells, actually encourages the cells being cultured to differentiate towards fibroblasts. The solution to this problem appears to be the use of the mouse feeder cell layer. This, however, appears to raise a second problem in that the mouse feeder cell layer alone is insufficient to produce a sustained culture. This second problem appears obviated by the use of a media containing leukemia inhibitory factor in combination with the mouse feeder cell layer.
The foregoing and other objects and aspects of the present invention are explained in greater detail in the figures herein and the specification set forth below.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows chicken embryonic stem cells (passage 8) cultured on STO feeder cells in BRL-conditioned media 48 hours after passage. Several nests of cells with an embryonic stem cell-like phenotype can be seen.
FIG. 2 shows a confluent layer of chicken embryonic stem cells ready for passage. Stem cell colonies have expanded to join each other.
DETAILED DESCRIPTION OF THE INVENTION
The term "avian" as used herein refers to any avian species, including but not limited to chicken, turkey, duck, goose, quail and pheasant. Chicken is currently preferred.
The term "sustained" as used herein with respect to cells and cell cultures refers to a cell or cell culture capable of undergoing further cell division, even if the cells are eventually subject to senescence.
Avian embryos from which cells are obtained for carrying out the present invention are preferably in a stage prior to formation of the primitive streak, and most preferably in stage IX to XIV of development (i.e., a blastoderm). Such embryos may conveniently be obtained from eggs immediately after they are layed (referred to as "unincubated eggs"). Embryo cells are preferably collected from the central disk of the area pellucida. Other regions could be used, but this dilutes out the desired cells and requires subsequent isolation of desired cell colonies during growth in culture.
The feeder cell layer as used herein is constructed in accordance with procedures known in the art. As noted above, the feeder cell layer preferably consists of mouse fibroblast cells. STO fibroblasts are preferred, but primary fibroblasts are also suitable. Also, while the present invention has been described with respect to the use of mouse cell feeder layers, it is contemplated that feeder layers comprised of cells from other murine species (e.g., rat) or other mammalian species (e.g., ungulate, bovine, and porcine species) may also be used.
The media used in carrying out the present invention may be any suitable media containing leukemia inhibitory factor (LIF) in a differentiation-inhibiting amount. The media may be a conditioned media or a synthetic media containing recombinant LIF, both of which are known in the art. Conditioned media, and particularly BRL conditioned media, is currently preferred.
Cells from the unincubated avian embryo are seeded onto the feeder layer with conditioned media, and the avian cells give rise to nests of cells exhibiting a stem cell phenotype. Unlike the case with mammalian stem cells, it currently appears necessary to have both a suitable feeder layer and conditioned media, since avian ESC-like cells do not appear to survive when transferred to a feeder-layer alone or to BRL-conditioned media alone. The avian embryo cells of the present invention can be cultured for at least one or two months, which is significantly greater than the usual two week life of primary cultures of cells from the unincubated avian embryo.
Cell cultures of the present invention may be formulated for administration to animals by dissociating the cells (e.g., by mechanical dissociation) and intimately admixing the cells with a pharmaceutically acceptable carrier (e.g., phosphate buffered saline solution). Arian cells in such formulations may be prepared to carry a heterologous DNA sequence into an avian subject in the manner described in greater detail below.
Stem cells of the present invention are useful, among other things, as a tool for the study of embryological development (i.e., by labelling the cells with a marker gene and observing their distribution after injection in vivo) and the production of transgenic poultry. They are useful in allowing the application homologous recombination to the production of transgenic poultry.
In avian species, certain donor cell types have been isolated that retain viability when injected into recipient embryos. See Etches et al., in Avian Incubation, Chapter 22, Butterworth Publishers (1990); Verrinder Gebbins et al., Fourth World Congress on Genetics Applied to Livestock Production, Edinburgh, (1990); Petitte et al., Development 108, 185-189 (1990)). These studies showed that blastodermal cells derived from Stage X embryos (embryo at oviposition) remained viable when transferred to comparable recipient Stage X embryos. The present invention provides a new method of altering the phenotype of a bird and the birds so produced with the avian embryonic stem cells disclosed herein. The method comprises transfecting avian embryonic stem cells as disclosed herein with the DNA sequence in vitro (e.g., by electroporation or transformation with a retroviral vector), and then injecting the transfected embryonic stem cells into an egg containing an embryonic bird (e.g., into the yolk sac or onto the chorioallantoic membrane, preferably into the subgerminal cavity, and preferably during early embryonic development (e.g., prior to day 2 or 3 of incubation, and most preferably prior to day 1 of incubation)), with the DNA sequence being effective to cause a change in phenotype in the bird after hatch (e.g., a change in growth rate, feed efficiency, disease resistance, or a combination of all of these factors). Preferably, the egg into which the DNA is introduced is incubated to hatch, and the bird so produced raised to at least an age at which the change in phenotype is expressed. It is of no deleterious consequence if the transformed embryo and bird is chimeric, so long as a physiological response is achieved in the animal after hatch sufficient to evoke the phenotypic change sought.
The mechanism of in ovo injection is not critical, but it is preferred that the method not unduly damage the tissues and organs of the embryo or the extraembryonic membranes surrounding it so that the treatment will not decrease hatch rate. A hypodermic syringe fitted with a needle of about 18 to 26 gauge is suitable for the purpose. Depending on the precise stage of development and position of the embryo, a one-inch needle will terminate either in the fluid above the chick or in the chick itself. A pilot hole may be punched or drilled through the shell prior to insertion of the needle to prevent damaging or dulling of the needle. If desired, the egg can be sealed with a substantially bacteria-impermeable sealing material such as wax or the like to prevent subsequent entry of undesirable bacteria. It is envisioned that a high speed automated injection system for avian embryos will be particularly suitable for practicing the present invention. Numerous such devices are available, exemplary being the EMBREX INOVOJECT™ system (described in U.S. Pat. Nos. 4,681,063 and 4,903,625 to Hebrank), and U.S. Pat. Nos. 4,040,388, 4,469,047, and 4,593,646 to Miller. The disclosure of these references and all references cited herein are to be incorporated herein by reference. All such devices, as adapted for practicing the present invention, comprise an injector containing the embryonic stem cell as described herein, with the injector positioned to inject an egg carried by the apparatus with the DNA. In addition, a sealing apparatus operatively associated with the injection apparatus may be provided for sealing the hole in the egg after injection thereof.
The DNA sequence introduced in ovo with embryonic stem cells of the invention is, in general, a construct comprised of a promoter functional in avian cells and a gene encoding a peptide or protein operably linked to the promoter. Preferably, the protein or peptide is physiologically active and capable of producing a phenotypic change in the bird. In general, the DNA construct may be a linear DNA sequence (introduced into the embryonic stem cells of the invention by electroporation) or a sequence carried by a vector or other suitable carrier for transforming the embryonic stem cells of the invention, such as liposomes, calcium phosphate, or DMSO. Vectors, as discussed below, may be plasmids, viruses (including retroviruses), and phage, whether in native form or derivatives thereof.
Illustrative of genes encoding a protein or peptide are those which encode a protein or peptide selected from the group consisting of growth hormone, thyroid releasing hormone (TRH), Marek's MDX, and immunogenic recombinant antigens such as that for coccidiosis.
The production of cloned genes, recombinant DNA, vectors, transformed host cells, proteins and protein fragments by genetic engineering is well known. See e.g., U.S. Pat. No. 4,761,371 to Bell et al. at Col. 6 line 3 to Col 9 line 65; U.S. Pat. No. 4,877,729 to Clark et al. at Col. 4 line 38 to Col 7 line 6; U.S. Pat. No. 4,912,038 to Schilling at Col. 3 line 26 to Col. 14 line 12. Protocols for restriction endonuclease digestion, preparation of vectors, DNA purification and other such procedures were essentially as described in standard cloning manuals. See Sambrook et al., Molecular Cloning, a Laboratory Manual, (2d Ed., Cold Spring Harbor Press, New York (1989)).
A vector is a replicable DNA construct used herein to either amplify and/or express DNA encoding the gene of interest. A suitable expression vector will have controlling elements capable of expressing the cloned cDNA or genomic DNA placed in the correct orientation when the vector is introduced into the correct host. Such elements typically include but are not limited to a promoter region which interacts specifically with cellular proteins involved in transcription, enhancer elements which can stimulate transcription many-fold from linked heterologous promoters, a splice acceptor and/or donor sequences, and termination and polyadenylation signals. Also required is the sequence for a ribosome binding site capable of permitting translation which is operably linked to the gene to be expressed. Recently, a muscle-specific promoter has been isolated which is positioned upstream of both the skeletal muscle structural gene and the essential proximal promoter element and is operably associated with each. (Mar and Ordahl, Proc. Natl. Acad. Sci. USA 85, 6404-6408 (1988)). Vectors comprise plasmids, viruses (e.g. adenovirus, cytomegalovirus), phage, and DNA fragments integratable into the host genome by recombination. The vector replicates and functions independently of the host genome, or may in some instances integrate into the genome itself.
The present invention is explained in greater detail in the following non-limiting Examples.
EXAMPLE 1
Preparation of Feeder Cells
Gelatinizing culture dishes are prepared as follows. First, 0.1% gelatin is added to water to prepare a gelatin solution, which is then autoclaved. 4 ml of the gelatin solution is added to each plate for 6 cm plates, or 2 ml/well of gelatin solution is added to each well for 12-well plates. The plates or wells are incubated at 4° C. for 30 minutes, and the gelatin aspirated prior to use.
STO feeder cells (American Type Culture Collection No. CRL 1503) are prepared by culturing STO cells to 80% confluency in DMEM with 10% FBS. The cells are then treated with mitomycin C at 10 μg/ml for 2-3 hours, after which they are rinsed three times with PBS. After rinse, the cells are trypsinized with a 0.25% trypsin/0.025% EDTA solution, the cells collected in DMEM with 10% FBS, and washed at 1,000 rpm for 5 min. After washing, cells are suspended in 5 ml of DMEM w0.10% FBS and counted. The cells are then seeded onto gelatinized plates prepared as described above at a density of 1×10 5 /cm 2 and incubated overnight before use.
Primary Chicken Embryonic fibroblasts are prepared by harvesting fibroblasts from 10-day old chick embryos, subculturing the cells once, and then preparing the cells as feeder cells as listed for STO cells above.
EXAMPLE 2
Preparation of Conditioned Media
Buffalo Rat Liver (BRL) cell conditioned media is prepared by culturing BRL-3A cells (American Type Culture Collection No. CRL 1442) in DMEM w/10% FBS to confluency, then adding 13 ml of DMEM/10% FBS to each 75 cm 2 flask. Media is collected from the flask every third day, with each flask being collected three to four times. Media is stored at -20° C. For use, the media is filtered, adjusted to pH 7.5 with HCl, diluted to 80% BRL-CM with DMEM supplemented with 15% FBS, and the diluted conditioned media then supplemented with 0.1 mM β-mercaptoethanol.
LMH (chicken liver cell) conditioned media is prepared by culturing LMH cells in the same manner as for BRL-3A cells above, and the conditioned media prepared in the same manner as BRL-conditioned media as given above.
EXAMPLE 3
Isolation of Unincubated Chick Embryo Cells
To isolate stages IX-XIV embryo cells, the surface of a fertilized chicken egg is sterilized with 70% ethanol, the egg opened, and the yolk separated from the albumen. The yolk is then placed in a petri dish with the blastoderm in the uppermost position. A filter paper ring is placed over the blastoderm and the yolk membrane cut around the periphery of the ring. The filter paper ring with the embryo is then transferred to PBS with the ventral side uppermost, excess yolk removed, the embryo teased from the yolk membrane, the embryo transferred to cold PBS and rinsed with PBS. PBS is then removed, trypsin added, and the embryo incubated for 10 min. at 4° C. DMEM/10% FBS is added, the cells pelleted by centrifugation, the supernatant removed, and the cells resuspended in 80% BRL-CM. Embryo cells are then seeded onto the appropriate culture system.
EXAMPLE 4
Culturing of Avrian Embryonic Stem Cells
Using the procedures given above several methods of culturing cell with an embryonic stem cell phenotype from unincubated chicken embryos were carried out.
First, 10 whole embryos at stage X were isolated, dissociated, seeded onto chicken embryonic fibroblast feeder layers, and cultured with 80% BRL-CM. A significant amount of differentiation occurred, mainly cells of a fibroblast-like phenotype. Only a few clusters of cells remained relatively undifferentiated and contained large amounts of lipid. These cells grew slowly, if at all, and were lost by the second passage.
Second, 10 whole embryos at stage X were isolated, dissociated, seeded onto STO feeder layers, and cultured with 80% BRL-CM. Upon culture, the cells attached to the feeder layer and grew as small flattened colonies. In the first 3 passages, the cells lost all lipid droplets and exhibited a phenotype and growth characteristics similar to that observed for murine and porcine embryonic stem cells. Specifically, the cells contained a large nucleus with a prominent nucleolus and relatively little cytoplasm (see FIG. 1 and FIG. 2). The cells grew in nests with a generally uniform phenotype. Each nest remained a single cell thick as it grew, a characteristic shared with porcine, but not murine, embryonic stem cells. Unlike either murine or porcine cells, the nests of chicken embryonic stem cells exhibited the tendency to invade the feeder layer, pushing the STO feeder cells to the side or growing underneath the feeder layer. It was possible to culture these cells for 23 passages. In general, 10 6 cells were seeded onto a STO feeder layer in a 6 cm dish and in 2-3 days 2×10 6 to 5×10 7 CES cells could be obtained.
On the fifth passage, a portion of the CES cells were transferred to BRL-CM media alone. Initially, the CES cells grew rapidly and formed large ES-like colonies. When passed onto new gelatinized plates in BRL-CM, the cells differentiated into fibroblast-like cells, accumulated lipid droplets and died with the nest passage. Likewise, at the tenth passage a portion of the CES cells grown on STO cells and in BRL-CM were seeded onto STO feeder cells alone. These cells also became fibroblast-like, and could not be maintained on STO feeder cells alone. These observation suggest that the culture of chicken embryonic stem cells requires both a feeder layer and conditioned media.
EXAMPLE 5
Initiating and Maintenance of Chicken Embryonic Stem (CES) Cells
Chicken embryonic stem cells are initiated by isolating stage IX-XIV unincubated chicken embryos, and the area pellucida used as the source of cells for culture. Cells are seeded onto mitotically inactivated STO feeder layers with 80% BRL-CM and DMEM supplemented with 15% FBS and 0.1 mM β-mercaptoethanol. After the initial seeding, the phenotype of the chicken cells is observed daily. Eventually, a portion of the cells begin to lose their lipid droplets and begin to invade the feeder layer while remaining a closely packed nest of cells generally one cell thick. During the first few passages, the entire culture is passed onto new STO feeder layers until several nests of stem cell-like cells appear.
Once an initial culture shows several nests of stem cells, the cultures are maintained by trypsinizing the culture and counting the number of chicken embryonic stem cells. About 0.3 to 1×10 6 CES cells are seeded onto new STO feeder layers. The cultures are fed twice each day with BRL-CM and passed onto new feeder layers every 2-3 days, depending upon the density of the CES cells. Using this procedure, CES cells have been maintained for 23 passages (approximately two months). Data are given in Table 1 below.
TABLE 1______________________________________Yield of CES cells with each passage.Chick embryo cells were seeded at 3.5 × 10.sup.5 cells/6 cm plateat day 0.1 × 10.sup.6 cells were seeded with each passage.Day of Culture Passage Number Total CES × 10.sup.6______________________________________23 9 3.025 10 3.527 11 4.029 12 2.031 13 1.534 14 3.037 15 1.338 16 2.042 17 2.544 18 3.049 19 1.051 20 1.653 21 .7______________________________________
The foregoing examples are illustrative of the present invention, and are not to be construed as limiting thereof. The invention is defined by the following claims, with equivalents of the claims to be included therein. | A method of producing undifferentiated avian cells expressing an embryonic stem cell phenotype is disclosed. The method comprises collecting avian cells from an avian blastoderm prior to formation of the primitive streak, then depositing the avian cells in contact with a mouse fibroblast feeder cell layer, and then growing the avian cells on the mouse fibroblast feeder cell layer in the presence of a media containing leukemia inhibitory factor in a differentiation-inhibiting amount for a time sufficient to produce a sustained avian cell culture. Cell cultures produced by the aforesaid process and veterinary pharmaceutical formulations containing such cells are also disclosed. | 0 |
BACKGROUND OF THE INVENTION
1. Field of Art
This invention relates to an agricultural furrow opening tool for planting seeds in paired rows.
2. Description of Prior Art
It is commonly desirable to perform seeding and fertilizing operations in one pass over a field to be planted. This trend has continued with advancements in low-till and no-till planting implements. Ground working tools have evolved for planting in these no-till and low-till conditions and for improving seed bed utilization. Presently a wide variety of types of ground working tools are available for planting in various soil conditions. These ground working tools are generally categorized as disc types or hoe types. Existing ground working tools designed for working well in certain conditions are not always suitable in other conditions.
For many types of crops such as cereals and oilseeds, planting of the seeds is efficiently achieved by bulk metering. The seeds become generally evenly spaced as seeds are distributed at a seeding rate through distribution lines to ground working tools by which they are planted in rows in the soil. The rows are spaced to achieve the best possible utilization of the soil area, however other factors effect row spacing, such as the need to allow field trash to pass between ground working tools while they are pulled through the soil for planting. This has led to the development of paired row seeding tools which each plant two rows of seed to achieve good seedbed utilization with fewer tools thus also allowing good field trash flow. It is also common that these tools are also designed to simultaneously place a fertilizer row between the seed rows. Research has shown that precise placement of seed at particular spacing along side an appropriate amount and type of fertilizer improves yields.
One such ground working tool is provided according to U.S. Pat. No. 5,025,736 by Anderson. A hoe ground working tool is disclosed which has a narrow leading end for opening a furrow for placement of fertilizer. Trailing the leading end is a press plate which tapers to a wider rearward end from a forward end centered behind the leading end. The press plate is also angled downwards and rearwards from the leading end. It acts to press down on an area wider than the furrow opened for fertilizer for closing the fertilizer furrow and preparing a firm seedbed. It has a wear strip along each side of the press plate which is claimed to extend beyond the rear end of the press plate so that grooves are formed in the seed bed. A seed distribution tube carries seed to a divider disposed behind the press plate which randomly divides the seed into two streams directing the seed to the sides of the seed bed and into the laterally spaced grooves. However it is known that in some soil conditions, particularly that known as heavy soil, more aggressive action is required to close the fertilizer furrow. If this furrow remains unclosed and no level seedbed is formed, then a large amount of seed falls into the fertilizer furrow rather than being placed to each side. Fertilizer too close to the seed is toxic to the seed as it germinates and they will die.
A similar hoe ground opener is disclosed in U.S. Pat. 4,674,419 by Kopecky. An auxiliary press plate is disclosed which has somewhat more aggressive wings for forming seed furrows. The press plate has a main flat central surface which in operation is also angled downwards and rearwards from a leading end to press down over a fertilizer furrow created by a preceding narrow opener. The wings have inner surfaces that taper laterally and downwardly from the central surface and outer surfaces that are generally vertical. The wings inner surfaces also converge toward the rear of the plate and thus in operation push some soil inwardly to close the fertilizer furrow. Such an arrangement of surfaces is more aggressive at closing a fertilizer furrow. However in conditions of heavy soil, when the soil is wet it tends to be bulldozed by opener surfaces that are too aggressive or restrict passage of the soil. The soil can bind to a furrow opener's surfaces. In these conditions ground tools do not properly cover the fertilizer furrow and seed and fertilizer are scattered ineffectively. A planting tools fertilizer delivery openings can even become blocked by soil that is pushed and builds up in front of the seed furrow forming surfaces. In fact, the Anderson patent discloses using low friction plastic as a press plate to prevent binding of soil. This can lead to a costly construction.
Flexicoil Ltd. also discloses furrow openers as shown on pages 45-47 of their Product Book (volume 2). Two different openers are promoted for use in different soil conditions. For heavy soil an HS paired row opener is promoted having a main central surface that runs level in operation, and wings that form a seed furrow on each side of a fertilizer furrow. Since the main surface runs level, it does not tend to restrict passage of heavy wet soils. It produces paired seed rows that are spaced apart about 2.5 inches. However if such an opener is made with wings more widely spaced for wider space between seed rows, it has been found that this shape may not perform aggressively enough to properly close the fertilizer furrow in all conditions. An LS paired row opener is promoted for use in light soils. It does not include a central pressing surface and rather the wing surfaces converge at a central edge forming bottom surfaces in an inverted V arrangement. The central edge runs generally horizontal. The wings also have leading surfaces that face slightly inward and downward for gathering soil and directing it inwards and downwards as it passes beneath the opener, closing the fertilizer furrow. This shape however has found to be too aggressive for heavy soils which becomes stuck between the wings.
In heavy wet soils particularly, the soil tends to bind to seeding tool surfaces between paired furrowing wings when those surfaces intersect at small obtuse angles or have little or no radius between them so the intersection forms a more distinct edge. Soil binding is more problematic especially when the intersection of the soil deflecting surfaces is angled or transverse to the direction of travel, and even when the angle between surfaces is moderately obtuse. Even with a surface smoothly curved, if there is significant concave curvature in a plane in the direction of travel, the soil tends to bind in the concavity.
It is desirable to have a paired row opener that works well without compromise in a broader range of soil conditions without fouling, and one which plants seed rows spaced widely while minimizing soil surface disturbance.
It is desirable to have these paired rows spaced sufficiently wide, closer to rows of adjacent tools, so there are not large spaces between rows planted by adjacent tools. Thus, during harvest there is an even stand of stubble to support a swath of cut crop above the ground for proper drying.
The prior art openers are generally quite narrow for seeding pairs of seed rows that are spaced quite closely. Seedbed forming portions of these planting tools generally operate within a space following a fertilizer furrow opening portion in which field trash has been cleared by the fertilizer opening portion. The seedbed forming portions therefor generally operate in soil that is substantially clear of field trash. An additional challenge in designing seedbed forming sections that form wider spaced paired rows is that a wider paired row opener will encounter field trash at it's outer edges which must not become caught on the opener, fouling it's operation.
SUMMARY OF THE INVENTION
A basic object of the invention is to provide an improved paired row opener that works well without compromise in a broader range of soil conditions without fouling, and one which plants seed rows spaced widely while minimizing soil surface disturbance.
Thus, in one aspect, the invention provides a ground engaging paired row furrow forming tool comprising: a tool body having fore and aft ends, an outer edge on each of two opposing sides of the tool body; a furrowing wing adjacent each of the opposing sides and protruding from bottom portions of the tool body; the tool body having lower surfaces including a central front surface portion which is angled upwards towards the fore end and a center passage being defined between the wings and which passageway is in part defined by a central rear surface portion which is substantially aligned fore to aft in a direction of travel T during operation of the ground engaging tool.
In a further aspect the invention provides a ground engaging paired row furrow forming tool comprising: a tool body having fore and aft ends, said body having surface portions defining an outer perimeter extending on each of two opposing sides of the tool body; a furrow forming wing adjacent each of the opposing sides and protruding in spaced apart relation from bottom portions of the tool body; said tool body having lower surfaces including a central front surface portion which is angled upwards towards the fore end and which leads into a central passage extending rearwardly of the tool body between the wings, which passage is capable of being substantially aligned fore to aft in a direction of travel during operation of the furrow forming tool.
Other features and advantages of the invention will become apparent from the following description of a preferred embodiment and the appended claims.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a side view of a hoe planting tool used for one pass fertilizing and paired row seeding.
FIG. 1A is a perspective view of the planting tool in FIG. 1 .
FIG. 2 is a side view of a paired row furrowing and seeding tool.
FIG. 3 is a bottom view of the seeding tool in FIG. 2 .
FIG. 4 is a view of a cross section taken through a line of symmetry of the seeding tool in FIG. 5 .
FIG. 5 is a rear view of the seeding tool in FIG. 2 .
FIG. 6 is a top perspective view of the seeding tool in FIG. 2 .
FIG. 7 is a bottom perspective view of the seeding tool in FIG. 2 .
FIG. 8 shows agricultural implement on which a seeding tool as shown in FIG. 2 is typically used.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
A hoe planting tool 1 has a mounting portion 14 for securing to a shank 2 . A plurality of planting tools 1 and shanks 2 are typically attached to a tillage implement 7 to fore and aft spaced toolbars as can be seen in FIG. 8 with a plurality of them spaced transversely on each toolbar. The spaced arrangement is selected to allow the best passage of field trash between adjacent tools yet minimize soil ridging. Three to five toolbars are typically provided, depending on the spacing desired between planted rows. The implement 7 includes a hitch 9 for attachment to a vehicle such as a tractor for pulling the implement across a field. A product cart 8 can be towed behind the tillage implement 7 , or alternately between the tractor and implement 7 . The product cart delivers seed and fertilizer through distribution headers 5 , 6 and distribution lines 3 , 4 to the planting tools 1 for planting in the soil.
As seen in FIG. 1 the planting tool 1 comprises a narrow soil opener 10 and a paired row opener 20 . Possibly these could be made as an integral opener, but narrow opener 10 is useful alone or in combination with other openers. The hoe planting tool 1 is a combination tool for one pass fertilizing and paired row seeding. It operates in the soil at a set depth controlled by the tillage implement 7 . In such operation the soil opener 10 places fertilizer while the paired row opener 20 places seed. The opener 10 includes a furrowing tip 13 secured to the frontal lower body portion 15 of the opener 10 . The upper body portion 14 of opener 10 is adapted for securing to a previously noted shank 2 , in a well known manner. The opener 10 receives fertilizer at inlet 11 and directs it from a lower outlet 12 into a fertilizer furrow formed by furrowing tip 13 .
The paired row seeding tool 20 includes two furrowing wings 30 as best seen in FIGS. 4 and 5, protrude below the main body of seeding tool 20 . Seeding tool 20 receives seed at an inlet 21 and directs it from outlets 22 into paired furrows formed by lower surfaces of wings 30 . A passage from inlet 21 within seeding tool 20 divides into two passages having outlets 22 and randomly and evenly separates seed into a pair of streams to be placed in the paired furrows. The seeding tool 20 is fastened to the rear of the opener 10 by fasteners 19 in well-known manner.
The body of the seeding tool 20 generally includes lower surfaces and upper surfaces, certain of which converge together to form outer edges 35 extending along the left and right sides of the seeding tool. These outer edges 35 are curved inwardly and upwardly toward the front of the seeding tool 20 . This curvature provides for shedding of field trash which might otherwise become caught on the seeding tool, in which event its operation is fouled and proper furrows are not formed. Left and right tool body upper surfaces 34 are angled upwards and inwards from outer edges 35 to the narrower central body of the seeding tool 20 and extend generally straight fore and aft in the direction of operation. Rearward portions of the outer edges 35 are straight and the seeding tool 20 is operated with these straight portions generally horizontal and at a depth in the soil at which the soil surface is at or above the edges 35 and along the upper surfaces 34 . The upper surfaces 34 in operation slip below the soil surface with minimum disturbance of the soil surface.
Seeding tool 20 is also suitable in sizes that have a width exceeding the trash cleared zone created by the soil opener 10 . The outwardly curved outer edges 35 prevent trash being pulled into and under the furrowing wings 30 , and prevent trash from remaining caught on the edges 35 . Moving along edges 35 from front to rear it will be seen that they gradually curve into general alignment with the direction of travel, so the parts of the outer edges 35 that are subject to field trash are generally aligned with the direction of travel and tend to shed off the trash.
The bottom side of seeding tool 20 comprises a central surface, the profile of which can be seen in the cross section of FIG. 4 . The central surface includes a central front portion 24 and a central rear surface portion 23 (FIG. 3) extending rearwardly therefrom in alignment with the direction of travel T. (FIGS. 3 and 7 ). Rear surface portion 23 is preferably at least about ¾ inch wide. The central rear surface 23 preferably is generally flat and level when in operation and the central front surface 24 is preferably angled slightly upwards and forwards relative to central rear surface 23 . These surface portions 23 , 24 are preferably blended together by a smoothly curved transition region 25 (FIG. 4) between them rather than having a distinct edge at which they intersect. This curvature is generally convex fore to aft and helps prevent soil from binding. The central front surface 24 presses soil downwards at a decreasing rate as it passes beneath the surface so that soil is not simultaneously subject to pressure from the wings 30 in a combination of forces that may otherwise cause relative movement of the soil to stall. The tool is normally oriented in operation so the central front surface 24 is angled upwards from the horizontal. There is preferably about ⅜ inch rise in the central front surface 24 from the rear to the front edge.
A furrow forming wing 30 as previously noted is positioned to each side of the central surfaces 23 , 24 as seen in FIGS. 3 and FIG. 5 . Each wing 30 includes a forward lower surface 31 , an inner surface 32 , and an outer surface 33 . The dihedral angle between inner surfaces 32 of wings 30 is shown as being approximately 90° although this angle can be varied somewhat. The wing forward surfaces 31 are arranged in flanking relation to the central front surface 24 and each surface 31 extends laterally, rearwards and downwards from the central front surface 24 . The forward surfaces 31 are therefore inclined such as to slightly face each other, and they taper inwards and rearwards so in operation they direct some soil inwards and downwards over the fertilizer furrow formed by the soil opener 10 . The wing inner surfaces 32 extend outwards and downwards from the central rear surface 23 , and intersect with the forward surface 31 . The wing outer surfaces 33 extend inwards and downwards from outer edges 35 to intersect with surfaces 31 and 32 and defining furrow forming edges 36 which are angled inwardly from fore to aft before reaching the extension edges 36 which are parallel to each other and to the travel direction T. In FIG. 5 rear view it can be seen that wing inner surfaces 32 and outer surfaces 33 converge to form V-shape profiles which operate to form corresponding V-shaped furrows. The tips of the V-shapes (which are defined by the extension edges 36 ) are preferably spaced apart at least about 3 inches. The wing inner and outer surfaces 32 , 33 extend generally parallel to the direction of travel T thus giving the wings 30 a longer wear life in which they maintain their furrow forming profile. A forward part of each wing outer surface 33 is curved to follow the associated curved outer edge 35 . Preferably the forward surface 31 is curved toward the rear to blend with inner surface 32 so there is no distinct edge along the intersection of these surfaces. The central front and rear surfaces 23 , 24 also blend along curved intersections with wing forward surfaces 31 and wing inner surfaces 32 so there are no distinct edges of intersection. This promotes smooth soil flow and prevents soil binding which often is evident where surfaces intersect at edges, particularly at sharper angles.
The edges 36 of the forward surfaces 31 appear as substantially straight in a side profile as can be seen in FIG. 2 and FIG. 4 . This is generally the same across the forward surfaces 31 and through the intersections with the central front surface 24 so that there is little to no concave curvature or angles in a plane in the direction of travel, in which soil can hang up and bind. Central rear surface 23 provides a free central passage between wings 30 where the soil is not simultaneously subject to downward deflection as the V-shaped furrows are being formed. Preferably the central rear surface 23 provides a space of about ¾ inch minimum between the bases of the wings 30 to provide a free passage for soil flow. (This is in contrast to certain prior art designs in which a surface between furrow forming wings continues to deflect soil downwards during furrow formation.) A small fillet or radius is formed between the wing surfaces 32 and central rear surface 23 to provide free passage of soil.
Seed passage outlets 22 , best seen in FIG. 5, are positioned behind each wing 30 with the outlets terminating above the lowermost edge 36 of each wing, preferably a distance of ¾ inch, which provides good control of material placement and prevents soil from blocking the outlets.
In operation, the seeding tool 20 is generally oriented with central rear surface 23 substantially horizontal (see FIG. 4 ). It may be slightly trimmed from this orientation with central rear surface 23 angled one or two degrees upward or downward from front to rear, depending on soil conditions. This can be achieved by adjusting a stop on a tripping device supporting the shank 2 , or by using shims in mounting the ground engaging tool 1 to change its angle relative to the shank 2 .
Although the present invention has been described with reference to preferred embodiments, those skilled in the art will recognize that changes may be made without departing from the spirit and scope of the invention. | A ground-engaging paired row furrow forming tool includes a tool body having fore and aft ends with an outer edge defined on each of two opposing sides of the tool body. A furrowing wing is located adjacent each of the opposing sides and protrudes from bottom portions of the tool body. The tool body has lower surfaces including a central front surface portion which is angled upwards towards the fore end and a center passage is defined between the furrowing wings. This passageway is in part defined by a central rear surface portion which is adapted to be substantially aligned fore to aft in a direction of travel T during operation of the ground engaging tool. This paired row opener works well without compromise in a broad range of soil conditions without fouling and enables planting of seed rows spaced widely apart while minimizing soil surface disturbance. | 0 |
BACKGROUND OF THE INVENTION
Removal of contaminants or debris from a flowing liquid stream by the employment of a filter media comprised of particulated filter material is old in the art, as evidenced by the patents listed herebelow. These prior U. S. patents teach the advantages of using various different sizes of various different particulated filter material. Many of the described filter systems require that the filter media be removed from the filter vessel each time it becomes necessary to scrub the contaminant from the media, thereby enabling the media to be used many times. These prior art systems require a considerable amount of additional space, and complicated plumbing must be connected between the various pumps, valves, and other mechanical members in order to interconnect the scrubbing vessel and filtering vessel so that various different predetermined flow patterns are attained. A substantial amount of equipment is required in order to return the filter media to the filter vessel. In addition to the added cost and the required additional space considerations, all of the external plumbing presents a continued maintenance problem; and, the numerous additional mechanical connections involved therein greatly increase the likelihood of leakage occurring from the different components of the filter system.
Furthermore, when transferring the filter media from the filter vessel into the scrubber vessel, one is never absolutely certain that all of the filter media has been properly translocated from one to the other vessel. Hence, in the absence of visual or other exacting determinations, one is never sure exactly what has been scrubbed in the scrubber vessel. Moreover, after the filter media has been scrubbed in the scrubbing vessel, it is never certain that all of the filter media has been returned to the filter vessel, in the absence of exact determination thereof. Accordingly, it would be desirable to have made available a filter system wherein the filter media remains within the filter vessel for the entire life of the media, and wherein the filter media is scrubbed or rejuvenated without removing the filter media to a second vessel. A filter system which achieves these and other desirable and novel attributes is the subject of the present invention.
______________________________________THE PRIOR ART______________________________________Hirs 25,761 Martin 2,136,660Hirs 3,557,955 Stuart, Sr. 3,557,961Hirs 3,737,039 Toth 3,757,954Hirs 3,780,861 Maroney 3,812,969______________________________________
SUMMARY OF THE INVENTION
The invention encompassed by this disclosure broadly comprehends filtering a liquid through a filter media, and thereafter scrubbing the media insitu, and thereafter filtering a liquid through the scrubbed media. More specifically the invention includes a vessel within which there is enclosed a filter media comprised of particles of particulated filter material. A screen means is positioned at the lower end of the vessel and below most of the filter media, while the upper end of the vessel provides a liquid and scrubbing space, with there being a contaminated water inlet, and a clean water outlet attached to the vessel in a manner whereby flow of dirty or contaminated water is conducted into the upper end of the vessel, proceeds down through the filter media, where the filter media removes the contaminants from the flowing liquid, whereupon the clean water flows through the screen, through the outlet, and away from the vessel, leaving the contaminants and media within the vessel.
From time to time, as the removed contaminants progressively accumulate within the vessel, the filter media is scrubbed clean, thereby re-establishing the original filter efficiency. The scrubbing of the media is carried out within the vessel by flowing the liquid along a unique flow path within the vessel, to cause great agitation of the media, to thereby translocate the removed contaminants from the media into the scrubbing liquid. The highly contaminated scrubbing liquid is then discharged from the vessel in an unusual manner, while relatively clean make-up water is added thereto.
Next, the filter media is reset or repositioned into the lower end of the vessel by shutting down all systems which causes the media to gravitate to the bottom. Thereafter, the various flow lines are cleaned by flowing filtered liquid from the vessel, along a closed circuit, and back into the vessel, thereby separating any residual contaminants from the liquid. The filter system is placed back on stream and used until the contaminant load on the media again increases to a magnitude which justifies undertaking another cleaning cycle.
The scrubbing cycle preferably is achieved by disposing the inlet and outlet of a pump means within the upper end of the vessel, and directing the outlet of the pump towards a circulation guide means. The guide means is supported at a central location respective to the interior of the vessel, with the guide means preferably being located slightly above the prescribed media level. The outlet of the pump is connected to a discharge nozzle which is arranged slightly above and in axial alignment with the guide means. This unusual arrangement of the scrubbing apparatus enables the pump suction to take liquid from the upper end of the vessel and to force the liquid through the guide means, whereupon the guide means directs the liquid down towards the bottom of the vessel. This action sets up a desirable flow pattern wherein the filter media becomes intimately admixed with the liquid contained within the vessel and great agitation of the individual particles of the media achieves an unusually efficient cleaning and scrubbing action. The flow at this time follows a geometrical flow path which is in the form of a toroid having a central vortex which coincides with the axial centerline of the vessel, with the outer upward flowing part of the vortex being confined by the inner peripheral wall surface of the vessel.
In one embodiment of the invention, the circulation guide means is in the form of an annular area, with an annulus being formed between an outer barrel and an inner screen means. The inner screen means is preferably cylindrical and arranged to provide the before mentioned outlet through which the heavy contaminated scrubbing water is exhausted from the system during a blow-down cycle which occurs towards the end of the scrubbing cycle. Hence, the inner screen precludes significant loss of filter media from the vessel during the scrubbing cycle. Another screen means is mounted below the filter media near the bottom of the vessel and precludes significant loss of media during the main filtering cycle.
Accordingly, a primary object of the present invention is the provision of method and apparatus for sequentially filtering with and then cleaning a filtering media which is used to filter a stream of liquid.
Another object of the invention is to provide method and apparatus by which a contaminated stream of liquid is filtered for one interval of time to provide separation of the contaminants and the liquid, and the filter media is then scrubbed clean in a new and unobvious manner during another interval of time, with the filtering step and cleaning step both occurring within the same enclosure.
A further object of this invention is to disclose and provide a method of filtering a stream of contaminated liquid by flowing the contaminated liquid into a vessel having a liquid space and a filter media space; whereupon, the contaminated liquid proceeds through the filter media, thereby leaving the contaminant within the media, so that clean, filtered liquid exits from the vessel; and, thereafter, the filter media is scrubbed without removing the media from the vessel.
A still further object of this invention is to provide an unusual and unobvious filter system having particles of filter media contained therein which filters contaminants from a flowing liquid, and wherein the filter media is occasionally scrubbed clean of contaminants, and the contaminants removed from the system, with both the scrubbing and filtering action occurring within the same vessel.
Another and still further object of the present invention is the provision of method and apparatus by which contaminated liquid flows into a liquid containing part of a vessel, through a filter media containing part of the vessel, thereby filtering the contaminant from the liquid and providing clean liquid as the liquid stream exits the vessel. The filter media is scrubbed within the vessel by flowing liquid through a circulation guide means which agitates the mixture of liquid and filter media in a manner to cause the contaminants to be translocated from the media into the liquid. The contaminated liquid is replaced with relatively clean liquid, and thereafter the filter media is repositioned within the media containing part of the vessel. A closed circuit flow path cleans contaminated liquid from the lines, and the filter then resumes efficient operation until the load of contaminant on the media necessitates another scrubbing cycle.
An additional object of the present invention is the provision of apparatus by which a contaminated stream of liquid is cleaned by flowing the contaminated liquid through a vessel containing particulated filter material which separates the contaminants from the liquid as the liquid flows therethrough. The media is scrubbed within the vessel by the employment of a pump means which flows liquid within the vessel along a toroidal flow path achieved with a circulation guide means. The circulation guide means causes the contaminants to be translocated from the filter media into the liquid contained within the vessel so that the contaminated liquid can be disposed, while relatively clean liquid flows thereinto.
These and other objects and advantages of the invention will become readily apparent to those skilled in the art upon reading the following detailed description and claims and by referring to the accompanying drawings.
The above objects are attained in accordance with the present invention by the provision of a method for use with apparatus fabricated in a manner substantially as described in the above abstract and summary.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a part diagrammatical, part schematical, side elevational view of a filter system made in accordance with the present invention;
FIG. 2 is a diagrammatical representation of part of the system seen in FIG. 1, and showing the flow characteristics during one part of the cycle of operation of the system;
FIG. 3 is a part diagrammatical, part schematical representation showing the filter system of FIGS. 1 and 2, shown in another operative configuration;
FIG. 4 is an enlarged, more detailed, longitudinal, cross-sectional representation of a filter apparatus made in accordance with the present invention;
FIGS. 5, 6, 7, and 8, respectively, are cross-sectional views taken along lines 5--5, 6--6, 7--7, and 8--8, respectively, of FIG. 4;
FIG. 9 is a cross-sectional view taken along line 9--9 of FIG. 5;
FIG. 10 is an enlarged, detailed, cross-sectional view of part of the apparatus disclosed in some of the foregoing figures; and,
FIG. 11 is a fragmentary, detailed, part cross-sectional representation of a modification of part of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIG. 1, there is disclosed a filter system 10 made in accordance with the present invention. The system 10 includes a vessel 12 having an inlet 14 located at the upper extremity 16 thereof. A filter media level 18 is defined by the uppermost surface of the particulated filter material 20 which is enclosed within the lower end of the vessel 12. A screen means 22, which can take on several different forms, is supported within the lowermost end of the vessel, and preferably is comprised of an array of screens, the details of which will be more thoroughly discussed later on in this disclosure. The screen means 22 is connected to outlet 24.
The arrows at numeral 26 broadly indicate scrubbing apparatus, made in accordance with the invention, by which the filter media 20 can be scrubbed while remaining within the interior of the vessel 12. The scrubbing apparatus includes a pump means 28 having a suction 30 located to receive flow from the upper end 16 of the vessel, and further includes the illustrated outlet shown connected to an outlet nozzle 32. A circulation guide means 34 is provided with a guide inlet 36, annulus 38, guide outlet 40, and interior scrubbing screen means 42. A back-wash discharge 44 is connected to receive flow from annulus 38, with the back-wash flow being directed through screen 42, so that liquid exits through the back-wash discharge 44.
As best seen illustrated in FIG. 3, during a scrubbing cycle a toroidal flow path 46 is established within the vessel 12, with the entire contents of the vessel being forced to assume the toroidal flow path and flow from the lower end 48 to the upper end 16 of the vessel, as illustrated. Numeral 50 indicates an outer barrel which forms part of the circulation guide means 34.
In FIGS. 4-10, together with other figures of the drawings, there is disclosed additional details of the present invention. As seen in FIG. 4, for example, the free upper terminal end 52 of the scrubbing inner screen means 42 is positioned in close proximity of the circulation guide inlet 36. The scrubbing screen means 42 is supported by a vertical support conduit 54. Conduit 54 is connected to the back-wash discharge 44. Valve 56 controls the flow of liquid through the back-wash discharge.
The before mentioned outlet header 24 is connected to a three-way valve 58 which controls flow of liquid from the vessel to a clean water outlet 60, and to conduit 62, which is a feed pump suction for clean tube purge cycle. Numeral 64 generally indicates a plurality of lower screens, each of which are connected to the before mentioned outlet header 24. The lower screens are located near the bottom of the vessel 12, and the details thereof will be more fully discussed later on in this disclosure.
Three-way valve 66 is connected to control the flow of contaminated water to pump 67 and into the inlet 14, and to receive flow from conduit 62. Numeral 68 indicates the free terminal end of the piping which forms the inlet 14.
In FIGS. 4 and 10, a pump discharge line 70 is connected to the outlet of pump 28. The pump 28 preferably has the suction 30 thereof located within the upper end 16 of the vessel, below the liquid level thereof, so that inexpensive seals such as associated with an open impeller can be advantageously employed in the system. Numeral 72 indicates the interior of the inner scrubbing screen means. In FIG. 4, numeral 74 indicates the bottom of vessel 12 while numeral 75 indicates the top thereof. In FIG. 9, the lower screen 64 and inner screen 42 are seen to be provided with a plurality of slots 76 which are discontinuous, thereby leaving lands 78 by which the slotted screen elements are attached to one another. Numeral 80 indicates the interior of the lower screens.
In FIGS. 1 and 2, it will be noted that valve 58 is connected to provide flow along two different flow paths, one of which is a closed path defined by 24, 58, 62, 66, 67, 14, 16, 18, 20, and 22. The valve 58 is also connected to provide flow from 24, 58, 82, and into the wellhead W and down through the string of well tubing 84.
As seen in FIG. 2, during the filtering mode of the invention, flow occurs from inlet 14, proceeds down through the upper end 16 of the vessel 12 as noted by numeral 86, where the flow continues in a downward direction at 88 through the top 18 of the filter media 20 as indicated by the arrow at numeral 90, where the flow enters the lower screens 22 and continues through the header at outlet 24, thereby providing clean water free of contaminants.
In FIG. 10, numeral 92 indicates a build-up or layer of filter material on the inner screen, while numeral 93 indicates the absence of any appreciable amount of filter media attached to the inner screen. Numeral 94 and 96 indicate the dynamic flow of particles of filter material admixed with contaminants through the annulus 38. As indicated, the discharge nozzle 32 provides a flow at velocity V1 which is reduced to velocity V2 as the flow is induced through annulus 38. Velocity V3 indicates entrained liquid from proximity of the inlet end 36 of the circulation guide. Velocity V4 indicates the velocity of material exiting the circulation guide outlet. The arrows at numeral 98 indicate highly contaminated liquid flowing into the interior 72 of the scrubbing inner screen means 42.
The scrubbing cycle is diagrammatically disclosed in FIG. 3, wherein a toroidal flow path 46 is established down through the annulus 38 and up along the outer annular area of the vessel 12. Pump suction 30 is connected to pump 28 which provides flow through nozzle 32 of piping 70. During the first part of the scrubbing cycle, it is preferred that only the internal toroidal flow path 46 be employed. During the latter part of the scrubbing cycle, contaminants are evacuated from the liquid phase of the vessel as a back-wash discharge at 44, while make-up water at 67 replaces the discharged material.
In FIG. 11, a screen means in the form of a flat plate 164 has been substituted for the wedge tubes. The flat plate member 164 has closely spaced slots 132 formed therein, thereby forming a lower screen 164 for supporting the filter media 20. Outlet 124 is connected to chamber 125 formed by the lower screen means 164.
In FIG. 1, a pressure sensor is connected at 108 to pipe 24, and at 110 to pipe 14, thereby enabling the computer 112 to monitor the pressure drop across the media. Scrubbing pump 28 is controlled at 114, while the operation of valves 56, 58, and 66 are computer controlled by circuitry 116, 118, and 120. Feed pump 67 is computer controlled by circuitry 122.
The computer is programmed to switch the variables of the system to achieve various modes of operation in accordance with the desired program thereof.
OPERATION
The method of the present invention is set forth in FIGS. 1-3, wherein, in FIG. 1, there is disclosed a source of contaminated liquid S, as for example salt water containing the following contaminants: sludge, scale, dirt, fiber, and other debris of relatively small particle size which is inherently suspended within the liquid pumped at P1 and through the valve 66. The valve 66 is a three-way valve which enables liquid to flow from S into the inlet 14, or alternatively from valve 58 and then through the inlet 14.
In the first mode of operation, contaminated liquid enters the upper end 16 of the vessel 12 and flows down through the filter bed 20 in the indicated manner of FIG. 2, whereupon the contaminants are removed from the liquid, and clean liquid exits at header outlet 24. The clean liquid at 24 flows along conduit 24, through three-way valve 58, into the wellhead W of the illustrated borehole, down through the tubing string 84 and into a geological strata located downhole in the borehole.
It should be understood that the employment of clean filtered water at 24 for purposes of the illustrated water flooding at W is illustrative of one of a multitude of uses for the apparatus and method of the present invention. Similarly, the use of contaminated salt water at source S is illustrative of one of a manifold of different liquid streams requiring filtration which can be used according to method and apparatus of the present invention.
The filtering process continues in accordance with FIGS. 1 and 2 until the magnitude of the removed contaminants unduly increase the load on the filter media, causing the pressure drop across the media 20 to attain the threshold of uneconomical or inefficient operation. At this stage of the operation, valves 58 and 66 are moved to the alternate closed positioned while simultaneously pump 28 is energized and pump means 67 is rendered isolated, thereby setting up the illustrated toroidal flow path seen indicated in FIG. 3, which represents the second mode of operation and the first phase of the scrubbing cycle of the system. At this time, as illustrated in FIG. 10, the velocity V1, V2, V3, and V4 of the flowing material is of a sufficient magnitude to intimately disperse particles 94 of the entire media 20 and contaminants 96 throughout the liquid contained within the vessel 12, so that the individual particles 94 of the filter media 20 continually abrade against one another, and great sheer forces are setup between the agitated liquid, media, and contaminants. During this mode of operation, flow occurs from the upper end 16 of vessel 12, into suction 30 of pump 28, through discharge nozzle 32 of the scrubbing apparatus, down through the annular area 38, where the flow is directed down towards the bottom 74 of the vessel 12, with the flow pattern describing the illustrated toroidal configuration 46 set forth in FIG. 3. The scrubbing cycle is continued for the required length of time for translocating sufficient contaminants from the media into the scrubbing liquid required to subsequently restore the media to efficient filtering condition.
During the third mode of operation, which is also the second phase of the scrubbing action, valves 56 and 66 are moved to the open position, whereupon scrubbing liquid flows from the vessel while make-up liquid flows through pump 67 and into the inlet 14. Clean make-up liquid at 102 (FIG. 1) can be ingested into the system at 104 if considered necessary; however, it is preferred to use second order dirty water at S, depending upon the concentration of contaminants contained within liquid S during this blow-down or third mode of operation. The rate of flow of make-up liquid at 14 equals the rate of discharge of the highly contaminated liquid being discharged at 44.
When the discharge at D indicates that the residual liquid flowing at 46 has been substantially replaced by relatively clean liquid, the system is changed to the fourth mode of operation, wherein valve 56 is closed and pump 28 is de-energized. The system then lies dormant while the filter media gravitates back into a bed 20. This fourth mode of operation is an important step in the operational cycle for it causes the media particle size to be stratafied or layered with the media size being graduated towards the larger size in a downward direction. This novel action has the unexpected advantage of placing the larger particles of filter material adjacent to the lower screens which minimize plugging the screen openings. Next the system is caused to assume the fifth mode of operation, wherein the pump 67 is energized, and the apparatus is arranged into the scavaging configuration as follows: valve 56 remains closed while valves 58 and 66 are shifted, whereupon liquid flows along a closed circuit comprised of outlet 24, valve 58, conduit 62, valve 66, pump 67, inlet 14, where liquid flows into the upper end 16 of the vessel 12, down through the filter media 20, into the header 24, until the liquid contained within the closed circuit is cleaned of all contaminants, and the media bed is set into place in response to the pressure differential effected thereacross. Thereafter, valves 58 and 66 are moved to another alternate position, thereby returning the apparatus back to the first mode of operation or to the filtering configuration seen illustrated in FIG. 2. This last shift in operation provides an unexpectedly smooth transition in modes and eases the system back on line with a minimum of disturbances due to the unique uninterrupted closed to opened flow paths involved.
Example. A vessel 12, which measures 10 feet in diameter and 12 feet in height, is provided with a 75 horsepower pump means 28 having the suction and discharge thereof arranged in the manner of FIGS. 1 and 4, and capable of delivering 3000 gpm. The scrubbing apparatus 26 further includes a barrel 50 having an inside diameter 24 inches, and length 4 feet, with there being a scrubbing screen means 42 located therein having an outside diameter of 20 inches, and a length of 4 feet, thereby leaving an annulus 38 which measured 2 inches from the exterior surface of the inner screen to the interior surface of the barrel. The screen 42 is preferably a commercially available wedge wire tube having 0.015 inch openings. The free end 52 of the screen 42 is located approximately one inch below inlet end 36 of the barrel, while the discharge end of nozzle 32 is located above inlet end 36 of the barrel. The outlet end 40 of circulation guide 34 is located approximately 2 inches above the desired or design level 18 of media 12, which varies depending upon the compactness of the media 20 during operation as well as the amount of media charged into the vessel; consequently, sometimes the media is slightly above outlet 40 at the beginning of the filtration cycle, and sometimes the media is below the outlet 40 at the end of the cycle. The media selected is 12-20 particle size (screened) walnut shells. Support 54 is a standard 4 inch pipe.
The outlet header 24 is 6 inches in diameter while the individual screens 64 were laterally arranged respective to the header 24, and each is provided with an effective screening length of 2 feet. The screens 64 are provided with 0.015 inch slots. The screens 64 preferably are wedge wire tubes.
As noted, the screens in the above examples are preferably wedge wire tubes having bars connected together in the manner illustrated at 78 in FIG. 9, with there being an 0.015 inch slot between adjacent bars, and the bars being 1/8 inch in thickness. This material is a commercially available product.
The filter media 20 preferably is walnut hulls which passes through a 12 mesh screen and are caught on a 20 or 30 mesh screen, depending upon the characteristics of the removed contaminants.
Feed pump 67 is a 40 horsepower pump designed to deliver 1000 gallons per minute at 50 psi.
12,000 pounds of media 20 in the form of 12-20 walnut shells can be directly or indirectly charged into the lower end of the vessel 12, and all the compressible fluid thereafter exhausted from the upper end of the vessel as flow of liquid occurs at 14. The characteristics of the contaminated liquids were as follows: The inlet water is fresh or salt water containing inert particles of iron sulfide, sand, metal particles, and semi-soluble particles of oil, waxes, paraffins, asphalts, and the like.
After the system had reached equilibrium, the characteristics of the liquid exiting at outlet 24 was found suitable for injection into a downhole formation of a water flood injection well. The system removes the filterable solids and organics up to 1 ppm of a size greater than 1 micron depending on specific characteristics of the filterable contaminants.
The apparatus filters a stream of liquid flowing at a rate of 30,000 barrels per day into inlet 14, with the initial pressure drop measured at sensors 108 and 110 being 3-5 psi ΔP. At the end of 18 hours, the pressure drop across media 20 had increased to 15-25 psi ΔP, at which time the rejuvenation cycle was commenced in the above described manner. The scrubbing cycle was carried out for 20 minutes, with scrubbing action lasting 15 minutes, and with discharge through conduit 44 occurring during the last 14.5 minutes of the 15 minute cycle. During this 14.5 minutes, relative clean makeup water or second order dirty water entered the vessel at 67 flowing at the rate of about 600 gallons per minute into the inlet 14, while a similar amount of very dirty water was discharged at 44. Thereafter, a delay of 3 minutes enables the media to gravitate into a bed, as previously described above, and then valves 58 and 67 were shifted to the appropriate position to provide the closed circuit flow for a time interval of 2 minutes, thereby cleaning up all of the lines flowing from the clean water outlet 24, and setting the bed. The system was then returned to mode 1, or the on stream and filtering mode.
The method of this invention therefore involves five modes of operation as follows:
Mode 1: on stream or filtering for 18 to 24 hours;
Mode 2: scrubbing cycle, 15 minutes;
Mode 3: blowdown cycle, 14.5 minutes of the above 15 minutes;
Mode 4: gravitate bed into position, 3 minutes;
Mode 5: set bed and scavage closed circuit, 2 minutes.
Total rejuvenation time 20 minutes for modes 2, 3, 4, and 5. | A filter system has a filter media comprised of particles of filter material contained within the lower end of a vessel. Liquid flows into the upper end of the vessel and down through the filter media, thereby removing unwanted contaminants from the liquid. When the accumulated contaminant load in the filter media reaches a selected value, the filter media is cleaned of contaminants by vigorously circulating the media within the vessel. This scrubbing action transfers the contaminants from the filter media into the scrub water, and thereby enables the contaminants to be removed from the vessel by discharging the scrub water therefrom. All activity is stopped to enable the media to gravitate back to the bottom of the vessel. The cleaned filter is returned to operation. | 1 |
BACKGROUND OF THE INVENTION
The invention relates generally to an improved support and transport stand for a personal watercraft such as a jet ski, water scooter, or the like. More particularly, this invention relates to a stand which is capable of receiving the personal watercraft from a motor vehicle such as a pick-up truck, transporting the personal watercraft to the water over typical beach terrain and yet is collapsible for convenient storage when not in use.
Personal watercraft have become increasingly popular in watersport activities throughout the world. Utilization of these watercraft, which can easily weigh several hundred pounds, can however be severely limited by the ability of an individual to easily transport such craft to the water in a convenient and economical fashion.
Specialized personal watercraft trailers have been developed to be towed behind motor vehicles. In most instances, however, these trailers represent single purpose devices much the same as a conventional boat trailer. As is the case with respect to a boat trailer, these personal watercraft trailers require a paved trailer ramp into the water in order to launch the personal watercraft.
In addition, wheeled carts have been developed to carry personal watercraft over the sand or other beach terrain to transport the personal watercraft into the water. These carts, which usually include balloon type tires, are normally low to the ground and still require that the personal water craft be lifted onto the cart from a primary carrier such as a pick-up truck or trailer.
Further, loading or unloading ramps have been designed to remove personal watercraft from the back of a pick-up truck and directly into the water. In addition, there are also numerous winch and frame designs to load, unload and/or support personal watercraft. None of these winch and frame designs, however, are designed to be moved over typical beach terrain.
There exists, therefore, a need for a support and transport stand for personal watercraft to easily remove the watercraft from the back of a pick-up truck and transport the watercraft into the water. Such a design should be lightweight and collapsible into a smaller configuration for storage when not in use. The present invention fulfills these needs and provides further related advantages.
SUMMARY OF THE INVENTION
In accordance with the invention, an improved support and transport stand for personal watercraft is provided with a cradle at an adjustable height in accordance with the vehicle from which the personal watercraft is to be retrieved, for example, the height of the tailgate of a pick-up truck. Thus, the personal watercraft can be easily removed from the pick-up truck to the cradle of the support and transport stand whose width is also adjustable to accommodate varying sizes of personal watercraft.
The support and transport stand is provided with skids having spring-biased retractable wheels so that the stand can be easily transported over both pavement, sand and other surfaces common to a beach environment. It should thus be a simple matter to move the stand, including the personal watercraft thereon, into the water such that the personal watercraft can be utilized therein.
The stand is of a lightweight tubular construction with many of its elements telescoping to not only provide adjustability but also to provide reduced space requirements for storage when the stand is not in use. The legs are not only telescoping but are also pivotable to a stowed position underneath the cradle of the stand.
Other features and advantages of the present invention will become more apparent from the following detailed description, taken in conjunction with the accompanying drawings which illustrate, by way of example, the principles of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings illustrate the invention. In such drawings:
FIG. 1 is a perspective view illustrating the collapsible support and transport stand embodying its novel features and having a personal watercraft received thereon from the back of a pick-up truck;
FIG. 2 is a perspective view of the collapsible support and transport stand of FIG. 1 shown without the personal watercraft thereon;
FIG. 3 is an enlarged perspective view of the collapsible support and transport stand of the present invention illustrating the support legs in a collapsed and stowed position underneath the cradle for the support and transport stand;
FIG. 4 is an enlarged transverse vertical section taken generally along the line 4--4 of FIG. 3;
FIG. 5 is a side view of the collapsible support and transport stand having a personal watercraft thereon and illustrating transport over an uneven beach surface;
FIG. 6 is an enlarged side view of a spring biased retractable wheel mounted on the skid for the collapsible support and transport stand with the wheel extending beyond the skid upon which it is mounted; and
FIG. 7 is an enlarged side view of the spring-biased retractable wheel shown in a retracted position on the skid for the collapsible support and transport stand.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
As shown in the exemplary drawings, the collapsible support and transport stand for personal watercraft referred to generally by the reference numeral 10 is provided to receive and transport a personal watercraft 11 from the back of a motor vehicle such as a pick-up truck 12. As illustrated in FIG. 1, the stand 10 can be adjusted such that its height will be generally the same as the height of the tailgate 13 of the pick-up truck 12 for ease in transferring the watercraft 11 from the pick-up truck 12 to the stand 10.
As best illustrated in FIG. 2, the top of the stand 10 generally comprises an elongated rectangular cradle 14 having a starboard frame member 15 and a port frame member 16 both of a tubular construction. A plurality of cross frame members 17, 18, 19, and 20, also of a tubular construction, extend between the starboard frame member 15 and port frame member 16 to form the elongated generally rectangular cradle 14.
The forward cross member 17 includes an outer tubular member 21 extending from an elbow 22 on the port frame member 16. An inner tubular member 23, having an outer diameter slightly less than the inner diameter of the outer tubular member 21 is joined to the starboard frame member 15 by elbow 24 and extends into the outer tubular member 21.
A plurality of holes 25 are provided in the inner tubular member 23 having the same spacing and alignment as corresponding holes 26 in the outer tubular member 21 such that a pin 27 can be inserted through a pair of aligned holes 25 and 26 to secure outer tubular member 21 to inner tubular member 23 and establish a fixed distance between starboard frame member 15 and port frame member 16.
The aft cross frame member 20 is constructed similarly to the forward cross member 17 and includes outer tubular member 28 joined to the port frame member 16 by elbow 29 and inner tubular member 30 joined to the starboard frame member 15 by elbow 31. Pin 32 is used to secure the outer and inner tubular member 28 and through holes 33 and 34. A tow lope 51 can be secured to eye rings 50 in elbows 22 and 24.
The aft cross member 20 also includes a tee 35 pivotably disposed on the outer tubular member 28 and a tee 36 pivotably disposed on the inner tubular member 30. A generally U-shaped tailgate 37 extends between tees 35 and 36 and generally comprises an outer L-shaped tubular member 38 and inner L-shaped tubular member 39, with the inner member 39 telescoping within the outer member 38. Each of the tees 35 and 36 include holes 40, aligned with corresponding holes in the aft cross member 20 to receive a pin 41, to position and maintain the tailgate 37 in a vertical position with respect to the cradle 14 once the personal watercraft is loaded on the cradle 14. The pin 41 would be removed for loading and unloading so that the tailgate 37 can be pivoted out of the way to a position below the cradle 14, as depicted in FIG. 1.
The intermediate cross members 18 and 19 similarly include outer tubular members 42 and 43 and inner tubular members 44 and 45, respectively. Outer tubular members 42 and 43 extend from tees 46 and 47 respectively on the port frame member 16, while inner tubular members 44 and 45 extend from tees 48 and 49 respectively on the starboard frame member 15. Each of these cross members 18 and 19 are similarly telescoping to the forward and aft cross members 15 and 16.
A plurality of tees 53, 54, and 55 are slidably and pivotably disposed on the starboard frame member 15, while tees 56, 57, and 58 are similarly disposed on the port frame member 16. Forward, intermediate, and aft telescoping starboard legs 59, 60, and 61 extend from the tees 56, 57, and 58 respectively on the starboard tubular frame 15 to the starboard skid 65 while forward, intermediate and aft telescoping port legs 62, 63, and 64 extend from tees 56, 57, and 58 on the port tubular frame 16 to the port skid 66.
Each of the starboard legs 59, 60, and 61 include an outer tubular member 70, 71, and 72 respectively extending from tees 53, 54, and 55 to telescope with inner tubular members 73, 74, and 75 which extend from stubs 76, 77, and 78 respectively on the starboard skid 65. Each of the outer tubular members 70, 71, and 72 and each of the inner tubular members 73, 74, and 75 include equally spaced and aligned holes 79 and 80 respectively to provide for the insertion of a pin 81 to position the outer tubular member with respect to the inner tubular member and establish the height of the cradle 14.
On the port side, telescoping legs 62, 63, and 64 similarly include outer tubular members 82, 83, and 84 extending from tees 56, 57, and 58 to telescope with inner tubular members 85, 86, and 87 which extend from stubs 88, 89, and 90 on the port skid 66. Telescoping forward cross member 92, having an outer tubular member 96 and inner tubular member 97, extends between tee 94 on the forward starboard leg 59 to tee 95 on the forward port leg 62. A telescoping aft cross member 93, including outer tubular member 98 and inner tubular member 99, extends between the aft starboard leg 61 and aft port leg 64. The outer and inner tubular members 98 and 99 include a plurality of equally spaced and aligned holes such that a pin 111 can be inserted therethrough to maintain a parallel relationship between the starboard legs 59, 60, and 61 and the port legs 62, 63, and 64. Both the forward cross member 92 and aft cross member 93 are offset from the direct line between the forward legs 59 and 62 and aft legs 61 and 64 respectively to provide greater stability to the stand.
As best illustrated in FIGS. 5, 6 and 7, both the starboard skid 65 and port skid 66 include a plurality of spring biased retractable wheel member. For example, starboard skid 65 includes wheel members 100, 101, 102, and 103 generally equally spaced along the length thereof. Each wheel member is mounted to the skid 56 by means of a generally L-shaped bracket 109 which extends upward and outward from the skid 65. Each member generally comprises a shaft 105 disposed in a hole through the bracket 104 and includes a saddle 106 to receive an axle 107 upon which wheel 108 is mounted. A spring 109 extends between the top of the saddle 106 and the bracket 109 to bias the wheel 108 in a position extending below the bottom of the skid 65.
The wheel 65 can be retracted to a position which does not extend below the base or bottom of the skid 65 by compressing the spring 109 between the saddle 106 and bracket 104. A plurality of holes are provided in the shaft 105 to receive a pin 110 to hold the spring 109 in a compressed position as shown in FIG. 7. A spring-biased ball 111 near the end of the pin 110 can be utilized to maintain the pin 110 in the position as shown.
The collapsible support and transport stand 10 has been described as of a tubular type construction. Depending upon the specific application and more particularly the weight of the personal watercraft, the stand may be constructed of thick walled PVC plastic tubes and fittings. Alternately, either thin walled galvanized tubular steel or anodized tubular aluminum may be utilized with the structure either threaded or welded together to form the stand 10.
With the forward cross member 92 in place between the forward starboard leg 59 and forward port leg 62 and aft cross member 93 in place between aft starboard leg 61 and aft port leg 64, the stand 10 is rigidly maintained in its operable position as illustrated in FIGS. 1, 2 and 5. In this manner the stand 10, including a personal watercraft thereon, can be moved along typical beach terrain. When a paved surface is available, the wheel members can be maintained in their extended position as members 102 and 103 are shown in FIG. 5. If rough terrain or sand is encountered, the wheel members can be positioned and maintained in the retracted position as members 100 and 101 are shown in FIG. 5. The stand 10 can be easily pulled over either type of surface by a single person by means of the pull rope 51.
When the stand 10 is not in use the pins holding the forward cross member 92 and aft cross member 93 can be removed and the starboard legs and port legs pivoted apart from one another. The legs 59, 60, 61, 62, 63, and 64 can be telescoped to their shortest length and the port legs 62, 63, and 64 and skid 66 pivoted about port frame member 16 to a position underneath the cradle 14. Similarly the starboard legs 59, 60, and 61 and skid 65 can be pivoted about starboard frame member 15 to a position underneath the pivoted port legs and skid. This collapsed arrangement is generally illustrated in FIG. 3.
In order to maintain the stand in the position of FIG. 3, the intermediate legs 60 and 63 can be provided with clips 102. For example, clip 102 can be mounted on the outer tubular member 83 of the port leg 63. The open end of clip 102 would then receive outer tubular member 71 of starboard leg 60 to maintain the legs in the position shown.
Accordingly, the collapsible support and transport stand provide a simple and economical means to remove a personal watercraft from a pick-up truck and transport the watercraft into the water, which can be accomplished by a single individual. When not in use, the stand can be collapsed into a small space for storage until use is again required.
A variety of further modifications and improvements to the collapsible support and transport stand for personal watercraft of the present invention will be apparent to those skilled in the art. Accordingly, no limitation on the invention is intended by way of the description herein, except as set forth in the appended claims. | A collapsible support and transport stand is provided to receive a personal watercraft, such as a jet ski, water scooter, or the like from the back of a pick-up truck, for example, and to transport the personal watercraft into the water over typical beach terrain. The stand includes a cradle upon which the personal watercraft is supported and a plurality of telescoping legs which extend to a pair of skids having a plurality of spring biased retractable wheels. The telescoping legs are maintained in their support position transverse to the cradle by several telescoping cross members which extend therebetween. The cross members are adapted for disassembly to permit the legs to pivot to a stowed position underneath the cradle for ease of storage. | 1 |
RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application No. 60/438,175, Filed Jan. 7, 2003.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates in general to methods and devices for aligning adjacent plates prior to joining them together by welding, brazing, adhesive bonding, or the like.
2. Description of the Prior Art
In the field of welding, a number of clamping devices have been invented to serve the purpose of metal plate alignment. Daubon U.S. Pat. No. 4,513,955 proposes the expedient of an L-shaped member in which a working screw is threaded through one arm to apply pressure on one plate while the other arm is bolted to an angle bracket that is removably tack welded to the other plate. Varga U.S. Pat. No. 3,556,508 proposes a similar expedient except that the L-shaped member is welded to a flat bed and an adjusting screw is threadably mounted in the bed. The flat bed with the permanently mounted L-shaped member is removably tack welded to the plate. These proposed expedients require a specially manufactured flat bed or bracket that has a limited life because of the effects of repeatedly tack welding, breaking, and re-welding it in the same place. Both Varga and Daubon require the use of screws and threaded holes in the same mounting bracket that is consumed by repeated welding in the same spot. The tools for forming threads in holes are typically not immediately available to a welder at the job site where large plates are being welded together. Likewise, the removal and insertion of screws in clamps interrupts the flow of work and slows down the operation. If a small screw is lost it is often not immediately replaceable on a job site.
Conventional practice often comprises just cutting a C-clamp in half to form an L-shaped member much like that shown in Varga. The cut stub is then removably tack welded directly to a plate. Some part of the stub is consumed every time it is tack welded and then broken away from a plate, so the life of the tool is limited. The clamp itself is part of the tool so that when the bed or bracket is tack welded to a plate the clamp may be in the way or it may suffer damage during the welding.
Other prior proposed plate alignment expedients include, for example, Neuhaus, Apparatus for Clamping and Aligning Plates or the Like, U.S. Pat. No. 2,672,839, Howe, Welding Clamps, U.S. Pat. No. 3,342,479; and Minix, Alignment Clamp, U.S. Pat. No. 4,108,346. In general, these other proposed clamping devices are relatively complicated in design, difficult to manipulate, and subject to being easily damaged by the welding operation. In fact, the complicated designs make these devices more costly and time consuming to setup, remove, and maintain. Furthermore, many of these prior devices use a metal rod or a metal strap to feed through a thin gap between the plates to pull in a clamping member behind or underneath the plates to force the alignment. If the two plates are of different thickness, the upper or outer surfaces of the plates will not be brought into perfect alignment by the pulling/pushing force of the clamping member. Under such a situation, there is no way to make the adjustments that are necessary to achieve perfect alignment between the plates. Additionally, after the alignment is achieved and welding is completed, the metal rod or strap with the clamping member has to be removed from behind or underneath the plates. In some occasions, this may be very difficult or even impossible to do, especially where the welded plate is very large and heavy, or it forms part of a closed container. Another inconvenience of these proposed prior art expedients is that the holes left behind after the removal of the metal rods or metal straps have to be welded again to complete the job.
These and other difficulties of the prior art have been overcome according to the present invention.
BRIEF SUMMARY OF THE INVENTION
It is an object of the present invention to provide an alignment clamp and method that are very simple in design so that the manufacturing cost is low, and the cost of use is low. Another object of the invention is to provide an alignment clamp and method, which are very easy to setup before work, easy to remove after work, requires few steps for its use, and is rugged. A further object of the present invention is to provide a clamp and method to align metal plates of uneven or different thickness, or with curved surfaces, by individually adjustable mechanism repeatably usable in multiple setups. Yet another object of the present invention is to enable the clamping and alignment to be done only on one side of the metal or other plates, that is, the exposed upper side or the outer side. No part of the clamping member is behind or underneath the plates so that it has to be removed after the welding or other affixing is completed. The present invention is suitable for welding or other wise joining metal or other plates that are very large and heavy, which form a closed container, ceramic or plastic plates that are adhered or bonded together in other ways, or the like. A still further object of the present invention is to make alignment clamping possible without using a rod, strap or other element to feed through a gap between the two plates. As a result the plates can be joined together without gaps, and there will be no holes left behind to require sealing after the removal of the alignment clamp. Further, it is an objective to provide a simple separate anchor member that is reusable, disposable, and readily available, that can be handled and tack welded or otherwise breakably bonded or adhered to a plate without encumbering the clamp itself, and to which a clamp can be removably mounted without the use of additional tools. In addition, the traces left on the plate by spot mounting are easily removed during normal cleanup operations. It is an object of the present invention to provide an alignment clamp assembly and method that are adapted to all plate geometry, all materials of construction, and all methods and forms of plate joinder. Suitable plate materials include, for example, metals, ceramics, plastics, masonry, wood, and the like. Suitable plate joinder and breakable spot mounting methods and materials include, for example, arc or gas welding, plasma spray, brazing, soldering, sonic welding, solvent bonding, adhesive bonding, and the like. The methods and materials used for the purposes of plate joinder need not be the same as those used for breakable spot mounting purposes on the same job. Additional objectives will become apparent to those skilled in the art from the following teachings.
The present invention has been developed in response to the current state of the art, and in particular, in response to these and other problems and needs that have not been fully or completely solved by currently available expedients. Thus, it is an overall object of the present invention to effectively resolve at least the problems and shortcomings identified herein. To acquaint persons skilled in the pertinent arts most closely related to the present invention, a preferred embodiment of an alignment clamp that illustrates a best mode now contemplated for putting the invention into practice is described herein by, and with reference to, the annexed drawings that form a part of the specification. The exemplary alignment clamp assembly is described in detail without attempting to show all of the various forms and modifications in which the invention might be embodied. As such, the embodiments shown and described herein are illustrative, and as will become apparent to those skilled in the arts, can be modified in numerous ways within the scope and spirit of the invention, the invention being measured by the appended claims and not by the details of the specification or drawings. In a preferred embodiment of the invention, a clamp body member, for example, slidably engages an anchor member. The clamp body member includes for example, a force applicator element generally laterally spaced from a mounting element. The mounting element includes, for example, a generally arcuately extended semi-cylindrical socket portion. The generally cylindrical exterior of the anchor member is for example, of such a diameter that it slidably and snugly mounts the sectorial socket portion thereon. The axially opposed ends of the anchor member define end rim or circumference portions. The rim portions provide a plurality of spot mounting locations for spot welding, brazing or otherwise temporarily attaching the anchor member to a plate or other substrate. At least one of the force applicator or mounting elements is preferably adapted to the incremental application of force on an adjacent plate. According to one preferred embodiment, the body of the clamp bridges between the respective plates that are to be brought into line with one another. In this embodiment, the anchor member holds the mounting element to one plate, and the force applicator element is spaced from the anchor member generally along a lateral axis and bears on the other plate. This lateral axis is generally approximately parallel to the longitudinal axis of the anchor member.
In operation, in one preferred embodiment, a generally cylindrical anchor member is breakably spot mounted to a plate at one mounting location on a rim of the anchor member. A generally arcuately extended semi-cylindrical socket portion of the mounting element on a clamp body member is slidably mounted to the anchor member. A force applicator element on the clamp body member is positioned in engaging relationship to a second plate. Alignment between the respective plates is accomplished by incrementally adjusting one or both of the mounting or force applicator elements until the plates are brought to the desired alignment.
Other objects, advantages, and novel features of the present invention will become more fully apparent from the following detailed description of the invention when considered in conjunction with the accompanying drawings, or may be learned by the practice of the invention as set forth herein.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention provides its benefits across a broad spectrum of alignment clamp devices. While the description which follows hereinafter is meant to be representative of a number of such applications, it is not exhaustive. As those skilled in the art will recognize, the basic apparatus taught herein can be readily adapted to many uses. This specification and the claims appended hereto should be accorded a breadth in keeping with the scope and spirit of the invention being disclosed despite what might appear to be limiting language imposed by the requirements of referring to the specific examples disclosed.
Referring particularly to the drawings for the purposes of illustrating the invention and its presently understood best mode only and not limitation:
FIG. 1 is a perspective view of a preferred embodiment of a clamp body member according to the present invention.
FIG. 2 is a side elevational view of the embodiment of FIG. 1 showing the clamp body member aligningly mounted in an alignment clamp assembly with an anchor member to adjacent plates.
FIG. 3 is a perspective view of the embodiment of FIG. 2 .
FIG. 4 is a side view of two clamp body members of the embodiment of FIG. 1 aligningly associated with two cylindrical plates.
FIG. 5 is a partial rear elevational view of a preferred embodiment of an alignment clamp assembly showing a plurality of spot mounting locations on a rim portion of an anchor member.
FIG. 6 is a partial elevational view of another preferred embodiment of an alignment clamp assembly of the present invention showing a side mountable mounting element.
FIG. 7 is a perspective view of the attachment by breakably spot welding of an anchor member to a flat plate illustrating the best mode of practicing the invention as presently understood.
FIG. 8 is a perspective view of the embodiment of FIG. 7 illustrating the forces involved in utilizing a preferred embodiment of an alignment clamp assembly according to the present invention.
FIG. 9 is a perspective view of the embodiment of FIG. 8 illustrating the removal of a spot welded anchor member from a welded plate assembly.
FIG. 10 is a perspective view of a preferred embodiment according to the present invention illustrating several stages in the use of the present invention illustrating the best mode of practicing the invention as presently understood.
FIG. 11 is a partially broken side elevational view of an additional preferred embodiment wherein a force applicator is actuated from a side of the assembly.
FIG. 12 is a view similar to FIG. 4 illustrating in some additional detail the best mode of practicing the invention as presently understood.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings wherein like reference numerals designate identical or corresponding parts throughout the several views. It is to be understood that the drawings are diagrammatic and schematic representations of various embodiments of the invention, and are not to be construed as limiting the invention in any way. The use of words and phrases herein with reference to specific embodiments is not intended to limit the meanings of such words and phrases to those specific embodiments. Words and phrases herein are intended to have their ordinary meanings, unless a specific definition is set forth at length herein.
Referring particularly to FIGS. 1 through 3 of the drawings, there is illustrated generally at 1 a clamp body member at one end of which is an internally threaded block 6 , and at the laterally opposed other end is a mounting element 5 . A force applicator element in the form of a screw 2 is threadably received in block 6 . A floating pad or jaw 4 is mounted on the end of element 2 to provide accommodation for small misalignments or irregularities in the plates to which the alignment clamp assembly is to be applied. In this illustrated embodiment, element 2 is activated by the appropriate manipulation of handle 3 . Handle 3 is pivotally attached to the upper end of the threaded force applicator element. Handle 3 is spring loaded and foldable so that it can be used at the upright position for quick turning of the applicator element and at the horizontal position for stronger turning torque. Mounting element 5 comprises generally arcuately extending arms that in this embodiment define an arcuately extended semi-cylindrical socket portion 7 . The alignment clamp assembly includes an anchor member 8 , which in this embodiment comprises a short generally cylindrical section of pipe. Member 8 is breakably affixed to first plate 10 by means of a breakable spot mounting 9 at a location on the rim on one end of member 8 . Initially, first plate 10 is supported on first support 13 at a location where it is out of alignment with the adjacent edge of second plate 11 . Second plate 11 is supported on second support 12 . The socket portion 7 and the anchor member 8 are proportioned so that the sectorial socket portion slides over the anchor member. Where the plates are oriented at an angle to the horizon such that the socket portion 7 would slide off of the anchor member 8 under the urging of gravity, a detent is preferably provided to hold the socket portion and the anchor member in assembled configuration. Two detent elements in the form of screws 16 and 17 are illustrated at 16 and 17 , respectively. As will be understood by those skilled in the art, others forms of detent can be employed if desired. The application of force by element 2 causes the adjacent edges to be brought into alignment as shown particularly in FIG. 2 . Such application of force causes first plate 10 to be lifted off of its support 13 .
With particular reference to FIG. 4 , plates in the form of cylindrical pipes 24 and 25 are brought into alignment by the provision of three alignment clamp assemblies spaced generally equal angularly around the cylindrical pipes. The third alignment clamp assembly is hidden from view behind the pipes. The first and second clamp bodies 20 and 21 , respectively, are mounted in operative association with first pipe 24 through anchor members 22 and 23 , respectively. The three clamp assemblies function together much as a conventional tree-jawed chuck in a lathe. Precise alignment of the adjacent edges of pipes 24 and 25 is accomplished by adjusting the force applicator elements relative to one another.
The clamp body 58 illustrated in FIGS. 5 and 6 is mounted at one end to an anchor member 50 . The arms of mounting element 54 ( FIG. 5 ) encircle anchor member 50 through an arc of more than 180 degrees so as to retain the clamp body in assembled configuration to the anchor member. That is, the mounting element is defined by a generally arcuately extended semi-cylindrical socket portion. A sector is missing from the wall of the generally cylindrical mounting element so as to provide the clearance indicated at 68 . Clearance 68 permits the alignment clamp assembly to be formed without impediment from any engagement with the surface of the plate 56 . Clearance 68 also permits some rotational alignment of the clamp body as may be desired to effect alignment between a particular pair of plates. The permitted rotation is less than approximately 90 degrees because the partially encircling walls of the mounting element 54 extend through an arc of substantially more than 180 degrees. The longitudinal axis 51 ( FIG. 6 ) of the anchor member 50 is generally coincident with that of the mounting element 54 , and is approximately parallel with, if not coincident with, the lateral axis that extends between the force applicator element and the mounting element. A breakable spot mounting is illustrated at 52 . Spot mounting 52 mounts anchor member 50 to plate 56 . Preferably, a spot mounting is located as close as possible to the force applicator element. This, inter alia, reduces the moment arm of the force applied to the spot mounting, and tends to protect it from unintentional breakage. A detent element 48 in the form of a thumb screw is illustrated at 48 . Detent element 48 serves to prevent the mounting element and the anchor member from unintentionally disengaging by sliding axially of one another. The end rim of anchor member 50 provides a multiplicity of spot mounting locations as indicated at 60 , 62 , 64 , and 66 . When breakable spot mounting 52 is broken to release the anchor member from the plate, a fresh spot mounting location on the rim can be selected for purposes of remounting the anchor member to a new location on the same or a different plate. No reworking is required of the location on the rim where the spot mounting 52 was accomplished. Cycle time for mounting, using, de-mounting, and remounting is thus reduced.
Some locations are such that there is not room or it is awkward to slide the sectorial socket portion of the mounting element over the anchor element. The embodiment of FIG. 6 illustrates the side mounting of a mounting element 70 over anchor member 50 . One arm 74 of the mounting socket is pivotally mounted at 72 so that it swings to the open position illustrated at 76 . This is in the nature of a clam shell coupling, and it permits the mounting element to be moved sideways into engagement with the anchor member without any axial sliding of one relative to the other. A conventional detent, not shown, is provided to hold clam shell element 74 in the engaged configuration.
FIGS. 7 through 10 illustrate the operation of one embodiment of the invention. Anchor member 80 is breakably spot welded to first plate 86 by means of a welding member 84 . As shown particularly in FIG. 7 , a second plate 88 is positioned generally adjacent to but misaligned with first plate 86 so that the plates can not be welded at juncture 90 . Clamp body member 34 is assembled to anchor member 80 by sliding the mounting element 40 and generally cylindrical anchor member 80 axially of one another into a nested relationship. As illustrated particularly in FIG. 8 , the incremental application of force by means of rotating threaded force applicator 36 causes a downward force to be applied to plate 88 , and an upward force to be applied to plate 86 . This brings the two plates into alignment at their adjacent edges. The juncture 90 is welded at 92 ( FIG. 9 ). Anchor member engaging slot 46 on clamp body member 34 is engaged with the remote rim of anchor member 80 and upward force is applied to break the spot weld 82 . The anchor member 80 is then available for re-use at another location on the same or a different plate.
Often, large plates require alignment one segment at a time. This is diagrammatically illustrated, for example, in FIG. 10 . First plate 94 and second palte 96 are misaligned, and the misalignement is of such a nature that it must be addressed one segment of the juncture between them at a time. A first anchor member 98 was spot mounted at 102 to first plate 94 , a clamp member 34 was mounted thereto and adjusted, and first weld 104 was formed. The misalignement of the next segment of the juncture between these plates is illustrated, for example, at 110 . Clamp member 34 was slidably removed from engagement with first anchor member 98 , and slidably installed on third anchor member 108 . The removal of an anchor member from the surface of a plate is illustrated at 100 where the free end of the anchor has been twisted up away from the plate around the spot mounting at the other end so as to weaken and break the spot mounting. Once complete removal of the anchor is accomplished, it is available for re-use on the same or a different plate. The spot mountings are on the rims of the anchor members that are closest to the juncture between the plates. Removal of an anchor leaves a spot of weldment on the surface of the plate as illustrated at 106 . Typically, weldments are ground to smooth them. Grinding of the spot of weldment 106 serves to level the surface of the plate as may be desired.
A further embodiment of the invention is diagrammatically illustrated in FIG. 11 . In some situations it is desirable to be able to actuate the force applicator from one side of the clamp body. A clamp alignment assembly 112 includes a force applicator element 128 that is actuated by a laterally projecting threaded actuator 134 . Actuating force is applied to actuator 134 by the rotation through T-handle 136 or hex head 138 of a shank that is threadably mounted in clamp body member 114 so as to incrementally drive transmitting spheres 130 along actuator channel 132 . A floating foot pad or jaw 126 on the remote end of force applicator element 128 serves to accommodate slight angular misalignment between the first plate 116 and second plate 118 . Mounting element 122 is slidably mounted in nesting relationship to generally cylindrical member 120 . Anchor member 120 is attached by a spot mounting 124 at a rim location adjacent to force applicator 128 to second plate 118 . Movement of the force applicator element 128 responsive to the urging of force transmitting spheres 130 will cause the adjacent edges of plates 116 and 118 to move into alignment with one another.
FIG. 12 , for example, is illustrative of the best mode as presently contemplated of the clamp assemblies according to the present invention. The clamp body 34 is in the form of an inverted L-shape clamping arm and webbed for added strength. Thumb screws, of which 48 is typical, are provided for detent purposes so that no extra tools are required to actuate these detents. The threaded socket 38 is reinforced as illustrated for strength purposes. The threaded actuator 36 for applicator element 37 is incrementally actuatable by means of T-handle 42 or hex head 44 . In general, a third clamp assembly, not illustrated would typically be applied to the opposed side of the pipes 28 and 30 generally as described above with reference to FIG. 4 to align the edges of the curved plates along juncture 32 . Spot welds 140 and 142 serve to breakably mount the respective anchor members 22 and 23 to pipe 28 . Curved plates are used to illustrate this embodiment so that both sides of the clamp assemblies are visible. The geometry of the plates is not a part of the alignment clamp assemblies. The plates are the workpieces to which the clamp assemblies of this invention are applied. The use of curved plates in FIG. 12 is not intended to indicate that the invention or the best mode of practicing the invention are limited by the geometry of the plates.
Several sets of alignment clamps can be used to align the adjacent edges of the plates with fine adjustment and desired accuracy. Alternatively, one clamp can be used in one location with a partial weld formed as the desired alignment is achieved at that location. That one clamp can then be moved to another location, and the process repeated. This cycle of use can be repeated until the entire weld is formed. In one specific embodiment, several two and one-eighth long pieces of one and seven-eighth inch diameter metal pipe were spot welded to the surface of the metal plate along the welding edge, with the axis of each metal pipe parallel to the surface of the second metal plate but at right angle to the edge to be welded. An alignment clamp was mounted onto each plate. To align the edges of the plates to the same level, the threaded screw of the alignment clamp was turned until the edges of the plates were brought into alignment by raising one or lowering the other. Accurate alignment of the two edges was obtained by fine adjustments of the threaded screws of each alignment clamp. Then the two metal plates were welded together along the aligned edges in one operation. After the weld cooled down, the alignment clamps were removed from the one and seven-eighth inch short pipes by releasing the screws and sliding the clamp bodies off the pipe sections. The final steps of the process were to remove the one and seven-eighth inch diameter short pipes by striking them with a hammer or prying them off, and to polish the surface of the metal plate where the spot weld was located.
What have been described are preferred embodiments in which modifications and changes may be made without departing from the spirit and scope of the accompanying claims. Many modifications and variations of the present invention are possible in light of the above teachings. It is therefore to be understood that, within the scope of the appended claims, the invention may be practiced otherwise than as specifically described. | To align the edges of plates prior to joining them, a generally cylindrical anchor member is spot welded at one location on one of its rims to a plate. A mounting element of a clamp body member slidably engages the anchor member. A force applicator element of the clamp body member is generally laterally spaced from the mounting element. The mounting element includes a generally arcuately extended semi-cylindrical socket portion of such a diameter that it slidably and snugly mounts the socket portion thereon. The rim portions of the anchor member provide a plurality of spot mounting locations for breakably spot welding, brazing or otherwise temporarily attaching the anchor member to a plate or other substrate. At least one of the force applicator or mounting elements is adapted to the incremental application of aligning force on adjacent plates. The body of the clamp bridges between the respective plates that are to be brought into line with one another. Typically, the anchor member holds the mounting element to one plate, and the force applicator element is spaced laterally from the anchor member, and bears on the other plate. This lateral axis is generally approximately parallel to the longitudinal axis of the anchor member. | 8 |
CROSS-REFERENCE TO RELATED APPLICATION
This application is a divisional of application Ser. No. 10/458,260, which was filed on Jun. 11, 2003, now U.S. Pat. No. 6,839,296.
FIELD OF THE INVENTION
The present invention relates generally to a control clocks generator, and more particularly, to a control clocks generator and method thereof for a high speed sense amplifier (SA).
BACKGROUND OF THE INVENTION
Sense amplifier is typically used to read out the state, e.g., “0” or “1”, of the memory cell in a memory array, for example, ROM. A ROM array contains probably millions of memory cells arranged in rows and columns, each one of the memory cells in a column has a source that could be connected to a column source line, and during the sense amplifier is reading a selected memory cell, the column source line connected to the selected memory cell could be connected to a reference voltage or grounded. The drain of each one of the memory cells in a column is connected to an individual bit line, also known as column drain line, and during the sense amplifier is reading the selected memory cell, the column drain line connected to the selected memory cell is connected to the input of the sense amplifier. The control gate of each one of the memory cells in a row is connected to a word line, and the word line connected to the selected memory cell is connected to a predetermined voltage in the reading process.
During the reading operation, the current flowing through the selected memory cell is compared with a reference current to determine the selected memory cell is programmed with a “0” or a “1”. The reference circuit is coupled to the input of a current sense amplifier whose output is coupled to one input of a differential amplifier. When reading the selected memory cell, the differential amplifier compares the output voltage of the sense amplifier with the output voltage of another current sense amplifier coupled to the selected memory cell. If the reference circuit comprises a memory cell that is substantially identical to the selected memory cell, then the balance of the current sense amplifier is usually necessary to be broke for a reference current to be between the current of the selected memory cell being programmed with “0” and the current of the selected memory cell being programmed with “1”.
Precision control of the control clocks in timing is one of the fators for high speed operation in a sense amplifier. Unfortunately, due to the different process corners, temperature and voltage variations, the control clocks lack of well tracking capability and lead the sense amplifier difficult to be improved for the speed thereof. Referring to for example U.S. Pat. No. 5,771,196 issued to Yang, the control circuit consists of three blocks including the address transition pulse (ATP) generator, the precharge signal (PCB) generator and the latch signal (LATB) generator. The ATP signal is used as the trigger source of the control clocks, such as the precharge signal PCB, the latch signal LATB and the enable signal SAB of the sense amplifier. The precharge signal PCB should be the slower one of the word line delay and the bit line pull-up delay. For a flat ROM, the word line delay is much longer than the bit line pull-up delay, and thus, the word line delay is usually used to control the precharge signal PCB, and the width of the latch signal LATB should be larger than that of the precharge signal PCB. Further, the timing between the precharge signal PCB and latch signal LATB should be properly selected to latch correct data, and it is related to the sense time that is directly proportional to the memory cell current. The latch signal LATB is produced by adding a delay to the precharge signal PCB, in which the delay is controlled by the memory cell current from the mini-array, and the precharge signal PCB raises after several nanoseconds after the latch signal LATB to for correct data to be latched. In prior arts, the control signals are generated by referring to the memory cell current of the mini-array use in combination with RC (i.e., word line) delay and gate delay. Nevertheless, due to the different process corners, temperature and voltage variations, the control clocks lack of well tracking capability and as a result, it is difficult to improve the speed of the sense amplifier.
Therefore, it is desired a scheme to generate control clocks for high speed sense amplifier.
SUMMARY OF THE INVENTION
One object of the present invention is to provide a control clocks generator and method thereof for a high speed sense amplifier, by which control clocks are generated by use of the combination of RC delay, gate delay and reference sensing delay from the reference sense amplifier. As a result, it is obtained well tracking capability, regardless of process corners, temperature and voltage variations.
In a control clocks generator, according to the present invention, the address transition pulse signal is served as the trigger source to produce a precharge signal by a first RC delay and a latch signal by a combination of RC delay, gate delay and reference sensing delay induced from a reference sense amplifier, and the latch signal is further applied with a gate delay to produce a sense amplifier enable signal. In a prefered embodiment, the circuit to produce the latch signal includes three paths, among which the main path applies RC delay, gate delay and reference sensing delay to the address transition pulse signal, and the other two are used to add guard bands in front of and after the delay of the main path, respectively, for the latch signal to be located in a safe region. In particular, the second path applies RC delay and gate delay to the precharge signal such that the delay of the latch signal to the precharge signal is not over a maximum value, and the third path applies RC delay and gate delay to the address transition pulse such that the delay of the latch signal to the precharge signal is not smaller than a minimum value.
An improved sense amplifier is further provided to produce a sensing delay, which includes a reference data line to be coupled with the mini-array for memory cell current simulation. The improved sense amplifier seperates the precharge path and sense path, and connectes the precharge path and sense path with a common gated MOS pair, respectively, so as to adjust the sensing delay by changing the size ratio of the MOS pair.
As a result, the inventive control clocks generator and method has a sensing delay very close to the actual sensing delay, and thus provides the high speed sense amplifier with well tracking capability, regardless of process corners, temperature and voltage variations.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other objects, features and advantages of the present invention will become apparent to those skilled in the art upon consideration of the following description of the preferred embodiments of the present invention taken in conjunction with the accompanying drawings, in which:
FIG. 1 shows a scheme to generate control signals PCB, LATB and SAB in a sense amplifier;
FIG. 2 is a prefered embodiment control clocks generator according to the present invention;
FIG. 3 is a prefered embodiment reference sense amplifier according to the present invention;
FIG. 4 shows a typical RC delay circuit;
FIG. 5 shows a typical gate delay circuit; and
FIG. 6 shows a timing diagram of the control signals according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 is a block diagram to illustrate a scheme to generate control signals for a sense amplifier, in which an address transition pulse (ATP) generator 10 produces an address transition pulse signal ATP in response to a chip enable signal PCEB, and then a clock generator 20 produces three control signals from the ATP, including precharge signal PCB, latch signal LATB and sense amplifier enable signal SAB.
A prefered embodiment for the clock generator 20 is shown in FIG. 2 , which uses the address transition pulse signal ATP as a trigger source to produce the required control clocks. In the clock generator 20 , the two inputs of a NAND gate 21 a are coupled with the address transition pulse signal ATP and its delayed signal through an RC delay 22 a , respectively, and then the output of the NAND gate 21 a passes through an inverter 23 a to produce the precharge signal PCB. The circuit to produce the latch signal LATB is more complicated, which includes three paths, Path 1 , Path 2 and Path 3 , and the delay thereof is dominantly determined by the Path 2 to connect the address transition pulse signal ATP and its delayed signal from an RC delay 22 b to a NAND gate 21 b together with an inverter 23 b , and to further apply a gate delay 26 and a reference sensing delay 27 to the output of the inverter 23 b . On the other hand, the Path 1 applies an RC delay 24 and gate delay 25 to the output of the inverter 23 a , and the Path 3 connects the address transition pulse signal ATP and its delayed signal from an RC delay 22 c to a NAND gate 21 c together with an inverter 23 c and applies a gate delay 28 to the output of the inverter 23 c . Then the delays produced by these three paths Path 1 , Path 2 and Path 3 are combined to determine the latch signal LATB. In detail, after through an inverter 29 , the output of the reference sensing delay 27 is connected to a NOR gate 30 as well as is the output of the gate delay 28 , and the output of the NOR gate 30 is further coupled to an inverter 31 to be gated together with the output of the gate delay 25 by a NAND gate 32 and an inverter 33 to produce the latch signal LATB. In the operation, the timing of the latch signal LATB is dominantly controlled by the Path 2 , and the other two, Path 1 and Path 3 , add guard bands to the latch signal LATB, respectively, for the latch signal LATB to be in a safe region. In other words, the minimum delay of the latch signal LATB is controlled by the Path 3 , and the maximum delay is controlled by the Path 1 . The enable signal SAB for the sense amplifier is obtained by further applying a gate delay 34 to the output of the inverter 33 .
To achieve well tracking, the reference sensing delay 27 should be as close as possible to the sensing delay of the actual circuit, and FIG. 3 provides an improved sense amplifier 40 for this purpose. In the sense amplifier 40 , the precharge path and sense path are separated. Particularly, the sense path is built up from the supply voltage VDD through MOS 47 , 41 and 42 to the reference data line Dlref, and the precharge path is built up from the supply voltage VDD through MOS 48 and 42 R to the reference data line Dlref. The reference data line DLref is connected to the mini-array for memory cell current simulation. The NMOS 42 acts as a transmission transistor, and is common-gated with the MOS 42 R by a bias voltage Vx from the output of a NOR gate 43 . The precharge signal PCB is for the input IN of the sense amplifier 40 , and is applied on the gate of a PMOS 41 . The voltage on the sense node Vz passes through an inverter circuit composed of MOSes 44 a , 44 b , 45 a and 45 b and a latch circuit composed of inverters 46 a and 46 b to produce the output OUT. In the sense path, the PMOS 47 is connected as a diode to reduce the voltage swing of the sense node Vz and the sense time, without disturbing the precharge mechanism for the reference data line DLref, and the size of the NMOS 42 is increased in the safe range to improve the sense speed. Alternatively, the PMOS 47 as a diode could be replaced with an NMOS or a depletion NMOS. Furthermore, the precharge current could be adjusted by changing the size of the NMOSes 48 and 42 R for the reference data line DLref to be well controlled, without reducing the sense speed. The reference sensing delay produced by this sense amplifier 40 could be also adjusted by changing the size of the NMOSes 42 and 42 R.
Any commercial or conventional RC delay circuit can be employed for the RC delay shown in FIG. 2 , and FIG. 4 shows an example. The RC delay 50 of FIG. 4 includes a series of inverters 51 and 52 , resistor 53 and inverters 56 and 57 between its input IN and output OUT, a MOS 54 arranged between the input of the inverter 56 and the reference voltage or ground with its gate connected to the input of the inverter 52 , and an NMOS capacitor 55 connected to the input of the inverter 56 .
Likewise, any commercial or conventional gate delay circuit can be employed for the gate delay shown in FIG. 2 , and FIG. 5 shows an example. The gate delay 60 of FIG. 5 includes a series of inverters 61 , 62 , 64 and 66 between its input IN and output OUT. The input and the output of the inverter 64 are connected with NMOS capacitors 63 and 65 , respectively.
FIG. 6 is a timing diagram to illustrate the relationship among the control signals produced by the forgoing circuits. The address transition pulse signal ATP is first produced in response to chip enable signal PCEB and address signal ADD, and as mentioned in the above description, all the other control signals are produced according to the address transition pulse signal ATP. During period T 1 , the precharge signal PCB, latch signal LATB and sense amplifier enable signal SAB are produced, and due to the delays, the widths of the latch signal LATB and sense amplifier enable signal SAB are larger than that of the precharge signal PCB. During this period, the voltage of the sense node Vz will be pulled up to the level lower than the supply voltage VDD by a diode conductive voltage, for the diode 47 is inserted between the supply voltage VDD and PMOS 41 , and this period can be as the precharge period. Then, during period T 2 , the precharge signal PCB raises, and at this moment the voltage of the sense node Vz is changeable that will be sustained at high level or descended to a predetermined level depending on the data to be read out. Hence, this period could be as the sense period. During period T 3 , the latch signal LATB raises, and then the data is latched by the latch of the sense amplifier 40 . But the sense amplifier enable signal SAB raises a bit later than the latch signal LATB for the data to be latched properly. After period T 3 , the sense amplifier 40 could be turned off to decrease power consumption, and the output driver is turned on such that the correct data appear on the output bus, as designated by the data output DOUT in FIG. 6 .
While the present invention has been described in conjunction with preferred 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 that fall within the spirit and scope thereof as set forth in the appended claims. | A control clocks generator and method thereof for a high speed sense amplifier generates control clocks by utilizing RC delay and gate delay, in combination with reference sensing delay induced from a reference sense amplifier, and thereby, is tracking well for the high speed sense amplifier with process, temperature and voltage variations. | 6 |
This is a continuation of application Ser. No. 07/524,300, filed May 15, 1990, now abandoned.
BACKGROUND OF THE INVENTION
The invention concerns a press section of a paper or paperboard making machine, comprising a number of rolls which form press nips that dewater the web, the web being arranged to run through these nips, and of which rolls at least one roll is a smooth-faced so-called center roll, which forms a press nip with at least one other press roll, over which a press felt, which has been formed as an endless loop, is passed to absorb water from the web.
In a paper making machine, out of fiber pulp, a web is formed in the former of the paper machine, whereupon the formed web is passed, being supported and carried by one or more felts in the paper making machine, into the press section of the paper making machine, wherein both the web and the felts that support it are passed through nips formed by the rolls in the press section to absorb water from the web into the felts. From the press section the web is passed into the drying section of the paper machine. A conventional construction in a press section comprises a large and massive center roll as well as wire or felt loops grouped around it, the rolls placed inside these felt loops forming press nips either with one another or together with the center roll, and when the web runs through said press nips, water is drained out of the web by the effect of compression, this water being absorbed into the felts. In the drying section, water is removed from the web by means of evaporation, which is highly energy-consuming and therefore expensive and uneconomical. This is why attempts are made to remove a maximal proportion of water out of the web before it reaches the drying section, in the press section, by mechanical means.
It is known from the prior art that water is removed out of a web considerably more readily at an elevated temperature, because the viscosity of water and the springback coefficient of the web are thereby lowered together with the surface tension. Owing to this plienomenon, it has been previously found desirable to raise the temperature of the web in the press section. Based on this earlier experience, it can be established that, e.g., an increase in the temperature by 6° . . . 10° C. in the press section produces an increase of an order of 1% or more in the dry solids content of the web. An increased dry solids content in the press section produces considerable cost economies. For example, in paper making machines a rule of thumb is that, if the moisture content in the web in the press section can be lowered by 1%, the consumption of steam in the drying section is lowered by about 5%.
One drawback in the press sections which have been heretofore commonly used relates to the center roll in the press section. Generally, some suitable rock, such as granite, is used for the center roll. As is well known, rock rolls are quite sensitive to large and sudden changes in temperature, and the effects of such changes may be so severe as to crack the roll. This is why attempts have been made to develop suitable substitutes for granite rolls. As substitutes for rock rolls, e.g., rolls have been used which are coated, e.g., with a mixture of polyurethane and rock dust to make the surface properties of the roll similar to those of a rock roll. Advantages of metal rolls compared with rock rolls include their considerably better ability to tolerate variations in temperature. Moreover, owing to this phenomenon, they can be run at considerably higher temperatures than rock rolls. Moreover, a metal roll can be run at considerably higher running speeds than rock rolls.
A conventional construction of the press section of a paper machine wherein a center roll and a plurality of press rolls grouped around it are employed constitutes three press nips. In such a construction, the first press nip is formed between a grooved roll and a press-suction roll. In this construction, the second press nip is formed between a press-suction roll and the center roll, and a third press nip is formed between the center roll and a second grooved roll. Since, in the nips in the press section, it must be possible to make the linear loads as uniform as possible, in such a structure, as a rule, the grooved rolls are variable-crown rolls, preferably rolls whose crowns are variable in zones thereof. Thus, owing to the crown variation of the grooved rolls, in the first nip and in the third nip in the press section, a uniform linear load is achieved. In order that a linear load as uniform as possible can also be obtained for the second press nip, the mantles of the press-section roll and the center roll, which form the second press nip, are generally cambered. Because of the camber, a uniform linear load is never obtained for a nip and it is a further drawback of the cambering that the camber is always "fixed". If the camber has to be changed, the roll must be subjected to a grinding operation. This is a costly and laborious procedure. Also, cambering alone does not render the linear load profile subject to full control. For example, a problem with the metallic center rolls presently in use has been uneven heating. This has caused distortions in the linear load profile. Since the grooved rolls are provided with crown-variation means, the grooved rolls have been highly expensive. In this respect, the high cost has also been contributed to by the fact that it has been difficult to fit the crown-variation means inside a grooved roll, because the diameters of the grooved rolls are relatively small. When a fourth, separate press nip has been added to such a press section, a variable-crown grooved roll has also been used to achieve the fourth press nip.
Thus, to summarize the drawbacks of the prior art, they include high cost of construction, the aforementioned problems of uneven temperature related to metallic rolls, as well as the difficulties in providing uniform and, if necessary, adjustable profiles of linear loads in the press nips.
SUMMARY OF THE INVENTION
The principal object of the present invention is to provide a press section by means of which the drawbacks described above are minimized and by means of which an essential improvement is obtained with respect to increased dry solids content and increased running speed of a web passing through a paper making machine. A further object is to provide a structure to substitute for the rock rolls employed in press sections. With a view to achieving these objectives, the solution in accordance with the invention is mainly characterized in that the center roll is a variable-crown roll, which comprises a metallic roll mantle arranged so as to revolve around a stationary roll axle as well as at least one set of crown-variation means, which are arranged to load the roll mantle in the direction of the nip plane of the center roll and the roll that forms a press nip with the center roll so as to regulate the linear load profile in the nip.
As compared with the prior art, by means of the invention, a number of advantages are obtained, some of which have been heretofore discussed. With regard to the invention's advantages, the following can also be mentioned. First, in accordance with the invention, if necessary or desirable, two variable-crown rolls can be replaced by one variable-crown roll. Use of this option results in considerable economical savings. Since the crown-variation means are used exclusively in connection with the center roll, it is considerably easier to construct these members in the interior of the roll, because the available space is larger. With the use of the present invention, if desirable, it is also possible to control the profile of linear loads in the nip between a press-section roll and the center roll.
Moreover, by means of the structure in accordance with the invention, problems related to the uneven heating of the prior-art metallic center rolls are avoided. When the structure of the invention is used, the mantle of the center roll can be made thinner than in the prior art, whereby it has an improved thermal conductivity. If desired, the roll can also be used for heating the web. Nor is it necessary to grind any camber on a roll to achieve the press section structure in accordance with the invention.
An additional advantage obtainable by means of the invention is related to the construction of the grooved rolls that are presently used. Currently, the grooved rolls are manufactured such that they are provided with a suitable coating, e.g., of polyurethane. This results in their having a limited ability to tolerate heat. Variable-crown rolls, and in particular rolls whose crowns are adjustable in zones thereof, however, develop a considerable amount of heat. Since, when a structure in accordance with the invention is used, the grooved rolls therein do not have to be variable-crown rolls, they can be provided with cooling in a simple manner. An additional advantage is that the invention can be utilized as an addition to existing press sections. Other advantages of the invention are explained hereinafter in the detailed description of the invention.
BRIEF DESCRIPTION OF THE DRAWING
In the following, the invention will be described in detail with reference to the Figures in the accompanying drawings.
FIG. 1 is a schematical side view of the press section of a paper or paperboard making machine wherein a preferred embodiment of the invention is applied.
FIG. 2 is a corresponding view of an alternative preferred embodiment to the structure shown in FIG. 1.
FIG. 3 is a corresponding view of a further preferred alternative embodiment of the structures shown in FIGS. 1 and 2.
FIG. 4 shows yet another preferred alternative embodiment of a structure in accordance with the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
As is shown in FIGS. 1, 2 and 3, the web W is formed on the wire 50, which is either a fourdrinier wire or the carrying wire of a twin-wire former. On the downwardly inclined run of the wire 50 between the wire suction roll 51 and the wire draw roll 52, the web W is transferred on the detaching line P on the suction zone 14 of the pick-up roll 13 onto the first press felt 10, which, thus, also acts as the pick-up felt. The first press felt 10 carries the web W on its lower face into the first press nip N 1 , which is formed between two press roll, i.e. a press-section roll 11 and a grooved roll 22 or an equivalent roll provided with a hollow face 23. The first press felt 10 forms an endless loop by means of guide and alignment rolls (not shown), which also keep the first press felt 10 appropriately tensioned. The first nip N 1 is provided with two press felts, i.e. the first press felt 10 and a second press felt 20, the latter felt also forming an endless loop by means of guide and alignment rolls 21, which keep the second press felt 20 appropriately tensioned. The nip plane of the first nip N 1 is denoted with the reference K 1 notation.
After the first nip N 1 the web W is sucked by means of the suction zone 12 of the press-section roll 11 out of contact with the second press felt 20 onto the face of the first press felt 10 and, being guided by the press-suction roll 11, into the second nip N 2 . For this purpose, the press-suction roll is provided with a suction zone 12 of appropriate length, which ensures the detaching of the web W from the second press felt 20 onto the face of the first press felt 10. The second nip N 2 is formed between the press-suction roll 11 and the center roll 1 in the press section. After the second nip N 2 , the first press felt 10 is moved away from the center roll 1. Owing to the surface properties of the smooth-faced center roll 1, the web W is detached after the second nip N 2 from the first press felt 10 and adheres to the face of said center roll, under whose guidance the web W is thereupon transferred into the third nip N 3 in the press section. The third nip N 3 is formed between the center roll 1 and an opposite grooved roll 32 or an equivalent roll provided with a hollow face 33. Over this grooved roll 32, a third press felt 30 is passed, which is formed as an endless loop by means of guide and alignment rolls 31.
In the embodiments shown in FIGS. 1, 2 and 3, the press section further includes a fourth, separate press nip, in which case the fourth nip N 4 in the press section is formed between a second center roll 70, corresponding to the center roll, and an adjacent grooved roll 44 or an equivalent roll provided with a hollow face 45. After the third nip N 3 the web W is detached from the third press felt 30 onto the face of the center roll 1, from which it is detached by means of a transfer-suction roll 63. Thus, an open draw is formed between the center roll 1 and the transfer-suction roll 63. From the transfer-suction roll 63 the web W is transferred onto the fourth press felt 40 on the suction zone 42 of the suction roll 41, which acts as a pick-up roll. Between the transfer-suction roll 63 and the suction roll 41, there is also an open draw. The fourth press felt 40 is also a pick-up felt. The fourth press felt 40 is formed as an endless loop by means of guide and alignment rolls 43. The fourth press felt 40 transfers the web W into the fourth press nip N 4 , after which, owing to the surface properties of the second center roll 70, the web W is detached from the fourth press felt 40 onto the face of the second center roll 70. The nip plane of the fourth nip N 4 is denoted with the reference notation K 4 . From the second center roll 70, the web W is transferred onto the drying wire 60 by means of transfer-suction rolls 61 and 62, while the drying wire 60 transfers the web W further into the drying section (not shown).
FIG. 1 shows a first preferred embodiment of a press section in accordance with the invention. As is shown in FIG. 1, the center roll I in the press section is a variable-crown roll, which comprises a metallic roll mantle 2 which is arranged to revolve around a stationary roll axle 3. In the embodiment shown in FIG. 1, inside the center roll 1, crown-variation means 4 and 5 are fitted which act in the nip plane K 2 of the second nip N 2 as well as in the nip plane K 3 of the third nip N 3 , by means of which crown-variation means the roll mantle 2 is loaded in the nip planes K 2 and K 3 to produce the desired linear load profile. In the embodiment of FIG. 1, the crown-variation means comprise loading shoes supported on the roll axle 3 and acting upon the inner face of the roll mantle 2. Thus, in the embodiment of FIG. 1, the center roll 1 is a roll adjustable in zones thereof, wherein the crown variation is provided in two directions, which form an angle with each other. Thus, in the embodiment shown in FIG. 1, regulation of the respective linear load profiles is accomplished both in the second nip N 2 and in the third nip N 3 in the press section. Since, in the center roll in accordance with the embodiment of FIG. 1, there are two directions of crown variation, it is necessary to employ precisely the above-mentioned loading-shoe constructions for the crown variation relay. If a crown variation were provided in the center roll 1 in one direction only for example, either in the nip plane K 2 of the second nip N 2 or in the nip plane K 3 of the third nip N 3 , in such a structure it would be possible to employ any crown-variation means used in the prior art.
In the embodiment of FIG. 1, if necessary or desirable, it would also be possible to provide crown-variation means in the grooved roll 22, in which case the linear loads profile could also be controlled in the first part N 1 of the press section.
As has been heretofore mentioned, the press section shown in FIG. 1 also includes a fourth press nip N 4 . Thus, in the embodiment of FIG. 1, the second center roll 70 is arranged as a variable-crown roll, so that the second center roll 70 comprises a hollow, metallic roll mantle 71, which is arranged to be revolving around a stationary roll axle 72. In the interior of the roll mantle 71, crown-variation mans 73 are provided, by which means the fourth nip N 4 is loaded in the direction of the nip plane K 4 to produce the desired linear load profile. In FIG. 1 it is shown that in the second center roll 70, as the crown-variation means 73, a loading-shoe construction similar to that described above in relation to the center roll 1 is used. However, since in the fourth, separate press it is necessary to control one regulation direction only, as the crown-variation means 73 it is possible to use any structure that has been used for this purpose in the prior-art. Thus, if necessary, or desirable, in the embodiment shown in FIG. 1, it is possible to control linear load profiles in all the press nips in the press section.
The second embodiment of the invention shown in FIG. 2 differs from that shown in FIG. 1 in the respect that, in the center roll 1, crown-variation means 4 are provided in the nip plane K 2 of the second nip N 2 only. Owing to this, in the embodiment shown in FIG. 2, as crown-variation means 4 it is possible to use any structure that has been used. In FIG. 2, the linear load profile is also regulated in the first nip N 1 in the direction of the nip plane K 1 so that the grooved roll 22 is formed as a variable-crown roll. Thus, the grooved roll 22 comprises a tubular roll mantle 24, which is mounted to revolve around the stationary roll axle 25. Inside the roll mantle 24, the necessary crown-variation means 26 are provided to regulate the linear load profile in the nip N 1 . Since herein one direction of regulation only is concerned, as a crown-variation means it is possible to use any structure that has been used for this purpose in the prior art.
With a view to regulating the linear load profile in the third nip N 3 in the press section, in the embodiment shown in FIG. 2, the grooved roll 32 in said third nip N 3 is formed as a variable-crown roll, whose construction corresponds to that of the grooved roll 22 in the first nip N 1 described above. Thus, the grooved roll 32 comprises a tubular roll mantle 34, which is arranged to revolve around the roll axle 35. Further, inside the roll mantle 34, crown-variation means 36 is provided, which acts in the nip plane K 3 of the third nip N to regulate the profile of linear loads. Since, in this case as well, regulation is required in one direction only, the crown-variation means 36 can be embodied in several known structures. As the crown-variation means 36, it is possible to employ, for example, the loading shoes shown in FIG. 2, but in their place it is also possible to use, for example, a pressure fluid clambers or a series of such chambers provided between the roll axle 35 and the roll mantle 34. In the fourth, separate nip N 4 in the press section, in the embodiment shown in FIG. 2, the regulation of the load profile is arranged in a manner differing from that of FIG. 1. In the embodiment shown in FIG. 2, the grooved roll 44 in the fourth nip N 4 is arranged as a variable-crown roll so that the roll 44 comprises a tubular roll mantle 46, which is arranged to revolve around the axle 47 of the roll. Inside the roll mantle 46, crown-variation means 48 similar to the crown-variation means 26 and 36 of the grooved rolls 22 and 32 in the first nip N 1 and in the third nip N 3 are provided. Thus, in this embodiment, for the fourth nip N 4 , it is possible to employ a conventional metal roll or even a rock roll as the center roll 70.
The third embodiment of the invention, shown in FIG. 3, combines some of the structural elements of the embodiments shown in FIGS. 1 and 2. In the structure shown in FIG. 3, control of the linear load profiles in the first, second and third nips N 1 , N 2 , N 3 in the press section is achieved in the same respective manners as in the structure shown in FIG. 2, and in the fourth nip N 4 in the same manner as is shown in FIG. 1.
The embodiment shown in FIG. 4 differs from the embodiments of FIGS. 1-3 as follows. With respect to the first nip N 1 in the press section, the structure is similar to that described in the above mentioned embodiments. However, in FIG. 4, the second nip N 2 in the press section is not formed between the press-suction roll 11 and the center roll 1, but in this embodiment, on the run of the first press felt 10 after the press-suction roll 11, a grooved roll 15 or an equivalent roll provided with a hollow face 16 is provided, which forms the second nip N 2 in the press section with the center roll 1. The first press felt 10 is formed as an endless loop, as is the case in the other embodiments, by means of guide and alignment rolls 17. In the embodiment of FIG. 4, the construction and the operation of the center roll 1 are identical with those of the center roll shown in FIG. 1. The grooved roll 32 in the third nip N 3 and the related constructions are also, in this embodiment, identical with those shown in FIG. 1. In the solution of FIG. 4, a fourth, separate press nip is not shown but in this structure the web W can be transferred by means of the transfer-suction roll 63 directly onto the drying wire (not shown). It is clear, however, that this embodiment can also be provided with a fourth, separate press nip similar to that described in relation to the embodiments described above. In a corresponding way, it is fully clear that the embodiments of FIGS. 1, 2 and 3 may also be accomplished without a fourth, separate press.
Details of the present invention may easily vary within the scope of the inventive concepts set forth above, which have been presented by way of example only. Therefore, the preceding description of the present invention is merely exemplary, and is not intended to limit the scope thereof in any way. | The invention concerns a press section of a paper or paperboard making machine, comprising a number of rolls (1, 11, 22, 32, 44, 70) which forms press nips (N 1 , N 2 , N 3 , N 4 ) that dewater the web (W) with each other, the web being arranged to run through these nips. Of the rolls at least one roll (1;70) is a smooth-faced so-called center roll, which forms a press nip (N 2 , N 3 ;N 4 ) with at least one other press roll (11, 32, 44), over which a press felt (10, 30; 40), which has been formed as an endless loop, is passed to absorb water from the web (W). The center roll (1; 70) in accordance with the invention is a variable-crown roll, which comprises a metallic roll mantle (2; 71) arranged to revolve around a stationary roll axle (3; 72). The roll includes at least one set of crown-variation members (4, 5; 73), which are arranged to load the roll mantle (2; 71) in the direction of the nip plane (K 2 , K 3 ; K 4 ) of the center roll (1; 70) and the roll (11, 32; 44) that forms a press nip N 2 , N 3 ; N 4 ) with the center roll so as to regulate the linear load profile in the nip (N 2 , N 3 ; N 4 ). | 3 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This is a continuation of application Ser. No. 10/192,726 filed 11 Jul. 2002, now abandoned which is a continuation of application Ser. No. 09/619,647 filed Jul. 19, 2000, now U.S. Pat. No. 6,441,802 which is a continuation of application Ser. No. 09/374,263 filed Aug. 16, 1999, U.S. Pat. No. 6,100,857, which is a continuation of application Ser. No. 08/969,313 filed Nov. 13, 1997, U.S. Pat. No. 5,969,697, which is a continuation of application Ser. No. 08/230,369 filed Apr. 20, 1994, abandoned.
BACKGROUND OF THE INVENTION
(1) Field of the Invention
The present invention relates to an interactive processing apparatus for interactive processing of plural displays, and a method thereof.
(2) Description of the Prior Art
Current monitoring and controlling systems have a large display installed in front of operators in order to display overview information such as a system configuration map of a total system, alarms for indicating that something unusual is occurring, for allowing all the operators to grasp a condition of the system at a glance at any time. On the other hand, a display at hand prepared for respective operators displays integrally more detailed information. The amount of the detailed information displayed on each display at hand is numerous, and it is not rare to reach hundreds of images in a large scale system.
The operators monitor using both the large display and their display at hand. The operators grasp entire system states by watching the overview information on the large display, and when an abnormal condition is detected, they examine more detailed data by using their own display at hand and perform necessary control operation.
However, because information displayed on the large display and information shown in displays at hand are independently controlled, a conventional system required a complex operation to provide the necessary information to both in connection with each other. For instance, when a warning lamp blinks on the large display, the operators must retrieve an image displaying control data for the warning from hundreds of images by selecting menu repeatedly. Therefore, there has been a problem of a delayed response to an emergency such as an abnormal condition occurrence or an accident.
SUMMARY OF THE INVENTION
(1) Objects of the Invention:
One of the objects of the present invention is to provide a man-machine interface which is capable of referring related detailed information just by designating an objective on the large display. For instance, a man-machine interface such as the one wherein detailed information on a warning and control data related to it are displayed in a display at hand just by pointing to a blinking warning on the large display, and control data and setting devices related to an apparatus are displayed on a display at hand only by pointing to the apparatus in a system configuration map on the large display.
When realizing such a man-machine interface as the one above described, an important point to be considered is that the large display is shared by a plurality of operators. A monitoring and controlling system is operated by collaboration of plural operators, each of them is in charge of a different operation respectively, such as an operator in charge of operation, an operator in charge of maintenance and inspection, and a chief on duty for controlling total operation. Accordingly, the large display is shared by operators who perform different tasks simultaneously, which is different from a case of display at hand which is prepared for individual operators. Therefore, the above described interface must satisfy the following requirements:
(1) No disturbance to other operator's operation:
There is a possibility to hide information which has been watched by other operators when information necessary for only a specified operator is displayed arbitrarily on the large display.
(2) Simple retrieval of information necessary for individual tasks by respective operators:
Necessary information differs depending on contents of the charged task. For example, when a warning light indicating an abnormal condition of a boiler blinks, an operator in charge of operation examines control data such as a flow rate of fuel, while an operator in charge of maintenance examines an inspection record of the boiler. Accordingly, it is necessary for operators to be able to quickly retrieve information necessary for them without being distracted by information for others.
(3) An operating environment suitable for tasks assigned to each operator:
Commands used frequently and permission for operation differ depending on the task charged to respective operators. Accordingly, it is desirable that the operating environment such as a structure of menu and an operable range of operation can be customized for respective operators.
The object of the present invention is to provide a man-machine interface which satisfies the above requirements.
(2) Methods of Solving the Problems:
In accordance with the present invention, the above described objects can be realized by providing a registering means for registering an attribute of a respective operator to an input means, a process selecting means for selecting process contents based on the attribute responding to a process request from the input means, and an executing means for executing a process selected by the process selecting means and outputting to an output means selected based on the attribute, to an interactive processing apparatus having a plurality of input means and a plurality of output means.
An operator registers his own attribute, for example, charged task, etc, to his operating input means using the registering means. When the operator requests a process for displaying related information and menu from the input means, the process selecting means examines the operator's attribute which has been registered in the input means, and selects a process corresponding to the attribute. The executing means executes the process selected by the process selecting means, and outputs a result of the execution to an output device matched to the attribute, for example, a display at hand of the operator. In accordance with the execution of the process based on the operator's attribute, displaying only necessary images for the operator and providing convenient operating environment for the operator to operate in, can be realized. Furthermore, the operator can execute a necessary process without disturbing other operators' operation by selecting an output device based on the operator's attribute.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic total overview indicating structure of the plant monitoring and controlling system 91 in accordance with the present invention.
FIG. 2 is an example of image manner displayed on a large display 1 .
FIG. 3 is an example of image manner displayed in a display at hand 10 .
FIG. 4 is an example of moving manner of a pointer between the display at hand 10 and the large display 1 .
FIG. 5 is an example of moving manner of a pointer between the display at hand 10 and the large display 1 .
FIG. 6 is an example of moving manner of a pointer between the display at hand 10 and the large display 1 .
FIG. 7 is an example of image manner at registering charged task.
FIG. 8 is a problem analysis diagram (PAD) indicating steps for registering charged task.
FIG. 9 is a drawing indicating a corresponding table of input device identification (ID) and registered charged task.
FIG. 10 is a drawing indicating a corresponding table of registered charged task and output device identification (ID).
FIG. 11 is an example of image manner displayed on the large display 1 and the displays at hand 10 , 30 .
FIG. 12 is an example of image manner displayed on the large display 1 .
FIG. 13 is an example of image manner displayed on the large display 1 .
FIG. 14 is an example of image manner displayed on the display at hand 10 .
FIG. 15 is an example of image manner displayed on the large display 1 and the display at hand 10 .
FIG. 16 is a drawing indicating a corresponding table of input events and executing process.
FIG. 17 is an example of a format for designating an output device.
FIG. 18 is a flow chart indicating a process flow at a pointing.
FIG. 19 is a drawing indicating a realizing method for pointing on the large display 1 and the display at hand.
FIG. 20 is a problem analysis diagram indicating a process flow of a method for realizing pointing on the display at hand 10 and the large display 1 .
FIG. 21 is an example of moving manner of a pointer between the display at hand 10 and the large display 1 .
FIG. 22 is a schematic drawing indicating an example of a system structure of the present invention.
FIG. 23 is a schematic drawing indicating another embodiment of the present invention.
DETAILED DESCRIPTION
Embodiments of the present invention are explained hereinafter with reference to the drawings.
FIG. 1 indicates a total structure of the plant monitoring and controlling system 91 which is one of the embodiments of the present invention. The numeral 1 indicates a large display whereon overview information on a whole plant (system diagram, main warnings, important control data, main monitoring video image, etc.) is displayed. The display on the large display 1 is performed by a workstation 2 . Each of the displays 10 , 30 , 50 is placed at hand of a respective operator who is engaged in operation of the plant. Hereinafter, the displays 10 , 30 , 50 are called in general as displays at hand. The operators grasp status of the whole plant by watching the overview information displayed on the large display 1 , examine detailed data using the individual display at hand if an abnormal symptom is found, and perform a setting operation, if necessary. The displays in the respective displays 10 , 30 , 50 are performed by workstations 11 , 31 , and 51 , respectively. Mice 12 , 32 , 52 , key boards 13 , 33 , 53 , and headsets 14 , 34 , 54 are connected to the workstations 11 , 31 , and 51 , respectively. Operators point a position in the displays at hand 10 , 30 , 50 and on the large display 1 using the mice, respectively. The headset is a headphone having a microphone. The operator hears sound output from the system and inputs sound signal to the system using the headset. Furthermore, the workstations 2 , 11 , 31 , 51 are mutually connected via a local area network 90 , and mutual information exchange is possible. To the local area network 90 , various computers for controlling, controllers for apparatus (not shown in the drawing) are connected directly or indirectly via other networks, the workstations 2 , 11 , 31 , 51 are accessible to various control information on the plant through the local area network 90 .
In FIG. 1 , three displays at hand 10 , 30 50 are illustrated. However, the number of the displays can be changed naturally depending on the number of the operators. Although FIG. 1 indicates one large display, a plurality of the large displays can also be used. The large display composed by joining a plurality of displays in a seamless manner may be used. Furthermore, providing a speaker and a microphone instead of the headphone to each of the operators may be acceptable.
A concept of the present invention is explained referring to FIG. 22 . In FIG. 22 , the workstation 200 and the workstation 250 are connected to the network 230 , and the two workstations can exchange information arbitrarily with each other. To the workstation 250 , other workstations having the same structure as the workstation 250 are connected (not shown in FIG. 22 ). The process executing part 201 of the workstation 200 outputs information to output apparatus of the other workstations connected to the network 230 as well as displaying information in the output apparatus 205 via the output processing part 202 .
To the workstation 250 , an attribute is registered at the start of the operation. The attribute registration processing part 257 displays a menu for the attribute registration in the output apparatus 256 via the input/output processing part 252 . When the menu is selected by the input apparatus 255 , the attribute registration processing part 257 registers the selected attribute to the attribute memory part 253 , and further, stores a corresponding relationship between the selected attribute and the output apparatus 256 to the attribute memory part 203 of the workstation 200 via the network 230 .
Input information from the input apparatus 255 is transmitted to the process executing part 251 via the input/output processing part 252 . The process executing part 251 executes a responding process and outputs results of the execution to the output apparatus 256 when the input information is such to a designate a position in a display of the output apparatus 256 . On the other hand, when the input information is such as designating a position in a display of the output apparatus 205 , the process executing part 251 transmits the input information with an attribute called out from the attribute memory part 253 to the process executing part 201 of the workstation 200 . The process executing part 201 executes a process corresponding to the transmitted input information and the attribute. The process executing part 201 transmits results of the execution to an output apparatus corresponding to the transmitted attribute which is called out from the attribute memory part 203 .
FIG. 2 illustrates an example of display manner on a large display 1 . On the large display 1 , overview information such as a system diagram 5 and warnings 4 on the plant is displayed. When an abnormal condition of the plant is detected, a warning 4 related to the abnormal condition blinks. Especially, when the abnormal condition is serious, warning sound alarms from the headsets 14 , 34 , 54 in addition to the blinking of the warnings 4 . The numeral 3 designates a display controlling menu for controlling the display on the large display 1 . By selecting the display controlling menu 3 , the large display can display various images such as (1) prior displayed objects, (2) subsequent display objects, (3) weather information, (4) monitoring video image, (5) various system diagrams, etc. Each of pointers 15 , 35 , 55 works with each of the mice respectively, and/or is colored with different colors so as to facilitate identification. The pointers 15 , 35 , 55 naturally may have shapes different from one another, or may be added with information on operator's attribute, such as name of work, or personal name, instead of color coding. The pointers 15 , 35 , 55 can be transferred continuously between the displays at hand 10 , 30 , 50 and the large display 1 , respectively. The transferring of the pointers will be explained in detail referring to FIGS. 4–6 later.
FIG. 3 illustrates an example of display manner on the display at hand 10 . Hereinafter, an embodiment is explained taking the display at hand 10 as an example, but the explanation can be applied to other displays at hand 30 , 50 if any exception is not mentioned especially. FIG. 3 indicates an example of detailed information on the plant displayed on the display at hand 10 . On the display at hand 10 , a plate hanger icon 17 and a person in charge icon 16 are displayed. The plate hanger icon 17 provides a function to put a memorandum by voice to the display at hand 10 and the large display 1 . The person in charge icon 16 provides a function to register charged task (operator, inspector, chief on duty, etc.) of an operator who uses input/output apparatus at hand, such as display at hand 10 , a mouse 12 , a keyboard 13 , and a headset 14 . On the person in charge icon 16 , the registered charged task, that means the charged task to the operator who uses the display 10 at the time, is displayed. In the case shown in FIG. 3 , “operator” is displayed on the icon 16 . It means an operator in charge of operation is registered.
Next, a method for transferring the pointer 15 between the large display 1 and the display at hand 10 is explained referring to FIGS. 4–6 . In the present embodiment, the pointer moves continuously from the display at hand to the large display 1 only by moving the mouse 12 forward as shown in FIG. 4 . That means, under a condition wherein the pointer located on the display at hand 10 , the pointer 15 moves toward upper portion of the display at hand 10 in accordance with moving the mouse 12 forward, and reaches finally at the uppermost point of the display at hand 10 . If moving the mouse 12 forward further, the pointer 15 transfers to the lowest point of the large display 1 , and the pointer 15 moves upward to the top of the large display in accordance with further moving the mouse 12 forward. On the contrary, if the mouse 12 is moved backward under a condition wherein the pointer 15 is displayed on the large display 1 , the pointer 15 moves downward to the lowest point of the large display 1 . If moving the mouse 12 backward further, the pointer 15 transfers to the uppermost point of the display at hand 10 . Display position of the pointer 15 at a moment when the pointer 15 transfers from the display at hand 10 to the large display 1 is decided as shown in FIG. 4 . That is, when putting x for a horizontal position of the pointer 15 at the moment of transferring from the display at hand 10 to the large display 1 , h for the number of pixels in a horizontal direction on the display at hand 10 , X for a horizontal position of the pointer 15 at the moment of entering into the large display 1 , and H for the number of pixels in a horizontal direction, the X is decided so as to be x:h=X:H. Similarly, when the pointer transfers from the large display 1 to the display at hand 10 , x is decided so as to be x:h=X:H.
When the large display is composed of a plurality of displays, the display position of the pointer 15 is decided in the same manner as explained referring to FIG. 4 taking an assumption that the plurality of displays are joined in a seamless manner. FIG. 5 illustrates a case when the large display is composed of two displays 6 , 7 . When putting d for width of each display of the two displays, X or x can be obtained by replacing X with (X 1 +d), and H with 2d.
Referring to FIG. 4 , a method for transferring the pointer 15 as if the top portion of the display at hand 10 joins the total span of the lower portion of the large display 10 has been explained. However, a method for transferring the pointer 15 as if the top portion of the display at hand 10 joins the partial span of the lower portion of the large display can also be useful. A range of the partial lower span of the large display to be joined to the display at hand 10 can be decided in consideration of a relative relationship of an arrangement between the large display 1 and the display at hand 10 . That means, when the display at hand 10 is arranged at left side to the large display 1 , X and H are substituted by (X−d 1 ) and (H−d 1 −d 2 ), respectively, so that the pointer 15 transfers within a ranged d 1 the at left side of the lower portion of the large display. Here, d 2 is a distance from the right side of the large display 1 to right side of the display at hand 10 when the right side of the display at hand 10 is arranged at the right side of the large display 1 . On the contrary, when the display at hand 10 is arranged at the right side of the large display 1 , the pointer 15 is arranged so as to transfer at a right side range of the bottom of the large display 1 .
The image size (the number of pixels) of the pointer 15 may be changed in the large display 1 from that in the display at hand 10 . Especially, when the display at hand 10 and the large display are installed far apart. Making the display size of the pointer 15 larger facilitates identification. For instance, the pointer 15 is displayed with pixels 16.times.16 on the display at hand 10 , and with pixels 36.times.36 in the large display 1 .
According to the above selection, the pointer becomes easily recognizable even in the far away large display.
Advantages of the above described method are as follows:
(1) a position on the display at hand 10 and the large display 1 can be designated continuously without changing grip of a pointing device;
(2) interactive operation of the large display can be performed with the same feeling as that of operation of the display at hand 10 ;
(3) depending on the above advantage (2), learning of operation is easy.
At the start of operation of a system in the present embodiment, an operator registers his own charged task to the system. The system provides service based on the registered charged task. The service includes, for example, arranging a suitable operation environment for the charged task, facilitating to retrieve information only necessary for the charged task, and setting a permission for operation for each of the charged task. Here, the operation environment means items in a menu, an order of its arrangement, setting of default, and setting a permission for operation, etc.
A method for registering the charged task is explained hereinafter with reference to FIGS. 7 and 8 . FIG. 7 is an example of image manner at registering charged task. FIG. 8 is a problem analysis diagram (PAD) indicating steps for registering charged task. When the charged task icon 16 on the display at hand 10 is indicated by the mouse 12 (step 100 ), the charged task selecting menu 18 is displayed on the display at hand 10 . Items in the charged task selecting menu are as follows:
Operation: Selected when a service for a person in charge of operation is desirable.
Inspection: Selected when a service for a person in charge of inspection is desirable.
Chief on duty: Selected when a service for a person in charge of chief on duty is desirable.
Supervisor: Selected when a service for a person responsible for all task is desirable. This item is selected, for example, at adjusting the system, or operating the system by only one person.
General: Selected for a service within a range of task which does not cause serious disturbance to the system even though erroneous operation is executed. This item is selected, for example, when the system is operated by a person who is not familiar with the system for on-job training.
When a desired item in the charged task selecting menu 18 is selected by the mouse 12 (step 101 ), a password input region 19 is displayed. When a password which is designated to each of the charged task is input (step 102 ), the charged task for the operator is registered to the system, and the registered charged task is displayed in the charged task icon 16 . When the charged task must be changed, the same procedure as that of the registering ( FIG. 8 ) is performed.
In the system of the present embodiment, a correspondence of the charged task for the operator and input/output devices used by the operator is controlled using tables shown in FIGS. 9 and 10 . In FIG. 9 , a table 120 indicating correspondence between input device IDs, such as mice 12 , 32 , 52 , keyboards 13 , 33 , 53 , and headsets 14 , 34 , 54 , and the charged task for the operator who uses the input devices is utilized for retrieving the charged task for the operator using the input devices with the input device IDs as keys.
In FIG. 10 , a table 121 indicating correspondence between the charged task for the operator and output device IDs, such as displays at hand 10 , 30 , 50 , and headsets 14 , 34 , 54 , used by the operator is utilized for retrieving the output devices used by the operator by using the charged task as keys.
Referring to FIG. 11 , an example of utilizing manner of the plant monitoring and controlling system 91 is explained hereinafter.
When an operator points out an image displayed on the large display 1 by a mouse at hand, detailed information related to the pointed image and necessary for the task charged to the operator is displayed in the operator's displays at hand 10 , 30 , 50 . FIG. 11 illustrates a status wherein the display at hand 10 is used by an operator in charge of operation, and the display at hand 30 is used by an operator in charge of inspection. When the operator in charge of operation points out a boiler in a system diagram displayed on the large display 1 by the mouse 12 , a display 20 for setting control data for the boiler is displayed on the display at hand 10 , and an operation procedure of the boiler becomes operable. On the other hand, when the operator in charge of inspection points out the boiler in the same system diagram displayed similarly on the large display 1 , monitoring video image of the boiler in the plant site is displayed on the display at hand 30 , and the condition of the boiler at the plant site can be inspected.
FIG. 11 shows an example of displaying information 22 in the displays at hand 10 , 30 , 50 responding to pointing on the large display 1 . However, the information can be output in sound. Even in a case when the information is output in sound, the information is output to only a person who needs the information. For instance, when the operator in charge of operation points out a display on the large display 1 by the mouse 12 at hand, the information related to the display is output to the headset 14 provided to the operator in charge of operation in sound. Furthermore, not only information, but also sound feed back to the operation on the large display 1 is output to only the operator. For instance, when a sound signal is fed back at every pointing, the feed back is output to only the headset 14 for the operator who has pointed, but not to the headsets for the other operators. That means, when the operator in charge of operation points a display on the large display 1 by the mouse 12 at hand, a sound signal is output to the headset 14 provided to the operator in charge of operation.
An error message to an erroneous operation on the large display 1 is also output to the display at hand 10 or the headset 14 only for the operator who has operated. Of course, the error message which must be referred to other operators is output to the other operators.
As explained above, information related to the displayed information on the large display 1 can be referred easily by pointing out the display by the mouse 12 at hand. And, the information is output only to the output device for the operator who has pointed out the display, and consequently, the operation does not distract other operators. The large display is used commonly with many operators. Therefore, if information necessary for only a specified operator is displayed on the large display 1 , it may hide information which has been watched by other operators. In a case when a sound is output, if the sound is output loudly so as to reach all operators, it may distract operators who do not need the information. Furthermore, by displaying only information selected so as to correspond to the charged task for the operator who has pointed out, the operator can easily access the information necessary for only himself without being distracted by information to other operators.
The large display 1 is used commonly by a plurality of operators who are in charge of different tasks. Because a suitable operation environment for performing each of the tasks differs, the plant monitoring and controlling system 91 provides an operation environment corresponding to the charged task for each of the operators who use the large display 1 for interactive operation.
FIG. 12 illustrates an example of changing an arranging order of the menu items corresponding to the charged task of the operator. The numeral 22 indicates a menu displayed when the operator in charge of operation must point out any one of symbols in the system diagram 5 displayed on the large display 1 by the mouse 12 . By selecting the menu 22 , any one of the information related to the pointed symbol such as data setting, monitoring video image, and inspection record, is displayed on the display at hand 10 . Here, the items in the menu 22 are arranged from the top to the bottom in an order based on frequency of selection by the operator in charge of operation. On the other hand, the menu 42 is displayed by pointing out any one of the symbols in the system diagram 5 by the inspector. The items in the menu 42 are the same as those of the menu 22 , but the items are arranged from the top to the bottom in an order based on frequency of selection by the inspector, that is, an order of monitoring video image, inspection record, and data setting.
FIG. 13 illustrates an example of changing operation permission based on the charged task. Permission to operate the display control icon 3 for controlling display contents on the large display 1 is given only to the chief on duty. When the chief on duty who has registered his charged task to the display at hand 10 points out the display control icon 3 by the mouse 12 at hand, the display control menu 6 is displayed. The chief on duty can change the contents of the display on the large display 1 by selecting the display control menu 6 . However, even if the operator in charge of operation, or the operator in charge of inspection points out items in the display control icon 3 and display control menu 6 , the pointing is neglected.
In the above description, a case when some information is output to the operator corresponding to the task of the operator is explained. However, there may be cases wherein information, such as warning, is output to the operator by the system voluntarily. Even in this case, the information is output only to the operator in charge of the task which needs the information. For example, warning sound to generate warning which can be treated only by the operator in charge of operation is output only to the headset 14 of the operator in charge of operation.
In a case when the large display 1 is too large to be within the operator's visual field, there may be a possibility that the operator fails to be aware of information which is displayed out of his visual field. To prevent such a case from occurring, a sound is output simultaneously with the display on the large display 1 so as to indicate the display position. The operator becomes aware of displaying new information by the sound without watching the large display 1 . Further, because the sound is output so as to indicate the display position, the operator can be aware of the approximate position of the displayed information. When the sound is output simultaneously with the display, the sound is output to only the operator in charge of the task which requires the displayed information. For instance, when information relating to operation is displayed, the sound is output to only the headset 14 for the operator in charge of operation.
Referring to FIGS. 14 and 15 , a plate hanger by voice is explained hereinafter. The plate hanger by voice, so called here, means a memorandum by voice hung over the display on the large display 1 or the displays at hand 10 , 30 , 50 . When pointing the plate hanger icon 17 by the mouse 12 as shown in FIG. 14 , the plate hanger menu 23 is displayed. By selecting an item, GENERATE, of the plate hanger menu 23 , the icon 24 is displayed on the display at hand 10 . Subsequently, by selecting an item, RECORD, of the plate hanger menu 23 , voice transmitted from a microphone of the headset 14 is recorded. By selecting an item, END, of the plate hanger menu 23 after finishing the input of the voice, the recording is stopped and the display of the plate hanger menu 23 is erased. The recorded voice can be regenerated by clicking the icon 24 by operating, for example, a right button of the mouse 12 . The voice is regenerated at the headset of the operator who has made the clicking. For instance, when the operator in charge of operation clicks the icon 24 by the mouse 12 at hand, the recorded voice is output to the headset 14 . On the other hand, when the operator in charge of inspection clicks the icon 24 by the mouse 32 at hand, the recorded voice is regenerated at the headset 34 .
The icon 24 can be placed at an arbitrary position of the display at hand 10 and the large display 1 by dragging. The dragging of the icon 24 can be performed by moving the pointer 15 on the icon 24 and subsequent moving of the mouse 12 with pushing, for example, a left button of the mouse 12 . FIG. 15 illustrates a moving manner of the icon 24 to the boiler in the system diagram 5 on the large display 1 by dragging.
Referring to FIGS. 16–20 , a method for realizing the system 19 is explained.
A program for realizing the system 19 can be composed so as to be executed in any one of the workstations 2 , 11 , 31 , 51 , or in any several or all of the workstations 2 , 11 , 31 , 51 .
In a corresponding table 130 of events/executing process which is controlled per every display object shown in FIG. 16 , the event can be divided into three categories, such as kind of operation, button number, and person in charge. The kind of operation includes the following items, and designates a kind of event.
(1) Button push down: Kinds of events generated by pushing down a mouse button.
(2) Button release: Kinds of events generated by releasing a mouse button.
(3) Key push down: Kinds of events generated by pushing down a key in the keyboard.
(4) Key release: Kinds of events generated by releasing a key in the keyboard.
The button number designates the button or the key which has generated the event. The person in charge designates charged task of the operator who has generated the event.
The executing process can be divided into two categories such as routine and output. The routine stores a process to be executed when an event is generated, and output designates an output apparatus which is used by the operator who must receive the output. The above designation of the operator is performed by designating a kind of task charged to the operator. That means, when an operator in charge of operation is designated as a destination of an output, the output is transferred to the output apparatus which is used by the operator in charge of operation.
FIG. 17 illustrates a format 131 for designating an output destination. Each of the bits in the format 131 corresponds to a respective charged task. A bit corresponding to a person in charge to receive the output is designated as “1”, and a bit corresponding to a person in charge not to receive the output is designated as “0”. For example, when an output must be transmitted to both, an operator and an inspector, the second bit and the third bit in the format 131 are designated as “1”, and other bits are “0”.
Referring to FIG. 18 , a process flow when a displayed object on the large display 1 is pointed is explained hereinafter.
In the event of input step 140 , input event cues of the workstations 11 , 31 , 51 are examined. If the event is stored in the input event queue, the event is taken out. The event includes information such as an input device ID which generates the event, a button number which generates the event, and a location where the event is generated. In the step 141 , a table 120 ( FIG. 9 ) is searched using the input device ID of the taken out event as a key to retrieve charged task of the operator who has generated the event. In the step 142 , a displayed object in the location where the event is generated is searched based on the event generated location.
If no displayed object exists at the event generated location (step 143 ), the operation returns to the step 140 and continues to process the next input event. If any displayed object exists at the event generated location (step 143 ), the operation goes to step 144 . In step 144 , the input event items in the corresponding table 130 of the event/executing process for the displayed object which is searched in step 142 is examined whether any input items are matched with kind of operation, button number, and person in charge of the input event. If there are any event items matched with the input event (step 145 ), an output destination of corresponding executing process items is taken out, the table 121 ( FIG. 10 ) is searched using the charged task stored in the output destination as a key, an output device ID is taken out, and the output device is set as for an output destination at routine execution (step 146 ). Subsequently, the routine stored in the routine items in the executing process items is executed (step 147 ).
When no event item matching to the input event is found in step 144 (step 145 ), the operation returns to the step 142 , and other object at the event generated location is searched. The above described processing is repeated until the plant monitoring and controlling system 91 is ended (step 148 ).
Referring to FIGS. 19 , 20 , a method for realizing the pointing by the mouse 12 on the display at hand 10 and the large display 1 is explained hereinafter.
The explanation is performed taking the display at hand 10 as an example, but cases of the other displays at hand 30 , 50 are entirely the same. In FIG. 19 , H is the number of pixels in a horizontal direction of the large display 1 , V is the number of pixels in a vertical direction, h is the number of pixels in a horizontal direction of the display at hand 10 , v is the number of pixels in a vertical direction: q is one pixel or a several pixels.
The coordinate values renewed in the workstation 11 corresponding to input by the mouse 12 are expressed as (curx, cury). When the mouse 12 is moved, an amount of moving (dx, dy) is reported to the workstation 11 , and the (curx, cury) is renewed by the following equation;
( curx, cury )=( curx, cury )+( dx, dy ) (1)
where,
0.1 toreq.curx<h, 0.1 toreq.cury. 1 toreq.v (2)
That means, if a result of the renewal exceeds the region defined by the equation (2), the (curx, cury) is set as a value at a boundary. For example, −2 for cury is obtained by executing the equation (1), cury is set as 0. Origin of the coordinate on the large display 1 and the display at hand 10 is assumed to be located at top-left.
Referring to FIG. 20 , a process flow of a method for realizing pointing by the mouse 12 on the display at hand 10 and the large display 1 is explained hereinafter. At the start of the processing, an initial setting is q<cury<v, and the pointer is displayed at a position (curx, cury) on the display at hand 10 (step 162 ). As far as cury>q (step 160 ), when any event, such as pressing a button of the mouse 12 occurs, the event processing is executed to the displayed object on the display at hand 10 (step 163 ). When the mouse 12 is moved forward and cury becomes less than q, that is cury<q, the pointer transfers on the large display 1 . That means, a value of cury is set as hV/H (step 164 ), and the pointer is displayed (step 167 ) at a position (curx, cury)=(HcurX/h, Hcury/h−1) (step 166 ). As far as cury<hV/H (step 165 ), when any event, such as pressing a button of the mouse 12 , occurs, the event processing is executed to the displayed object on the large display 1 (step 168 ).
In the above embodiment, the charged task for the operator is registered first. And, by controlling the corresponding relationship between the registered charged task and input/output device, information corresponding to the charged task is displayed and operation environment is set. However, any attribute of the operator other than the charged task can be usable. For instance, name, age, order, class, rank, sex, mother language, skillfulness can be used registration for the control. Further, not only one attribute, a several attributes connected by logical equations can be used for the registration. In accordance with the above variation, the service can be provided with contents matched with various attribute of the operator.
Further, in the above embodiment, a method to register the attribute of the operator by selecting the menu is used. However, the attribute of the operator may be recognized by the plant monitoring and controlling system 91 itself. For instance, the operator sitting in front of the display 10 may be recognized by the operator's face, or by the operator's voiceprint input from a microphone.
Furthermore, in the above embodiment, the attribute of the operator is registered at the beginning of the operation. However, the attribute of the operator may be asked (a menu for selecting the attribute is displayed), or a processing for recognizing the attribute may start, at a moment when the system needs to know the attribute of the operator.
In the above embodiment, a mouse is used for pointing on the large display 1 , but a laser beam pointer can also be used. A pointing position on the large display 1 is determined by taking video with a video camera in front or back of the large display screen and processing the video image for determining position of the laser beam. Recognition of the device ID when a plurality of laser pointers are used is performed by using the laser pointers each having a laser beam of different color, and determining the color of the laser beam. Similarly, infrared pointers can be used. In this case, devices can be recognized by using different frequencies of infrared each other.
In the above embodiment, the pointer 15 moves between the display at hand 10 and the large display 1 as if the upper side of the display at hand 10 and a whole or a part of the lower side of the large display 1 were connected. However, as shown in FIG. 21 , the pointer 15 may be arranged so as to move from lateral side (left side or right side) of the display at hand 10 . Further, the moving manner of the pointer 15 between the display at hand 10 and the large display 1 may be set depending upon relative positions of the large display 1 and the display at hand 10 . Therefore, the operator can operates as if the large display 1 were located on an extended line of the display at hand 10 , and natural interface for the operator can be realized.
In the above embodiment, a conventional display apparatus is used as for the display at hand 10 . However, a see-through display apparatus can be used as for the display at hand 10 . The see-through display is a translucent display, and information displayed on it is visible with a background of the display in a superimposed manner. As one of example of such see-through display apparatus, there is a see-through head-mounted display described in a reference, Proceedings Of The ACM Symposium on User Interface Software And Technology, November, (1991) ACM Press pp. 9–17.
Referring to FIG. 23 , the second embodiment using the see-through display of the present invention is explained hereinafter. In FIG. 23 , it is assumed that an operator A uses a see-through display 1100 and another operator B uses a see-through display 1200 . On the large display 1000 , only information which is shared with the operator A and B is displayed. On the contrary, information necessary for only the operator A is displayed on the see-through display 1100 , and other information necessary for only the operator B is displayed on the see-through display 1200 . For instance, a pointer 1110 which is moved by operating a mouse at hand of the operator A is displayed on the see-through display 1100 , and a pointer 1210 which is moved by operating a mouse at hand of the operator B is displayed on the see-through display 1200 . Further, a menu 1120 which is displayed when the operator A presses a button of the mouse is displayed on the see-through display 1100 . The pointer, the menu, detailed information and others which are displayed on the see-through display are visible with displayed object on the large display in a superimposed manner. That means, the displayed object on the see-through display looks for the operator as if it were displayed on the large display. The operator can point the displayed object on the large display arbitrarily by the pointer displayed on the see-through display.
Naturally, a relationship between display coordinates of the see-through displays 1100 , 1200 and of the large display 1000 is maintained constant. That means, in such a case as mounting a see-through display at the overhead of the operator, a 3D tracking system is used for tracking the position and orientation of the see-through display, and the display coordinates of the see-through display are corrected in connection with a relationship with a relative position of the large display 1000 .
Furthermore, a see-through display and a conventional display can be used together as for displays at hand. That means, information which is desired to be displayed in a superimposed manner with information displayed on the large display 1000 such as a pointer for designating a position on the large display 1000 , and a menu for operating a displayed object on the large display 1000 , are displayed on the see-through display, and other information which is not required to be seen in a superimposed manner with the displayed object on the large display 1000 may be displayed on the conventional display.
Advantages of using the see-through display for a display at hand are as follows:
(1) Interference between operators can be completely eliminated. Although displaying a pointer or a menu directly on the large display distracts other operators, displaying the pointer or the menu on an operator's own display at hand does not interfere with to other operators' work because the display on his own see-through display is not visible to other operators. For instance, when many pointers are displayed on the large display simultaneously, it becomes difficult to identify one specified operator's own pointer among many pointers, and it causes a problem to be solved. However, if a pointer for each operator is displayed only on his own see-through display, the above problem can be eliminated because each operator sees only his own pointer at any time.
(2) Information displayed on the display at hand and information displayed on the large display can be integrated visually. When a conventional display is used as the display at hand, it is necessary to move a line of sight in order to refer both the information displayed on the large display and the information displayed on the display at hand, and it is difficult to see both of the above information simultaneously. On the contrary, information displayed on the see-through display is visible with information displayed on the large display in a superimposed manner, and both of the above information can be referred to simultaneously. Furthermore, related information can be displayed next to each other.
In accordance with the present invention, the following advantage is achieved:
(1) A process matching with an operator who has operated can be executed. An attribute of the operator is registered corresponding to an input means which is used by the operator, and when the operator operates the input means, a process matching with the operator who has operated can be executed by examining the registered attribute of the operator and selecting a matched process with the attribute of the operator for executing.
(2) An output destination can be selected corresponding to the operator who has operated so as not to distract other operators' task. An attribute of the operator is registered corresponding to an input means which is used by the operator, and when the operator operates the input means, a result can be output without distracting other operators by examining the registered attribute of the operator and selecting an output destination of the result of the processing matched with the attribute of the operator.
(3) An operating environment can be set matching with the operator. An attribute of the operator is registered corresponding to an input means which is used by the operator, and when the operator operates the input means, an operating environment matching with the operator who has operated can be provided by examining the registered attribute of the operator and setting the matched operating environment with the attribute of the operator. | An interactive computer system with plural displays includes a first computer, having an input device and an output including a display and a second computer having an output including display coupled to the first computer.
A voice recorder is provided to create an icon representing a recorded voice, and the icon is displayed on the display of the first computer. The input device of the first computer, which may be a mouse, is adapted to drag the icon from the display of the first computer to the display of the second computer, and to reproduce the recorded voice in response to a pointer displayed on the displays and controlled by the input device. | 8 |
CROSS-REFERENCE TO RELATED APPLICATION:
[0001] This application claims benefit of Provisional Application 60/791,805 filed Apr. 13, 2006.
[0002] This application claims benefit of Provisional Application 60/791,805 filed Apr. 13, 2006.
BACKGROUND OF THE INVENTION
[0003] 1. Field of the Invention
[0004] This invention relates to lubricating oil compositions suitable for use in internal combustion engines. More particularly, this invention relates to a low sulfur, ash and phosphorous lubricating oil composition containing is additives.
[0005] 2. Background
[0006] Many means have been employed to reduce overall wear and friction as well as to control oxidation/cleanliness in modern engines, particularly automobile engines. The primary methods include prolonging engine life by reducing engine wear and increasing the resistance to oxidation by reducing the engine's sludge/deposit build-up through degradation. Some of the solutions to reducing wear have been primarily mechanical including building engines with wear resistant alloy or ceramic parts, modifying the contact geometry and adding special coating materials. Other solutions to improve cleanliness also involve modifications to the oil, including the use of metal containing detergents. Recently, considerable work has also been done with lubricating oils to enhance their anti-wear/anti-oxidation properties by modifying them with ashless antioxidants and anti-wear components.
[0007] Contemporary lubricants such as engine oils use mixtures of additive components to achieve numerous performance benefits. Examples of additives components include, anti-wear and extreme pressure components, fuel economy improving components, friction reducers, dispersants, detergents, corrosion inhibitors and viscosity index improving additive.
[0008] These additives provide energy conservation, engine cleanliness and durability and high performance levels to the lubricating oil under a wide range of engine operating conditions including temperature, pressure and lubricant service life.
[0009] Throughout the world, legislation aimed at reducing automotive emissions is forcing down the level of sulfur in fuels. Recently, lubricants are coming under scrutiny as a source of air pollution and emission catalyst deactivation. Phosphorus is known to be poisonous to automotive three-way HC conversion catalysts.
[0010] Conventional engine oil technology relies heavily on zinc (dialkyl) dithiophosphate (“ZnDTP” or “ZDDP”). ZnDTP is a versatile, anti-wear/anti-oxidant component that provides extremely low cam and lifter wear and favorable oxidation protection under severe conditions. ZnDTPs are disadvantageous, especially at high treat rates because they contain the three disfavorable elements of Zn, S, P and no reduction in phosphorus and zinc levels can be realized until new additive technology permits replacing or eliminating zinc dithiophosphates. Sulfur is known to be poisonous to deNox catalysts and zinc phosphates cause plugging of the exhaust particulate filters. The sulfur, ash and phosphorous components in oil are commonly referred to as “SAP” or “SAPS” in the art.
[0011] The major problem with ZnDTP is the poisoning effects to after-treatment devices that may aggravate emission problems. In addition, ZnDTP has strong interactions with dispersants, detergents, other anti-wear components and moly dithiocarbamates causing antagonistic effects on friction, sludge and deposit, if inappropriate concentrations are utilized. Replacing ZnDTP additives is not a simple endeavor because the wear protection demand for today's engine is extremely high and extremely rigorous chemical limits on any reductions in ZnDTP treat levels.
[0012] Engine lubricating oils are often used in high temperature applications, where extreme temperatures can significantly reduce the useful life of the lubricant. Under high temperatures, the lubricant can become oxidized prematurely unless a strong antioxidant system can also be employed in the oil to prevent this degradation process. Good piston, ring, cam and lifter wear protection are also an important characteristic of today's engine oil. Additionally, many engine oils are often required to perform well in the presence of water, therefore, protecting against rust formation. Traditionally, ZnDTPs are used to provide adequate protection as described above. Engine designers are now requiring even greater anti-wear protection and more demanding test protocols are being put in place to insure that lubricants can meet these more stringent specifications. However, stringent regulations in emission control have forced lubricant formulators to move away from ZnDTPs for the reasons discussed above.
[0013] Accordingly, there is a need for an additive or additive system for engine oils that has the ability to improve both rust and wear protection, and at the same time significantly enhance oxidative stability, while meeting stringent emission requirements. This invention satisfies that need.
SUMMARY OF THE INVENTION
[0014] In a first embodiment, a lubricating oil composition is disclosed. This composition, comprises a lubricating oil basestock, an organic silane containing additive present in the amount of at least 0.1 and less than 2.0 weight percent of the composition, a dispersant-detergent-inhibitor system of less than 15 weight percent of the composition, an organic boron additive present in the amount of at least 0.1 and less than 8.0 weight percent of the composition, a zinc dithiophosphate additive present in the amount of at least 0.1 weight percent of the composition and less than 1.6 weight percent of the composition. The final formulation of the composition has at least 80 PPM and less than 1600 PPM silicon, at least 100 PPM and less than 630 PPM phosphorus, at least 10 5 PPM and less than 710 PPM zinc, at least 1,000 PPM and less than 4,000 PPM sulfur, at least 800 PPM, less than 10,000 PPM ash and at least 80 PPM and less than 450 PPM Boron.
[0015] In a second embodiment, an additive composition for lubricating oils is disclosed. This composition comprises an organic silane containing additive present in the amount of at least 0.4 and less than 8.0 weight percent of the additive a dispersant-detergent-inhibitor system of less than 60 weight percent of the additive, an organic boron additive present in the amount of at least 0.4 and less than 32.0 weight percent of the additive, a zinc dithiophosphate additive present in the amount of at least 0.4 weight percent of the additive and less than 6.4 weight percent of the additive. The final formulation of the composition has at least 80 PPM and less than 1600 PPM silicon, at least 100 PPM and less than 630 PPM phosphorus, at least 105 PPM and less than 710 PPM zinc, at least 1,000 PPM and less than 4,000 PPM sulfur, at least 800 PPM, less than 10,000 PPM ash and less than 450 PPM Boron.
[0016] In a third embodiment, a method of obtain a favorable lubricating properties is disclosed. This method, comprises obtaining a composition comprising a lubricating oil basestock, an organic silane containing additive present in the amount of at least 0.1 and less than 2.0 weight percent of the composition, a dispersant-detergent-inhibitor system of less than 15 weight percent of the composition, an organic boron additive present in the amount of at least 0.1 and less than 8.0 weight percent of the composition, a zinc dithiophosphate additive present in the amount of at least 0.1 weight percent of the composition and less than 1.6 weight percent of the composition. The final formulation of the composition has at least 80 PPM and less than 1600 PPM silicon, at least 100 PPM and less than 630 PPM phosphorus, at least 105 PPM and less than 710 PPM zinc, at least 10,000 PPM and less than 4,000 PPM sulfur, at least 800 PPM, less than 1,000 PPM ash and less than 450 PPM Boron and lubricating an engine with the composition.
DETAILED DESCRIPTION OF THE INVENTION
[0017] This invention relates to engine lubricants formulated with unique functional fluids and/or additives to achieve performance improvements. One embodiment is a low SAP engine lubricant composition comprising combinations of borates, high levels of ashless antioxidants, and low levels of ZnDTP to achieve high level of performance equal to or better than using high level of ZnDTP alone. In one embodiment, the component synergy is built upon a variety of functionalities to achieve well balanced performance features. In a preferred embodiment, these performance features favorably exceed engine oils formulated with high levels of zinc dithiophosphates and metallic detergents.
[0018] In a second embodiment, the lubricating oils maintain low frictional properties of film under various operating conditions. This embodiment favorably maintains sufficiently high film thickness at high operating temperatures to provide a minimum lubricant film to protect against wear at a variety of temperatures.
[0019] In a third embodiment, the lubricating oil maintains cleanliness over the entire range of operating conditions while reducing wear to an absolute minimum. In a fourth embodiment, the lubricating oil provides favorable oxidation, deposit and corrosion control, under the most severe operating conditions.
[0020] It has been discovered that organic silanes when blended with high levels of organic borates, and low levels of zinc dithiophosphates provide substantial property benefits. U.S. Pat. No. 6,887,835 discloses suitable silanes including organic silane additives for lubricants. U.S. Pat. No. 6,887,835 is incorporated by reference herein.
[0021] In a preferred embodiment, high levels of ashlees antioxidants are added to the compounds to achieve even more favorable property benefits. An even more preferred embodiment combines the synergistic benefits of low levels of non-corrosive sulfur, organic silanes, high levels of organic borates with ashless antioxidants and low levels of ZnDTP. These benefits include but are not limited to reductions in wear, corrosion, and increases in oil induction temperature or time (OIT) during oxidative conditions that result in potentially significant improvements in engine service life and durability with excellent overall performance benefits. In an additional embodiment, these benefits can be achieved without deleterious effects such as instability, undesirable high viscosity, deposits and the like, when added to lubricating oils.
[0022] This new engine oil technology is based on an advanced anti-wear, anti-friction and antioxidant system, suitable for combination with typical, contemporary dispersants, ashless antioxidants, detergents, defoamants and others including contemporary DI additive packages. These additives enhance anti-wear, anti-oxidation and anti-corrosion performance.
[0023] Persons skilled in the art with the benefit of the disclosure herein will recognize the ability to include additives that favorably enhances lubricant performance including anti-friction, anti-oxidation and anti-wear performance while successfully meeting the stringent wear, oxidation and cleanliness performance requirements in modern engines. Examples of suitable additives include but are not limited to contemporary ZDDP in low levels, borated or non-borated dispersants, phenolic and aminic ashless anti-oxidants, high and low levels of metal detergents, molybdenum or organic friction modifiers, defoamants, seal swell additives, pour point depressants including contemporary DDI additive packages, and any combination thereof.
[0024] Suitable dispersants include borated and non-borated succinimides, succinic acid-esters and amides, alkylphenol-polyamine coupled Mannich adducts, other related components and any combination thereof. In some embodiments, it can often be advantageous to use mixtures of such above described dispersants and other related dispersants. Examples include additives that are borated, those that are primarily of higher molecular weight, those that consist of primarily mono-succinimide, bis-succinimide, or mixtures of above, those made with different amines, those that are end-capped, dispersants wherein the back-bone is derived from polymerization of branched olefins such as polyisobutylene or from polymers such as other polyolefins other than polyisobutylene, such as ethylene, propylene, butene, similar dispersants and any combination thereof. The averaged molecular weight of the hydrocarbon backbone of most dispersants, including polyisobutylene, is in the range from 1000 to 6000, preferably from 1500 to 3000 and most preferably around 2200.
[0025] The preferred organic borates are borated hydroxyl esters, such as borated glycerol mono-oleate (GMO), borated glycerol di-oleate (GDO), borated glycerol tri-oleate (GTO), borated glycerol mono-cocoate (GMC), borated mono-talloate (GMT), borated glycerol mono-sorbitate (GMS), borated polyol esters with pendant hydroxyl groups, such as borated pentaerythritol di-C8 ester, and any combination thereof. Short chain tri-hydroxyl orthoborates may be used but are not desirable due to their relatively poor thermal/oxidative stability properties when compared to borated hydroxyl esters. Borated dispersants and borated detergents can be used as a source of boron. However, in order to achieve best overall performance, specific organic borates, such as borated hydroxyl esters are more preferable.
[0026] Suitable detergents include but are not limited to calcium phenates, calcium sulfonates, calcium salicylates, magnesium phenates, magnesium sulfonates, magnesium salicylates, metal carbonates, related components including borated detergents, and any combination thereof. The detergents can be neutral, mildly overbased, or highly overbased. The amount of detergents usually contributes a total base number (TBN) in a range from 1 to 9 for the formulated lubricant composition. Metal detergents have been chosen from alkali or alkaline earth calcium or magnesium phenates, sulfonates, salicylates, carbonates and similar components.
[0027] Antioxidants have been chosen from hindered phenols, arylamines, dihydroquinolines, phosphates, thiol/thiolester/disulfide/trisulfide, low sulfur peroxide decomposers and other related components. These additives are rich in sulfur, phosphorus and/or ash content as they form strong chemical films to the metal surfaces and thus need to be used in limited amount to reduce sulfur, ash and phosphorous.
[0028] Inhibitors and antirust additives may be used as needed. Seal swell control components and defoamants may be used with the mixtures of this invention. Various friction modifiers may also be utilized. Examples include but are not limited to amines, alcohols, esters, diols, triols, polyols, fatty amides, various molybdenum phosphorodithioates (MoDTP), molybdenum dithiocarbamates (MoDTC), sulfur/phosphorus free organic molybdenum components, molybdenum trinuclear components, and any combination thereof.
[0029] The preferred non-corrosive sulfur compounds are chosen from the group consisting of ashless derivatives of thiadiazoles, ashless derivatives of benzothiazoles, ashless alkyl or aryl sulfides/di-sulfides/tri-sulfide including thianthrene, and its alkylates, diphenyl sulfide and disulfide, and their alkylates, dinonyl sulfide or disulfide, dipyridyl sulfide or disulfide, and their alkylates, ashless dithiocarbamates, and thioesters/sulfurized esters including thioglycolates, dialkyl thiodipropionates, dialkyl dithiopropionates. Examples of ashless thiadiazoles are Vanlube 87™, Cuvan 826™ and Cuvan 484™. Examples of ashless dithiocarbamates are Vanlube 7723™ and Vanlube 981. A prerequisite to the selection of sulfur additives is that they all need to meet copper corrosion requirements according to ASTM (D130) and low temperature storage compatibility tests.
[0030] The anti-corrosion performance can be judged by the copper corrosion test ASTDM D130 under normal conditions. For ASTDM test D130-6 normal conditions are 250 degrees Fahrenheit at 3 hours. For ASTDM test D130-8, normal conditions are 210 degrees Fahrenheit for 6 hours with 1 percent water, as well as a more severe condition at 250 degrees Fahrenheit for 24 hours. For purposes of this invention, non-corrosive sulfur shall be defined as any sulfur that provides a performance classification of 2B or better under the ASTM D-130 Copper Corrosion Test.
[0031] For example, dibenzyl disulfide was found to have deficiency in a severe copper corrosion test at degrees Fahrenheit for 24 hours and 2,2′-dipyridyl disulfide has poor low temperature compatibility in engine oils. Therefore, both these additives are deemed less favorable, despite their strong EP performance.
[0032] Sulfur additives containing a small portion of polysulfides (tri-sulfide/tetra-sulfide and higher order of polysulfides) are still acceptable providing that they could meet the copper corrosion requirements. The preferred ashless antioxidants are hindered phenols and arylamines. Typical examples are butylated/octylated/styrenated/nonylated/dodecylated diphenylamines, 4,4′-methylene bis-(2,6-di-tert-butylphenol), 2,6-di-tert-butyl-p-cresol, octylated phenyl-alpha-naphthylamine, alkyl ester of 3,5-di-tert-butyl-4-hydroxy-phenyl propionic acid, and many others. Sulfur-containing antioxidants, such as sulfur linked hindered phenols and thiol esters can also be used.
[0033] In a preferred embodiment, this new synergistic combination of lubricant base stocks and additives provide favorable performance parameters while maintaining excellent compatibility to exhaust after-treatment devices. This embodiment comprises a novel anti-wear, friction reduction and antioxidant system consisting of multi-functional, organic silane additives, organic borates, high level of ashless antioxidants and low level of zinc dithiophosphates. More specifically, this formulated engine oil embodiment comprises about 80 to 1600 PPM silicon, about 100 to 630 PPM phosphorus, and about 0.1 to 0.3 weight percent sulfur, less than 1 weight percent ash and from about 80 to 450 PPM boron, and about 0.5 to 3.0 wt % ashless antioxidants such as total amounts of hindered phenols and arylamines.
[0034] In one example embodiment, the general formulation of the low SAP engine oil containing the organic silanes is summarized in Table 1. In this table and throughout the application weight percent is intended to be active weight percent of the entire composition unless otherwise stated.
[0000]
TABLE 1
Elements in Formulated Oils
Component Type
Wt %
(ppm) + Other Restrictions
Organic boron additive
0.1–8.0%
80 to 450 PPM boron
Zinc dithiophosphate
0.1–1.0%
100 to 630 PPM phosphorous and
additive
105 to 710 PPM zinc
Dispersant-detergent-
<15.0%
inhibitor system
Organic Silane additive
0.1–2.0%
80 to 1600 PPM silicon
Ashless antioxidants
0.5–3.0%
[0035] These components can be used with a variety of base stocks, including group I, II, III, IV, and V, and gas-to-liquids (“GTL”) as well as a variety of mixtures thereof. However, due to other performance requirements including volatility, stability, viscometrics, and cleanliness feature, premium engine oils preferably utilize group II and higher (“Group II+”) base oils to ensure that they can achieve desirable overall performance levels as well as maximizing the full potential of the unique synergies among additives. Additional significant synergies were identified among alkylated aromatics and Group II+ high performance base stocks including Group II, III, IV, V, VI or GTL base stocks.
[0036] Groups I, II, III, IV and V are broad categories of base oil stocks developed and defined by the American Petroleum Institute (API Publication 1509; www.API.org) to create guidelines for lubricant base oils. Group I base stocks generally have a viscosity index of a range about 80 to 120 and contain greater than about 0.03% sulfur and/or less than about 90% saturates. Group II base stocks generally have a viscosity index of between about 80 to 120, and contain less than or equal to about 0.03% sulfur and greater than or equal to about 90% saturates. Group III stock generally has a viscosity index greater than about 120 and contains less than or equal to about 0.03 % sulfur and greater than about 90% saturates. Group IV includes polyalphaolefins (PAO). Group V base stocks include base stocks not included in Groups I-IV. Table 2 summarizes properties of each of these five groups.
[0000]
TABLE 2
Base Stock Properties
Saturates
Sulfur
Viscosity Index
Group I
<90% and/or
>0.03% and
≧80 and <120
Group II
≧90% and
≦0.03% and
≧80 and <120
Group III
≧90% and
≦0.03% and
≧120
Group IV
Polyalphaolefins (PAO)
Group V
All other base oil stocks not included in
Groups I, II, III, or IV
[0037] Base stocks having a high paraffinic/naphthenic and saturation nature less than 90 weight percent can often be used advantageously in certain embodiments. Such base stocks include Group II and/or Group III hydroprocessed or hydrocracked base stocks, or their synthetic counterparts such as polyalphaolefin oils, GTL or similar base oils or mixtures of similar base oils.
[0038] In a preferred embodiment, at least about 20% of the total composition should consist of such Group II or Group III base stocks or GTL, with at least about 30% being preferable, and more than about 80% on being most preferable. Gas to liquid base stocks can also be preferentially used with the components of this invention as a portion or all of the base stocks used to formulate the finished lubricant. We have discovered, favorable improvement when the components of this invention are added to lubricating systems comprising primarily Group II, Group III and/or GTL base stocks compared to lesser quantities of alternate fluids.
[0039] GTL materials are materials that are derived via one or more synthesis, combination, transformation, rearrangement, and/or degradation/deconstructive processes from gaseous carbon-containing compounds, hydrogen-containing compounds, and/or elements as feedstocks such as hydrogen, carbon dioxide, carbon monoxide, water, methane, ethane, ethylene, acetylene, propane, propylene, propyne, butane, butylenes, and butynes. GTL base stocks and base oils are GTL materials of lubricating viscosity that are generally derived from hydrocarbons, for example waxy synthesized hydrocarbons, that are themselves derived from simpler gaseous carbon-containing compounds, hydrogen-containing compounds and/or elements as feedstocks. GTL base stock(s) include oils boiling in the lube oil boiling range separated/fractionated from GTL materials such as by, for example, distillation or thermal diffusion, and subsequently subjected to well-known catalytic or solvent dewaxing processes to produce lube oils of reduced/low pour point; wax isomerates, comprising, for example, hydroisomerized or isodewaxed synthesized hydrocarbons; hydroisomerized or isodewaxed Fischer-Tropsch (“F-T”) material (i.e., hydrocarbons, waxy hydrocarbons, waxes and possible analogous oxygenates); preferably hydroisomerized or isodewaxed F-T hydrocarbons or hydroisomerized or isodewaxed F-T waxes, hydro-isomerized or isodewaxed synthesized waxes, or mixtures thereof.
[0040] GTL base stock(s) derived from GTL materials, especially, hydroisomerized/isodewaxed F-T material derived base stock(s). These base stocks are hydroisomerized/isodewaxed wax derived base stock(s) are characterized typically as having kinematic viscosities at 100° C. of from about 2 mm 2 /s to about 50 mm 2 /s, preferably from about 3 mm 2 /s to about 50 mm 2 /s, more preferably from about 3.5 mm 2 /s to about 30 mm 2 /s. For example, a GTL base stock derived by the isodewaxing of F-T wax, has a is kinematic viscosity of about 4 mm 2 /s at 100° C. and a viscosity index of about 130 or greater. The term GTL base oil/base stock and/or wax isomerate base oil/base stock as used herein and in the claims is to be understood as embracing individual fractions of GTL base stock/base oil or wax isomerate base stock/base oil as recovered in the production process. Other examples, include mixtures of two or more GTL base stocks/base oil fractions and/or wax isomerate base stocks/base oil fractions, as well as mixtures of one or two or more low viscosity GTL base stock(s)/base oil fraction(s) and/or wax isomerate base stock(s)/base oil fraction(s) with one, two or more high viscosity GTL base stock(s)/base oil fraction(s) and/or wax isomerate base stock(s)/base oil fraction(s) to produce a dumbbell blend wherein the blend exhibits a viscosity within the aforesaid recited range. Reference herein to Kinematic viscosity refers to a measurement made by ASTM method D445.
[0041] GTL base stocks and base oils derived from GTL materials, especially hydroisomerized/isodewaxed F-T material derived base stock(s), and other hydroisomerized/isodewaxed wax-derived base stock(s), such as wax hydroisomerates/isodewaxates, which can be used as base stock components of this invention are further characterized typically as having pour points of about −5° C. or lower, preferably about −10° C. or lower, more preferably about −15° C. or lower, still more preferably about −20° C. or lower, and under some conditions may have advantageous pour points of about −25° C. or lower, with useful pour points of about −30° C. to about −40° C. or lower. If necessary, a separate dewaxing step may be practiced to achieve the desired pour point. References herein to pour point refer to measurement made by ASTM D97 and similar automated versions.
[0042] The GTL base stock(s) derived from GTL materials, especially hydroisomerized/isodewaxed F-T material derived base stock(s), and other hydroisomerized/isodewaxed wax-derived base stock(s) which are base stock components which can be used in this invention are also characterized typically as having viscosity indices of 80 or greater, preferably 100 or greater, and more preferably 120 or greater. Additionally, in certain particular instances, viscosity index of these base stocks may be preferably 130 or greater, more preferably 135 or greater, and even more preferably 140 or greater. For example, GTL base stock(s) that derive from GTL materials preferably F-T materials especially F-T wax generally have a viscosity index of 130 or greater. References herein to viscosity index refer to ASTM method D2270.
[0043] In addition, the GTL base stock(s) are typically highly paraffinic (>90% saturates), and may contain mixtures of monocycloparaffins and multicycloparaffins in combination with non-cyclic isoparaffins. The ratio of the naphthenic (i.e., cycloparaffin) content in such combinations varies with the catalyst and temperature used. Further, GTL base stocks and base oils typically have very low sulfur and nitrogen content, generally containing less than about 10 ppm, and more typically less than about 5 ppm of each of these elements. The sulfur and nitrogen content of GTL base stock and base oil obtained by the hydroisomerization/isodewaxing of F-T material, especially F-T wax is essentially nil.
[0044] In a preferred embodiment, the GTL base stock(s) comprises paraffinic materials that consist predominantly of non-cyclic isoparaffins and only minor amounts of cycloparaffins. These GTL base stock(s) typically comprise paraffinic materials that consist of greater than 60 weight percent non-cyclic isoparaffins, preferably greater than 80 weight percent non-cyclic isoparaffins, more preferably greater than 85 weight percent non-cyclic isoparaffins, and most preferably greater than 90 weight percent non-cyclic isoparaffins.
[0045] Useful compositions of GTL base stock(s), hydroisomerized or isodewaxed F-T material derived base stock(s), and wax-derived hydroisomerized/isodewaxed base stock(s), such as wax isomerates/isodewaxates, are recited in U.S. Pat. Nos. 6,080,301; 6,090,989, and 6,165,949 for example.
[0046] Typically, engine oils have multi-component oxidation inhibition systems including ZDTP and other ashless antioxidants such as hindered phenols, arylamines and/or low sulfur peroxide decomposers to prevent oil from oxidation through different mechanisms. As the levels of ZnDTP are reduced, the anti-wear, anti-oxidation and anti-corrosion protection must rely on the new multi-functional additive system.
[0047] The absence of ZDDP antioxidancy may be compensated by other antioxidants. The principle advantage of a preferred embodiment of this invention is the unique synergistic combination of organic borates, organic silane additives in the presence of low level zinc dithiophosphates and high level of ashless antioxidants that provides favorable oxidation, corrosion stability, deposit control, and more importantly, anti-wear performance. These favorable performance levels can be achieved while reducing the levels of sulfur, ash, phosphorus, and zinc in the engine oil formulations compared to the typical engine oil used today.
EXAMPLES
[0048] As illustrated in the attached Table 3, very good oxidation and corrosion resistance can be achieved with Silane additives. In table 2, a commercial silane additive sold by Chemtura Chemical Company as Silquest A-1589 is used with both PAO/ester synthetic blends and group I mineral oils. The chemical structure for Silquest A-1589 is shown below:
[0000]
[0049] Another suitable Silane is Silquest Y-9805 and is sold by Chemtura Chemical Company. The chemical structure for Silquest Y-9805 is shown below:
[0000]
[0050] The general chemical composition of Silquest Y-9805 is (R 1 —O)(R 2 —O)(R 3 —O)Si—(CRR′) n —Si(OR 3 )(OR 2 )(OR 1 ) where R 1 , R 2 , R 3 are H or C1 to C9 hydrocarbyl groups, R and R′ are H or C1 to C4 hydrocarbyl groups, and n=2-6.
[0051] Another suitable silane is Silquest A-137 sold by Chemutra Chemical Company. The chemical structure for A-137 is
[0000]
[0052] The general structure for Silane A-137 is (R1-O)(R2-O)(R3-O)Si—R where R could be a C1 to C30 hydrocarbyl group.
[0053] As shown by the Pressure Differential Scanning Calorimetry (“PDSC”) Table in 3(a) and 3(b), the onset temperature of oil 2 and oil 4 is 8 to 10 degrees higher than that of oil 1 and oil 3 in the ramping method because oxidation rates generally double with about 10 degrees Celsius increase in temperature, theses results can be translated into about 60 percent to 100 percent better control of viscosity or acid number increases or any other comparable measurements for control of oxidation.
[0000]
TABLE 3(a)
Oil 1
Oil 2
Test Oil = PAO/Ester
1% A-1589
Base Blend 1 (80:20)
99% Base Blend 1
[0000]
TABLE 3(b)
Solubility
Clear & bright
PDSC (Ramp 10° C./min)
Onset T (° C.)
206.4
216.4
Oil 3
Oil 4
Test Oil = 100 SPN
Stock 142
1% A-1589
Group I Base Blend 2
99% Base Blend 2
Solubility
Clear & bright
PDSC (Ramp 10° C./min)
Onset T (° C.)
201.8
210.1
Test Oil = 100 SPN
Cu Corrosion (D130-6)
3 hrs/250° F.
1A
1B
[0054] Table 4 illustrates very good oxidation control with Silquest A-1589 silane additive in a low P engine oil with less than 0.025% P as in oil 5. The antioxidation performance of oil 5 is even better than reference oil A and B when more ZnDTP, instead of silane, was added to Base oil 3 as evidenced by the PDSC data of approximately 5 degree higher onset temperature in the ramping method). Also, excellent corrosion resistance can be maintained with oils formulated with silane additives as shown in oils 5 and 6. The 4-Ball wear results are all consistent and promising.
[0000]
TABLE 4
Reference
Reference
Entry
oil A
oil B
Base
Oil 5
Oil 6
Engine Oil (0.025% P)
Base Blend 3
Reference
Reference
Base
1% A-1589
1% Y-
Blend 3
Base blend 3
9805
Base Blend 3
(0.10% P)
(0.05% P)
0.025% P
0.025% P
0.025% P
Solubility
C & B
C & B
C & B
C & B
C & B
Appearance
Condition Set 1
WSD (mm)
0.39
0.4
1.66
0.33
0.59
4 Ball Wear (D4172)
40 Kg/1800 rpm/30 min./
K Factor
0.2
6
200 F.
Condition Set 2
WSD (mm)
0.4
0.38
0.47
0.36
0.33
4 Ball Wear
40 Kg/1200 rpm/60 min./
K Factor
0.6
1.9
1.4
0.3
0.1
200 F.
Condition Set 3
WSD (mm)
0.35
0.43
0.47
0.36
0.47
4 Ball Wear
40 Kg/600 rpm/30 min./200 F.
K Factor
0.9
3.9
5.8
1.1
5.9
4 Ball EP (D2783)
LNS (Kg)
80
50
63
80
63
30 C./10 sec./1760 rpm
Weld Ld (Kg)
250
250
250
250
250
LWI
37
32
26
36
30
Cu Corrosion (D130-6)
3 hrs/250 F.
1A
1A
1A
1B
1B
Cu Corrosion (D130-8)
3 hrs/210 F./1 wt %
1A
1A
1A
1A
1A
H 2 O
Cu Corrosion (D130-9)
24 hrs/250 F.
1B
1B
2A
1B
1B
PDSC (Ramp 10 C./min)
Onset T (C.)
235.8
235.7
233.6
240.6
234
HFRR
Ave. Friction
0.13
0.12
0.12
0.12
0.12
0.7 Kg/60 Hz/0.5 mm/
% Ave. film
0
14.4
82.1
79.1
89.2
60 min./75 C.
High Temperature
week 1
C & B
C & B
C & B
C & B
C & B
Storage Stability Test
week 2
C & B
C & B
C & B
C & B
C & B
Temperature = 80 C.
week 3
C & B
C & B
C & B
C & B
C & B
Duration: 1 to 4 weeks
week 4
C & B
C & B
C & B
C & B
C & B
Low Temperature
week 1
C & B
C & B
C & B
C & B
C & B
Storage Stability
week 2
C & B
C & B
C & B
C & B
C & B
Temperature = 10° C.
week 3
C & B
C & B
C & B
C & B
C & B
week 4
C & B
C & B
C & B
C & B
C & B
[0055] Adding a silane additive to the 0.025% P base formulation (Base ), results in a 64 to 80 percent reduction in wear scar diameter for condition set 1. Furthermore, a 23 to 30 percent reduction is found for condition set 2 and a 0 to 23 percent reduction can be seen in condition set 3. The High Frequency Reciprocating Rig (HFRR) data demonstrates silanes can help maintain strong film formation and excellent frictional properties, while adding more ZnDTP may destroy the film formation mechanism.
[0056] All silanes dissolve easily in engine oils and remained clear and bright on the shelf at both low and elevated temperatures over a period of four weeks at both 10 degrees Celsius and 80 degrees Celsius. Apparently, the stability of silane containing oils is satisfactory and silanes cause no adverse effects to compatibility in the presence of other commonly used additives in engine oil compositions. The 4-Ball EP test, demonstrate significant improvements in last non-seizure (LNS) load and load wear index (LWI) with oils formulated with a silane additive. This improvement is most prevalent, in is oil containing disulfide-silanes such as, Silquest A-1589 as shown in oil 5. An increase of 4 to 10 units in LWI over base oil is significant as this performance is almost identical or better than what ZnDTP provides when comparing oil 5 versus reference oils A and B.
[0057] As illustrated in Table 5, very good oxidation control can be achieved when silanes and ZnDTP were used together in a low phosphorous, low ash engine oil of less than 0.05% phosphorous. The anti-oxidation performances of oils at columns 7 and 8 are much better than that of reference oil D as evidenced by PDSC data of 2 to 8 degrees higher onset temperature by the ramping method. In fact, oil 7 is even better than reference oil C as adding more Silquest A-1589 gives better performance than adding ZnDTP. Also, excellent corrosion resistance can be maintained with oils formulated with silane additives as shown by oils 7 and 8.
[0000]
TABLE 5
Entry
Reference oil C
Reference Oil D
Base
Oil 7
Oil 8
Base Blend 4
1% Silquest A-
1% Silquest A-
1589
137
1.0% ZnDDP
0.5% ZnDDP
0.5% ZnDDP
0.5% ZnDDP
Base Blend 4 is a P-free
99% Base
99.5% Base
0% P
98.5% Base
98.5% Base
Blend 4
Blend 4
Blend 4
Blend 4
Partially formulated engine
(0.10% P)
(0.05% P)
(0% P)
(0.05% P)
(0.05% P)
oil
Solubility/Compatibility
Good
Good
Good
Good
Good
Appearance
Clear & bright
Clear & bright
Clear & bright
Clear & bright
Clear & bright
4 Ball Wear
WSD (mm)
0.37
0.4
0.45
0.4
0.43
40 Kg/600 rpm/30 min./200 F.
K Factor
1.4
2.5
4.9
2.5
3.9
4 Ball EP (D2783)
LNS (Kg)
80
80
50
80
80
30 C./10 sec./1760 rpm
Weld Ld (Kg)
200
200
160
250
200
LWI
35
34
22
42
34
Cu Corrosion (D130-6)
3 hrs/250 F.
1A
1A
1B
1A
1A
Cu Corrosion (D130-8)
3 hrs/210 F./H 2 O
1A
1B
3A
1A
1A
Cu Corrosion (D130-9)
24 hrs/250 F.
1A
1A
2A
1A
1A
PDSC (Ramp 10 C./min)
Onset T (C.)
232
229.7
233.5
238.4
232
Hot Tube Test (288 C./16 hr)
Tube Rating
3.8
3.5
1
3
3.5
(1 = Clean, 9 = dirty)
HFRR
Ave. Friction
0.14
0.15
0.14
0.13
0.13
0.7 Kg/60 Hz/0.5 mm/
Scar X/Y (mm)
0.32/0.7
0.3/0.77
0.37/0.73
0.3/0.73
0.3/0.73
60 min./75 C.
Calc. Sc. Area
0.17
0.18
0.21
0.17
0.17
D2896
TBN
4.27
4.23
4.12
D874 (wt %)
Sulfated Ash
0.53
0.38
0.32
D6443 (wt %)
Phosphorus
0.1003
0.0507
<0.002
0.0474
D6443 (wt %)
Zinc
0.1118
0.0577
<0.002
0.0545
D6443 (wt %)
Calcium
0.0329
0.0332
0.0334
0.0326
D6443 (wt %)
Magnesium
0.0595
0.0496
0.494
0.0525
D6443 (wt %)
Copper
<0.002
<0.002
<0.002
<0.002
D6443 (wt %)
Chlorine
0.0047
0.0049
0.0047
0.0061
D6443 (wt %)
Sulfur
0.2799
0.1783
0.072
0.3165
High Temperature
week 1
C & B
C & B
C & B
C & B
Storage Stability Test
week 2
C & B
C & B
C & B
C & B
Temperature = 80 C.
week 3
C & B
C & B
C & B
C & B
Duration: 1 to 4 weeks
week 4
C & B
C & B
C & B
C & B
Low Temperature
week 1
C & B
C & B
C & B
C & B
Storage Stability Test
week 2
C & B
C & B
C & B
C & B
Temperature = 10° C.
week 3
C & B
C & B
C & B
C & B
Duration: 1 to 4 weeks
week 4
C & B
C & B
C & B
C & B
[0058] The 4-Ball wear results are good as equivalent wear scar diameters are reported. The HFRR data showed that silanes can help reduce the calculated wear scar area while maintaining excellent frictional properties. The Hot Tube test which is a typical test to assess cleanliness features of engine oils under high temperature oxidation conditions. As indicated, oils 7 and 8 both have equivalent or slightly better Hot Tube results than reference oil D with the lower the rating, the better the cleanliness. These results demonstrate that silane additives contribute no adverse effects to cleanliness. All silanes dissolved easily in engine oils and remained clear and bright on the shelf at both low and elevated temperatures over a period of four weeks at 10 degrees Celsius and 80 degrees Celsius. Apparently the storage stability of silane containing oils is satisfactory and silanes cause no adverse compatibility effects in the presence of other commonly used additives in engine oil compositions. Perhaps, the most significant improvement of all is the exceptionally good load-carrying property. Evaluating silane containing oils in a 4-Ball EP test, illustrate significant improvements in last non-seizure (LNS) load and load wear index (LWI) can be observed as shown by oil 7 with 1 percent Silquest A-1589. An increase of 8 units in LWI over reference oil D is significant and an increase of 7 units in LWI over reference oil C is even more significant as this performance level exceeds what ZnDTP can provide.
[0059] In a preferred embodiment, very low levels of metals are present in the final composition of the formulation. As shown in Table 4 only trace amounts of copper iron, barium, aluminum, potassium, chromium, manganese, nickel, lead, silver, sodium, tin, and vanadium are present.
[0060] A synergistic combination of organic silanes and low level of zinc dithiophosphates in the low SAP engine oil formulations can reduce wear and increase oxidative stability. Table 6 illustrates this example embodiment.
[0061] As shown in the attached Table 6, three engine oils were formulated and compared to each other. Reference oil E is an oil of relatively high ash as evidenced by high sulfated ash level (0.94 weight percent) and high TBN number (7.73). Reference oil F is a low ash oil with essentially almost identical formulation to oil A except at much reduced detergent level (888 ppm versus 2169 ppm calcium). Inventive oil 9 has similar detergent level as oil F except that 1 weight percent of a sulfur containing silane was added. As a result, the sulfur level is higher in oil 9 (0.3266%, still below the industry standard limit of 0.5%), but the ash level is still much lower than the level is in reference oil E. Clearly, the silane additives have shown strong synergistic effect with low level of zinc dithiophosphates in low ash oils. Therefore, the silane additives are more suitable for low ash engine oil application. Comparing reference oils E and F the Four-ball wear performance of oil F is not as good as oil E when the total amount of detergents is reduced. The K-factor indicates a factor of 3 times weaker in anti-wear control in oil F compared to oil E (6.22/2.06). However, when silane was added to oil F to form oil 9, the anti-wear performance improves significantly (by a factor of 4.5, 6.22/1.37), which is even better than the performance of oil A at higher ash level. Also, as shown in Pressure Differential Scanning Calorimetry (PDSC), the onset temperature of oil 9 is 8.3 to 25 degrees higher than results of oil A and oil B (ramping method). Since oxidation rates generally double with about every 10° C. increase in temperature, these results are impressive with respect to the ability to reduce and control oxidation by these oils. If translated directly into the control of viscosity or acid number increases, or other measurements of control of oxidation, oil 9 is estimated to be 83% to 565.7% better than reference oils E and F.
[0062] In this embodiment, we have identified a new engine oil system based on very unique combination of additives that demonstrate outstanding and unexpected performance improvements. This unique component synergism concept is believed to be applicable to similar formulations containing (a) low TBN detergent system of less than 6 for the finished oils, (b) a low ash level of less than 0.8 weight percent ash, (c) a low level of ZnDTP of less than <0.08 weight percent phosphorus in the finished oil), and (d) a silane additives which are preferably sulfur containing silanes.
[0000]
TABLE 6
Entry
Reference oil E
Reference oil F
Oil 9
Metal Detergent
3.0% Ca
1.2% Ca
1.2% Ca
Detergent
Detergent
Detergent
Zinc Dithiophosphate
.75% ZDTP
.75% ZDTP
.75% ZDTP
Partial engine oil
96.25%
98.05%
97.05%
formulation (0% P)
Silane
1.0 wt % A-
1589
(0.075% P)
(0.075% P)
(0.075% P)
Solubility
C & B
C & B
C & B
Appearance
4 Ball Wear
WSD (mm)
0.389
0.6
0.367
40 Kg/600 rpm/30 min./200 F.
K Factor
2.06
6.22
1.37
4 Ball EP (D2783)
LNS (Kg)
100
100
100
30 C/10 sec./1760 rpm
Weld Ld (Kg)
250
250
250
LWI
42.5
42.9
43.1
Cu Corrosion (D130-6)
3 hrs/250 F.
1A
1A
1A
Cu Corrosion (D130-8)
3 hrs/
1A
1A
1A
210 F/H 2 O
Cu Corrosion (D130-9)
24 hrs/250 F.
1A
1A
1A
PDSC
700 Kpa O 2
Ramp method (Onset temp)
10 C./min
259.4 C.
276.1 C.
284.4 C.
D2896
TBN
7.73
4.53
5.3
D874 (wt %)
Sulfated Ash
0.93
0.54
0.78
D6443 (wt %)
Phosphorus
0.0776
0.0774
0.0771
D6443 (wt %)
Zinc
0.083
0.0841
0.0855
D6443 (wt %)
Calcium
0.2169
0.0888
0.0866
D6443 (wt %)
Magnesium
0.0028
<0.002
<0.002
D6443 (wt %)
Copper
<0.002
<0.002
<0.002
D6443 (wt %)
Chlorine
<0.002
<0.002
0.0037
D6443 (wt %)
Sulfur
0.2041
0.1987
0.3266
Comment
High
Low
Low
detergent
detergent
detergent
[0063] In summary, a new engine oil system is presented based on very unique combinations of silane additives and low levels of ZnDTP that demonstrate outstanding and unexpected performance to modern engines. This offers an effective way to reduce the amount of ZnDTP for contemporary engine oils while maintain excellent wear, oxidation and corrosion protection. | The present invention is directed to a lubricating oil composition comprising a lubricating oil basestock, an organic silane containing additive of at least 0.1 and less than 2.0 weight percent of the composition, a dispersant-detergent-inhibitor system of less than 15 weight percent of the composition, an organic boron additive of at least 0.1 and less than 8.0 weight percent of the composition, a zinc dithiophosphate additive of at least 0.1 weight percent of the composition and less than 1.6 weight percent of the composition and the composition having at least 80 PPM and less than 1600 RPM silicon, at least 100 PPM and less than 630 PPM phosphorus, at least 105 PPM and less than 710 PPM zinc, at least 1,000 PPM and less than 4,000 PPM sulfur, at least 800 PPM, less than 10,000 PPM ash and less than 450 PPM boron. In a second embodiment, an additive composition for lubricating oils is disclosed. In a third embodiment, a method of obtain a favorable lubricating properties is disclosed. | 2 |
This is a division, of application Ser. No. 773,037, filed Oct. 8, 1991, now U.S. Pat. No. 5,201,315.
The present invention relates to obtaining ultrasound images of body cavities, lumens, or vessels and, particularly, to obtaining images of coronary arteries. The present invention discloses a sheath containing a guide wire lumen, an ultrasound probe lumen, and a lumen which alternately serves as a passage for either the guide wire or the probe.
BACKGROUND OF THE INVENTION
Invasive ultrasound imaging catheters are designed for use in conjunction with a guide wire. In the past, four different methods have been used to adapt the imaging catheter to a guide wire.
In the first method a guide wire tip is attached to the distal end of an imaging sheath and is known as a "fixed wire" design. This method has been used with mechanically rotated probes. The design, however, has two disadvantages, first, the wire cannot be left across a lesion while the imaging catheter is withdrawn and replaced with a different device, and secondly, fixed wire devices are more difficult to "steer" than the common "steerable" and "removable" guide wires. An example of a fixed wire tip is disclosed in U.S. Pat. No. 4,794,931--Yock.
A second type of catheter, known as transducer-array catheters, have been designed so that a guide wire can be threaded through a lumen which passes coaxially through the array. This design allows a user to place the imaging catheter over a guide wire by the same methods practiced with standard dilatation catheters. Transducer array catheters work with electronically scanned transducer arrays however this type of catheter design cannot be adapted for use with mechanically-rotated probes. An example of a transducer-array catheter is disclosed in U.S. Pat. No. 4,917,097--Proudian et al.
The third catheter design uses a dual lumen sheath. A lumen for the guide wire and a parallel lumen for a rotating ultrasound probe are provided. Unfortunately, the side-by-side positioning of the wire and probe lumens causes the catheter to be of a larger cross-section than is necessary for ultrasound imaging. Large catheters are disadvantageous because they reduce or stop blood flow in small or narrowed arteries. A product of this type is sold by Cardiovascular Imaging Systems, Inc. of Mountain View, Calif. (USA).
Finally, a fourth design for this type of catheter provides a single-lumen sheath positioned over a guide wire and across the section of the vessel to be imaged. The wire is then removed and "replaced" with an ultrasound probe. This design has the advantage of yielding a catheter diameter which is not much larger than the probe diameter. However, using the single-lumen sheath in conjunction with "over-the-wire" catheters is time consuming. For example, to remove the ultrasound catheter and position a dilatation catheter a user would first remove the probe, then position the guide wire and remove the sheath. Finally, the user would place the dilatation catheter over the wire. In contrast, a user can exchange one dilatation catheter for another by removing the first catheter and placing the second catheter over the wire. The time difference can be very important when working within the coronary arteries. An example of this type of device is sold by InterTherapy, Inc. of Santa Ana, Calif. (USA).
Thus, it can be seen that there is a long-felt yet unfilled need to provide a design which permits a catheter containing a mechanically rotated probe to be steered into place using a guide wire while maintaining a minimum cross-section.
SUMMARY OF THE INVENTION
An object of the invention is to provide a method for using improved sheaths.
Thus, in a preferred embodiment the present invention provides a flexible sheath for positioning an ultrasound imaging probe within a region of a vessel comprising a distal tip portion with a lumen adapted to accept a guide wire, a flexible single lumen intermediate section connected proximally to the distal tip portion, and a dual lumen region extending proximally from the flexible intermediate section. The dual lumen region comprises a wire lumen adapted to accept a guide wire and a probe lumen adapted to accept an ultrasound probe wherein the probe lumen and wire lumen connect with the single lumen intermediate section.
Most preferably, the sheath of the present invention includes a tapered flexible tip at the distal portion which has a lumen for accepting the guide wire and a radio opaque marker for X-ray viewing. Similarly, in certain preferred embodiments, a radio opaque marker for X-ray viewing will be disposed within the flexible intermediate section. Most preferably, the intermediate section lumen and the probe lumen are coaxial and the wire lumen is connected to the intermediate-section lumen at a tapered transition. Additionally, in certain embodiments of the present invention a three lumen section may also be provided in place of the proximal dual lumen section of the exemplary embodiment described herein.
The present invention also discloses methods of ultrasonically imaging a region of a subject by using an ultrasound probe, a guide wire and an ultrasound sheath substantially made in accordance with the present invention. The guide wire is advanced through the subject until the distal tip of the wire is distal to the region to be imaged and the intermediate portion of the sheath is then advanced over the wire until it has passed through the region to be imaged. The wire is then withdrawn from the single lumen portion of the sheath while holding the sheath stationary within the subject and leaving the distal tip of the wire within the dual lumen portion of the sheath. The ultrasound probe tip is next advanced into the intermediate portion of the sheath while holding the sheath stationary within the subject and the probe is activated to obtain ultrasound images.
In certain embodiments of the methods of the present invention a further step permitting additional over-the-wire invasive procedures to be performed are disclosed that include the steps of holding the sheath stationary and retracting the probe from the single lumen portion of the sheath and then advancing the wire through the sheath tip, whereby the distal tip of the wire is again disposed at a point beyond the region to be imaged. The wire is then held stationary and the sheath and the probe are retracted whereby the probe and sheath are removed from the subject thereby leaving the wire in place for additional procedures. Also, certain methods of the present invention also permit recovery from ischemic episodes during use that include the steps of holding the sheath stationary within the subject, retracting the probe until it is disposed proximal to the single lumen, and advancing the wire through the single lumen. The wire is held stationary within the artery and the probe and sheath are withdrawn until the tip of the sheath is outside the narrow portion of the artery whereby increased blood flow occurs to combat the ischemia. After the ischemia episode passes, the above-described methods are undertaken at the step of advancing the sheath through the region to be imaged.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects and features of the present invention will appear after careful consideration of the preceding and following description including the drawings in which:
FIG. 1 is a longitudinal cross-section of the distal end of a sheath made in accordance with the present invention.
FIG. 2 is a cross-sectional view of the distal end of a sheath made according to the invention taken along line 2--2 of FIG. 1.
FIG. 3 is a partial view of the indicated portion of the sheath shown in FIG. 1 illustrating the transition region of the sheath.
FIG. 4 is a partial view of the indicated portion of the sheath shown in FIG. 1 illustrating an atraumatic tip.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to FIG. 1, the distal portion of a sheath 100 made in accordance with the present invention is illustrated. Those of ordinary skill will understand that the sheath 100 is typically substantially tubular and that FIG. I illustrates a longitudinal cross-section of the sheath 100. Those of ordinary skill will further be familiar with the types of materials and methods used to manufacture sheaths such as those disclosed herein. Preferably, the sheath 100 of the present invention is lubricated on its exterior surface and may also be lubricated on its interior surface. Assuming a coronary artery imaging application, the complete sheath 100 is preferably about 1.5 meters long. The distal tip portion of the sheath is preferably about 1.0 cm long and is flexible so that it may be advanced over a guide wire that has been threaded through a coronary artery. The distal tip portion of the sheath 100 is soft and tapered as explained below with reference to FIG. 4 so that it is atraumatic to the artery. The inside diameter of the distal tip portion of the sheath is preferably tapered as shown. This taper permits a guide wire tip to move freely through the distal tip, which is preferably radio opaque or contains an opaque marker 102 to indicate the sheath-tip location in X-ray views. The inside diameter is most preferably sized to accept a guide wire and is about 15 or 20 mils across.
The intermediate section of the sheath adjoining the distal portion is a flexible elongated substantially tubular section that is also substantially transparent to the acoustic energy used for imaging. The interior diameter of the intermediate section of the sheath 100 is large enough to pass either a guide wire or an imaging probe. The outside diameter is preferably only a few thousandths of an inch larger than the interior diameter, thus the sheath wall in this region is relatively thin. A wide range of choices exist for selecting the length of this portion of the sheath 100; a short length, for example 1 cm, could be used. However, a longer length, for example 10 cm, allows image collection at various positions in the artery without repositioning the sheath 100.
The region of the sheath 100 near cross-sectional arrows 2--2 shown in FIG. 1 is comprised of flexible dual lumen tubing. A guide wire lumen 110 and a probe lumen 120 are disposed side-by-side so that a wire and a probe may simultaneously be inserted into this portion of the sheath 100. The diameters of the guide wire lumen 110 and probe lumen 120 are thus sized to accept the wire and probe. In a preferred embodiment, this section of the sheath 100 is generally at least 10-20 cm long so that the wire can be retracted from the distal portions of the sheath 100 without accidentally retracting it from the dual lumen region. It is also feasible to extend the dual lumen region of the sheath 100 to a length that includes the proximal end of the sheath 100, i.e., toward the left side of the sheath 100 illustrated in FIG. 1.
The transition area between the dual lumen region and the intermediate section is smoothly tapered to make the sheath 100 atraumatic to the artery being imaged. As explained below, this section of the sheath can also be marked so that it can be seen in X-ray views. However, those of ordinary skill will realize that the physical marker can be placed in the sections of the sheath closer to the proximal or distal ends but should be kept near the transition section so that the user can easily infer this section's location in the artery. FIG. 1 shows the probe lumen 120 connecting straight into the lumen of the intermediate section while the wire lumen 110 is offset. This is just one example of how the taper in the section near the dual lumen can be accomplished; either or both lumens 110,120 of the dual lumen region can be offset from the lumen in the intermediate section.
The proximal section of the sheath 100 is a single lumen tubing which passes the ultrasound probe. It extends from the dual lumen region to essentially the proximal end of the sheath 100.
FIG. 2 shows the dual lumen region of the sheath in cross-section as indicated by arrows 2--2 in FIG. 1. The cross-section shows substantially circular inside and outside surfaces; however, it should be understood that other shapes could readily be used. From FIG. 2 one of ordinary skill can appreciate that the intermediate section is substantially smaller in cross-sectional area than the dual lumen region. Thus, with a given ultrasound probe diameter, the sheath of the present invention allows imaging in a smaller artery than is possible with a sheath design wherein the dual lumen region resides in the imaged portion of the artery. A numerical example is useful to illustrate this point. Assuming currently available probes and wires are used, a wire lumen 110 of about 0.016" (0.4 mm) and a probe lumen 120 of about 0.045" (1.1 mm) could be chosen. For reliability and construction ease, the minimum wall thicknesses in the sheath are at least several mils, for example 0.005" (0.1 mm). From these numbers it is possible to calculate the ratio, R, of the cross-sectional area of the dual lumen region of the sheath 100 with respect to the cross-sectional area of the sheath in the flexible intermediate section, thus: ##EQU1## (Values in parentheses in mils).
The sheath design of the present invention therefore offers an advantage over previous designs that include the distal end of the guide wire lumen terminating in the distal tip. The advantage is that with the sheath 100 of the present invention a smaller cross-section is placed in the section of artery to be imaged, thereby reducing blood flow blockage. As ultrasound probes are made smaller the ratio R will become larger and the advantage increased.
FIG. 3 shows an enlarged view of the transition section where the wire lumen 110 and probe lumen 120 join. A location for a proximal radio opaque marker 104, as discussed above is also shown. The radio opaque marker 104 is preferably formed using a metallized band comprised of platinum or gold alloy.
FIG. 4 shows an enlarged view of the distal tip portion of the sheath, which preferably includes a distal radio opaque marker 102 discussed above. The marker 102 can also be formed using a metal band.
The present invention also provides improved methods of obtaining images. Consider using the sheath of the present invention during a percutaneous transluminal coronary angioplasty (PTCA) procedure. An ultrasound probe is inserted into the probe lumen 120 with the probe tip proximal to the transition section. Doses of contrast media are supplied where needed to allow X-ray visualization and anatomic orientation. A guide wire is introduced through a guiding catheter and into the proper coronary artery. After the wire tip is positioned on the distal side of the restriction or lesion, the wire is used to guide the sheath 100 into the artery and through the stenosis. The flexible intermediate section is then placed within the stenosis using X-ray visualization, and the guide wire is retracted so that the distal tip of the wire resides in the wire lumen 110 and is clear of the intermediate section. The ultrasound imaging probe is then advanced into the intermediate section to obtain desired images. If the patient becomes ischemic before needed images are obtained, the probe tip can be extracted a short distance into the dual lumen section and the wire advanced through the distal tip of the sheath 100 into the artery. The sheath 100 and probe may then be retracted from the lesion and thereby allow increased blood flow through the lesion. When the ischemia passes, the sheath 100 and probe are repositioned and the needed images can then be obtained.
After obtaining images, the probe tip is drawn into the dual lumen region and the wire advanced a short distance through the sheath tip. The sheath 100 and probe are then withdrawn until outside the body and free from the wire. This last step leaves the wire and guiding catheter ready for use with a dilatation catheter. After the dilatation, additional images can be obtained by repeating the previously described steps.
The use of the present invention has been described in conjunction with a therapeutic PTCA procedure. It is understood, however, that the sheath 100 disclosed herein can also be used in conjunction with other invasive procedures or as part of a diagnostic procedure. Additionally, those of ordinary skill will realize that a third lumen could be incorporated proximal of the intermediate section into the sheath 100 illustrated and described. The sheath 100 could then be used to deliver other devices, probes or sensors and the like, permitting other signals or substances to be introduced into the patient, other parameters monitored or other therapies initiated. Thus, although the present invention has been described in what is presently considered the most practical and preferred embodiment it is to be understood that the invention is not to be limited to the disclosed embodiment. The invention is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. | An ultrasound imaging method for invasive imaging, in particular for imaging blood vessels including the coronary vessels. A sheath is comprised of three lumens; one serves as an ultrasound probe passage, one serves as a guide wire passage, and one serves as either a probe or a guide wire passage and is connected to the other two. Methods of using the sheath disclosed to obtain ultrasound images of a region within a subject are disclosed. | 0 |
CROSS REFERENCE TO RELATED UNITED STATES APPLICATIONS
This application claims priority from U.S. Provisional Application No. 61/033,958 of Dikici, et al., filed Mar. 5, 2008, and from U.S. Provisional Application No. 61/036,607 of Dikici, et al., filed Mar. 14, 2008, the contents of both of which are herein incorporated by reference in their entireties.
TECHNICAL FIELD
This disclosure is directed to the segmentation of vascular structures in volumetric image datasets.
DISCUSSION OF THE RELATED ART
Segmentation of vascular structures in volumetric datasets facilitates several forms of useful analysis. For example, quantification of the dimensions of an aortic aneurysm helps to determine the time point for intervention. In coronary artery disease, the degree of latency of a stenotic lesion influences treatment decisions. And, the planning for the placement of stents and by-pass graphs benefits greatly from the delineation of the vessel boundaries. Finally, a by-product of segmentation is enhanced visualizations, such as fly-throughs, curved reformats, and multiple vessel flattening.
Vessel segmentation is challenging, however. First, branch points, such as bifurcations or trifurcations, add a degree of difficulty to tracking the vessel path. Second, adjacent structures with similar signal intensities may cause a segmentation to “leak” into them. Finally, intensity values within the vessel may vary due to uneven distribution of contrast or partial volume effects and can complicate segmentation.
Fast, accurate vessel segmentation has been a long sought goal in medical image analysis. A rho-theta parameterization can be used for the detection of non-complex objects, such as lines and circles, and many papers have been published which generalize the idea to more complex shapes or even to 3-D. Iterative voting has also been applied for the localization of the salience using radial voting for the detection of the centers of blob shaped objects in stellar data and cell culture systems in 2D and 3D.
While minimal cuts have been extensively used in general image segmentation, it has rarely been applied to the recovery of tubular structures. Since the minimal cuts paradigm seeks to minimize a sum total of the weights of a cut, in single source seed scenarios, blobby structures are favored. Therefore, to segment a non-blob like shape, such as a tube, providing multiple strong t-link connection along the shape skeleton becomes useful. Up to now, it has been challenging to consistently and correctly identify which voxels (the centerpoints) should receive strong t-link weights to the source. As a result, recovery required a user to manually place multiple seeds, which is an impractical solution.
For the computation of vessel centerlines, Dijkstra's shortest path (DSP) algorithm is a natural fit because of the applicability of solution to the task domain. However, there are many caveats that should be addressed in DSP based solutions including but not limited to the following: (1) the scale of the graph should be limited to keep the computational costs low, (2) final centerlines should not hug the borders of the tubular object, (3) surrounding non-targeted objects should not define nodes.
SUMMARY OF THE INVENTION
Exemplary embodiments of the invention as described herein generally include methods and systems for segmenting vessels from volumetric datasets which rely on axial symmetries for the detection of centerpoints of vessels. A centerpoint identification scheme is introduced which exhibits robustness adequate for the application of the minimal cuts paradigm to 3D vessel segmentation and a method for tracking a coronary artery centerline given a single user supplied distal endpoint. Briefly, based on a user supplied seed point, a small cubic subregion of the image volume is extracted. Within this subregion, potential vessel centerpoints are identified by a two stage Hough-like election scheme whereby voxels vote for the most likely points belonging to the vessel centerline. Voxels are restricted to vote in a within a 3D cone-shaped kernel which has its tip located on the voxel, and is oriented in the direction of the voxel's image gradient, such as might be found on a vessel border. These candidates then are winnowed down via a normalized radius image. A point must be both popular according to a first vote image, as well as being consistently voted upon via the radius image to make it to the final vote image. Next, the image volume is reconfigured as a graph upon which the maxflow/minimal cut algorithm will be applied. The t-link weights in the graph are based on the vote image, and the n-link weights on the image intensity and gradient. Applying the min-cut algorithm, the vessel, including any branches, is segmented within the subregion. Intersections of the segmentation with the subregion's boundaries serve as starting points for tracking the vessels' paths. New subregions are centered on these starting points (overlapping with the previous subregion) and the process begins again. An optimal path can be searched from a user supplied endpoint to any point on the aorta surface (an ostium) to recover the vessel of interest.
An algorithm according to an embodiment of the invention can handle branching. Regardless of the number or degree, each branch defines an axial symmetry around its centerline because of its tubular structure. This will be detected. A minimal cut algorithm according to an embodiment of the invention can find a segmentation that does not require an a priori identification of any divisions off the vessel. An algorithm according to an embodiment of the invention can avoid leaking into adjacent strictures of similar intensity due to the normalized radius image. Since centerpoint detection is based on gradients rather than intensities, an algorithm according to an embodiment of the invention is less prone to failure in cases where the vessel intensity fluctuates. The minimal cuts paradigm facilitates simple and intuitive means for editing through the placement of seed points. An algorithm according to an embodiment of the invention does not require multiple scales. A size is specified for a cone-shaped kernel for performance reasons rather than for detection. As long as the cone height is greater than the vessel radius, the centerpoint will be identified.
According to an aspect of the invention, there is provided a method for segmenting tubular structures in digital medical images, including extracting a subregion from a 3-dimensional (3D) digital medical image volume containing a vessel of interest, for each voxel in the subregion, identifying potential vessel centerpoints by attaching to each voxel a tip of a 3D cone that is oriented in the direction of the voxel's image gradient and having each voxel within the cone vote for those voxels most likely to belong to a vessel centerline, selecting candidates for a second vote image that are both popular according to a first vote image, as well as being consistently voted upon by a radius image, reconfiguring the subregion as a graph where each voxel is represented by a node that is connected to 26 nearest neighbors by n-link edges, and applying a min-cut algorithm to segment the vessel within the subregion.
According to a further aspect of the invention, the segmented vessel includes branches.
According to a further aspect of the invention, the method includes detecting intersections of the segmented vessel with the subregion's boundaries, where intersection voxels serve as starting voxels for extracting a new subregion overlapping with the current subregion, where the new subregion serves to track the vessel's centerline.
According to a further aspect of the invention, the subregion is a cubic subregion of size
x i = [ - d 2 , d 2 ]
for each axis i centered on a user supplied starting voxel where d is predetermined based on a vessel category.
According to a further aspect of the invention, a voxel {right arrow over (v)} within the 3D cone is defined with respect to the cone tip voxel {right arrow over (x)} as
v -> = Θ -> ( ∇ I ( x -> ) ∇ I ( x -> ) ) [ r cos ( θ ) sin ( α ) , r sin ( θ ) sin ( α ) , r cos ( θ ) ] T ,
where ∇ I ( x -> ) ∇ I ( x -> )
is the image gradient,
Θ -> ( ∇ I ( x -> ) ∇ I ( x -> ) )
is a rotation matrix aligning the central axis of the cone with the image gradient direction, α:[−α max ,α max ], is an angle {right arrow over (v)} forms with the image gradient vector,
r : [ 0 , h cos ( α max ) ] ,
is a length of a vector represented by {right arrow over (v)}, and θ: [0,2π] is a sweep out parameter.
According to a further aspect of the invention, voting comprises incrementing a first vote image as V({right arrow over (x)}+{right arrow over (v)})=V({right arrow over (x)}+{right arrow over (v)})+K({right arrow over (v)})log(|∇I({right arrow over (x)})|) for each voxel {right arrow over (v)} in the cone, where
( - d 2 , - d 2 , - d 2 ) ≤ ( x -> + v -> ) ≤ ( d 2 , d 2 , d 2 ) ,
incrementing a radius image as R({right arrow over (x)}+{right arrow over (v)})=R({right arrow over (x)}+{right arrow over (v)})+K({right arrow over (v)})|{right arrow over (v)}−{right arrow over (x)}|, where K({right arrow over (v)}) is a kernel that weights a point {right arrow over (v)} in the cone by
K
(
v
->
(
r
,
α
)
)
=
exp
(
-
α
2
/
2
σ
2
)
r
cos
(
α
)
.
According to a further aspect of the invention, the method includes incrementing a weight image Σ({right arrow over (x)}) for each voxel vote according to Σ({right arrow over (x)}+{right arrow over (v)})=({right arrow over (x)}+{right arrow over (v)})+Σ({right arrow over (v)}), and after voting, normalizing the radius image by dividing by the weight image.
According to a further aspect of the invention, selecting candidates for a second vote image comprises finding, for each voxel {right arrow over (x)} in the subregion, a voxel, {right arrow over (v)} max within the cone whose tip is attached to voxel {right arrow over (x)} that has the maximum number of votes, and forming the second voting image V′({right arrow over (x)}) by voting for those {right arrow over (v)} max voxels whose distance to the cone tip {right arrow over (x)} is approximately equal to the normalized radius image value for that point, according to V′({right arrow over (x)}+{right arrow over (v)} max )=V′({right arrow over (x)}+{right arrow over (v)} max )+K({right arrow over (v)} max )log(|∇I({right arrow over (x)})|).
According to a further aspect of the invention, the method includes normalizing the second voting image by dividing by the weight image.
According to a further aspect of the invention, reconfiguring the subregion as a graph further comprises including two additional nodes, {s,t} representing a source and a sink respectively, linking the source and sink to the voxel nodes pεP forming t-link edges, t-link weights in the graph are determined by the second vote image, and the n-link weights are determined by the subregion's intensity and gradient.
According to a further aspect of the invention, the min-cut algorithm minimizes an energy of the form
E ( f ) = ∑ p ∈ P D p ( f p ) + ∑ p , q ∈ N V p . q ( f p , f q ) ,
where f=[0,1] is a label distinguishing a vessel node from a non-vessel node, V p,q is a weight for an n-link connecting voxel nodes p, q,
V p , q , ∈ N = C 1 exp ( ( ( I ( p ) - I ( q ) ) 2 + cos - 1 ( ∇ I ( p ) ∇ I ( p ) · ∇ I ( q ) ∇ I ( q ) ) ) 2 σ 2 ) ,
D p is a t-ink weight defined as D p =C 2 A(p) for voxel nodes p connected to the source node, and D p =C 2 (1−A(p)) for voxel nodes p connected to the sink node, σ 2 , C 1 and C 2 are predetermined constants, and A(p) is a normalized second vote image evaluated for node p.
According to another aspect of the invention, there is provided a method for segmenting tubular structures in digital medical images, including extracting a subregion of a digital medical image volume containing a vessel of interest, having each voxel in the subregion vote on a vessel center where votes are cast in a conical region whose tip is on the voxel and whose central axis is oriented in a gradient direction, where the votes are weighted proportional to the intensity of the gradient at a cone voxel and how close the cone voxel is to the central axis of the cone to create a first vote image, and are weighted proportional to the distance between the subregion point and the cone point to create a radius image, searching the first vote image for a most popular centerpoint candidate within the conical region for each subregion voxel, voting for the centerpoint candidate if the distance to the centerpoint candidate from the point is in agreement with the value for a corresponding location in the radius image to form a second vote image, constructing a graph from the second vote image, searching the graph for an optimal path from a user supplied endpoint to any point on a vessel surface to recover the vessel of interest.
According to a further aspect of the invention, extracting a subregion comprises segmenting a left ventricle from the image volume using an initial point found by searching for bright circular regions at an orientation commonly assumed by the left ventricle, determining a second point in an aorta based on spatial and intensity priors relative to the left ventricle segmentation, and extracting an aorta mask, T({right arrow over (x)}) by finding a connected component of voxels with intensities crossing a threshold, where the threshold is computed using the second point inside the aorta.
According to a further aspect of the invention, the method includes incrementing a weight image for each voxel vote by a weighting factor associated with the cone defined by
K ( v -> ( r , α ) ) = exp ( - α 2 / 2 σ 2 ) r cos ( α ) ,
where voxel {right arrow over (v)} is within the cone. α:[−α max ,α max ] is an angle {right arrow over (v)} forms with the image gradient vector,
r : [ 0 , h cos ( α max ) ]
is a length of a vector represented by {right arrow over (v)} and σ 2 is a predetermined constant, and normalizing the second voting image by dividing by the weight image to form an axial symmetry image.
According to a further aspect of the invention, vertices V={B,H,U} of the graph are defined as B={{right arrow over (x)}: ∇T({right arrow over (x)})>ε 2 } where T({right arrow over (x)}) is the aorta mask, H={{right arrow over (x)}: A({right arrow over (x)})>ε 3 }, the axial symmetry voxels over a threshold; and U is a user supplied endpoint, edges E ij are created between any two vertices i, j which are less than a predetermined distance apart, and the edges are weighted by line integral between two vertices through a multiplicative inverse of the axial symmetry image,
w ( E ij ) = ∫ C ij 1 A ′ ( s ) ⅆ s ,
where C ij is a line segment connecting vertices v i and v j .
According to a further aspect of the invention, the graph is searched using Dijkstra's algorithm.
According to another aspect of the invention, there is provided a program storage device readable by a computer, tangibly embodying a program of instructions executable by the computer to perform the method steps for segmenting tubular structures in digital medical images.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a flowchart of a method for segmentation of vascular structures in volumetric image datasets, according to an embodiment of the invention.
FIG. 2( a ) shows a conical voting region based on a voxel, according to an embodiment of the invention.
FIG. 2( b ) shows a view of the vessel cross-section with radius r, according to an embodiment of the invention.
FIG. 3( a ) illustrates starting points for a tracking scheme according to an embodiment of the invention.
FIG. 3( b ) illustrates the role of the normalized radius image, according to an embodiment of the invention.
FIG. 4 depicts views of two patients showing results for both the left and right trees, according to an embodiment of the invention.
FIGS. 5( a )-( b ) compare depict a vessel tree segmented by a method according to an embodiment of the invention with a manually segmented ground truth vessel tree.
FIGS. 6( a )-( b ) compare depict a vessel tree segmented by a method according to an embodiment of the invention with a manually segmented ground truth vessel tree.
FIGS. 7( a )-( b ) compare depict a vessel tree segmented by a method according to an embodiment of the invention with a manually segmented ground truth vessel tree.
FIGS. 8( a )-( b ) compare depict a vessel tree segmented by a method according to an embodiment of the invention with a manually segmented ground truth vessel tree.
FIG. 9 is a block diagram of an exemplary computer system for implementing a method for segmentation of vascular structures in volumetric image datasets, according to an embodiment of the invention.
FIG. 10 presents tables of test results of a coronary artery centerline tracking method according to an embodiment of the invention on sixteen datasets as compared with manually annotated results.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
Exemplary embodiments of the invention as described herein generally include systems and methods for segmentation of vascular structures in volumetric image datasets. Accordingly, while the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. It should be understood, however, that there is no intent to limit the invention to the particular forms disclosed, but on the contrary, the invention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
As used herein, the term “image” refers to multi-dimensional data composed of discrete image elements (e.g., pixels for 2-D images and voxels for 3-D images). The image may be, for example, a medical image of a subject collected by computer tomography, magnetic resonance imaging, ultrasound, or any other medical imaging system known to one of skill in the art. The image may also be provided from non-medical contexts, such as, for example, remote sensing systems, electron microscopy, etc. Although an image can be thought of as a function from R 3 to R, the methods of the inventions are not limited to such images, and can be applied to images of any dimension, e.g., a 2-D picture or a 3-D volume. For a 2- or 3-dimensional image, the domain of the image is typically a 2- or 3-dimensional rectangular array, wherein each pixel or voxel can be addressed with reference to a set of 2 or 3 mutually orthogonal axes. The terms “digital” and “digitized” as used herein will refer to images or volumes, as appropriate, in a digital or digitized format acquired via a digital acquisition system or via conversion from an analog image.
A flowchart of a vessel segmentation method according to an embodiment of the invention is presented in FIG. 1 . A method begins at step 100 by extracting a subregion of the image containing a vessel of interest, either semi-automatically, starting from a user supplied seed point, or automatically. Then, a two-stage Hough-like election scheme is applied to the volume which enhances axial symmetries. In a first stage, the image is convolved with a gradient and each point votes on the vessel center. At step 101 , votes are cast in a conical region (with the tip of the cone on the point and its central axis oriented in the gradient direction). The votes are weighted proportional to the intensity of the gradient at the point and how close it is to the central axis of the cone. This creates the “standard Hough” image. In the same manner, a “radius Hough” image is also created at step 102 . That is, instead of each vote being a simple weighted yes/no, the weighted radius (the distance between the point and the vote) is recorded. The sum of the weights is additionally recorded at step 103 so that the “radius Hough” image can be scaled at step 104 to a “normalized radius Hough” image.
In a second stage, agreement is sought between the “standard Hough” and the “normalized radius Hough” images in a second round of voting. For each point in the volume, a same conical region of interest as before is used, and the “standard Hough” image is searched at step 105 for the most popular location within the region, the centerpoint candidate. If, at step 106 , the distance to the centerpoint candidate from the point is in agreement with the value for this location in the “normalized radius Hough” image, the candidate receives a vote. The resulting Hough is normalized at step 107 to form the Axial Symmetry Image.
Finally, at step 108 , a graph is formed based on the subregion. At step 109 , a mincut algorithm is applied to segment the vessel within the subregion. Intersections of the segmentation with the subregions's boundaries are detected at step 110 , and can serve as starting points for another iteration, returning to step 100 to extract a new subregion. A graph can also be constructed from the Axial Symmetry Image and searched for an optimal path from a user supplied endpoint to any point on the aorta surface (an ostium) to recover the vessel of interest.
Each of these steps is described in detail below.
Methods
A semi-automatic subregion extraction, step 100 of FIG. 1 , starts with a user supplied seed point and classification of the target vessel in one of three size categories (coronary, carotid or aorta). A cubic subregion, I({right arrow over (x)}), of the image centered on this seed is extracted. The size of the subregion,
x i = [ - d 2 , d 2 ] , i = 0 , 1 , 2 ,
is dependent on the vessel category, as the aorta requires a larger subregion than the coronaries.
An aorta subregion can be automatically extracted as follows. First, an aorta mask, T({right arrow over (x)}), is extracted automatically from the image volume by first finding the left ventricle. A fast variant of the isoperimetric algorithm is used for only segmenting a mask. The mask in this case can be generated by finding a connected component of voxels with intensities crossing a threshold. This threshold was computed using an initial point given inside the aorta. The initial point in the aorta was determined based on spatial and intensity priors relative to left ventricle segmentation. Note that, in other embodiments of the invention, the initial point could be user supplied. The left ventricle was also segmented using the variant of the isoperimetric algorithm, with an initial point given by searching for bright circular regions at the orientation commonly assumed by the left ventricle. This procedure for segmenting the aorta and left ventricle produced a correct segmentation in all test datasets.
Next, three separate images of the same dimensions as the subregion I({right arrow over (x)}) above are created. These are: a vote image, V({right arrow over (x)}), for storing the votes cast for vessel centerpoints, a radius image. R({right arrow over (x)}), for computing the expected vessel cross-sectional radii, and Σ({right arrow over (x)}), a sum image which will be used to normalize the radius image. To collect the votes, the image, I({right arrow over (x)}), is convolved with a cone-shaped kernel.
FIGS. 2( a )-( b ) illustrate conical voting kernels, according to an embodiment of the invention. FIG. 2( a ) shows a kernel, based at the point {right arrow over (x)}, having angular extent α max and oriented in the direction of the image gradient
∇ I ( x -> ) ∇ I ( x -> )
with a maximal height, h. The values of h and α max may be determined empirically. A point {right arrow over (v)} lies within the voting region. According to an embodiment of the invention, the gradient direction is used for performance reasons to orient the cone. However, in other embodiments of the invention, the direction could come from the two eigenvalues associated with the two largest eigenvectors of the Hessian matrix at {right arrow over (x)}.
Point {right arrow over (v)}, within the cone may be described with respect to {right arrow over (x)} as:
v -> = Θ -> ( ∇ I ( x -> ) ∇ I ( x -> ) ) [ r cos ( θ ) sin ( α ) , r sin ( θ ) sin ( α ) , r cos ( θ ) ] T , ( 1 )
where
Θ -> ( ∇ I ( x -> ) ∇ I ( x -> ) )
is a rotation matrix aligning the central axis of the cone, {right arrow over (Z)}, with the image gradient direction; α:[−α max ,α max ] is the angle {right arrow over (v)} forms with the image gradient vector;
r : [ 0 , h cos ( α max ) ] ,
is the length of the vector, {right arrow over (v)}; and θ:[0,2π] serves as a sweep out parameter. These parameters form the conical region,
C
(
x
->
α
max
,
h
,
∇
I
(
x
->
)
∇
I
(
x
->
)
)
.
The kernel K weights a point, {right arrow over (v)}, by
K ( v -> ( r , α ) ) = exp ( - α 2 / 2 σ 2 ) r cos ( α ) , ( 2 )
where σ is determined empirically. Since it is assumed that a shortest line segment from the centerpoint of the vessel to the vessel wall is perpendicular to the vessel wall, this weight function penalizes angles deviating from the gradient. Also, the larger the radius, the more pixels there are to vote for that centerpoint. The
1 r cos ( α )
term compensates for this effect.
Voting comprises a two stage process. A first stage, step 101 , begins by initializing the vote, radius, and sum images: V({right arrow over (x)})=0, ∀{right arrow over (x)}, R({right arrow over (x)})=0, ∀{right arrow over (x)}, Σ({right arrow over (x)})=0, ∀{right arrow over (x)}. Then, for each {right arrow over (x)} in I({right arrow over (x)}), the cone-shaped kernel is aligned with the image gradient,
I ( x -> ) I ( x -> ) ,
the cone is swept out, and the vote image is incremented with kernel values weighted by the log of the strength of the gradient at {right arrow over (x)}:
V ( {right arrow over (x)}+{right arrow over (v)} )= V ( {right arrow over (x)}+{right arrow over (v)} )+ K ( {right arrow over (v)} )log(|∇ I ( {right arrow over (x)} )|), (3)
where
( - d 2 , - d 2 , - d 2 ) ≤ ( x → + v → ) ≤ ( d 2 , d 2 , d 2 ) .
In this way, each voxel casts multiple votes for where the centerpoint of the vessel is. On the vessel wall, voxels will cast their votes for a centerpoint which is in the direction (more or less) of the image gradient. Since the image gradient is strong those votes will have stronger weights. In a similar fashion, at step 102 , votes are collected for the approximate radius of the vessel:
R ( {right arrow over (x)}+{right arrow over (v)} )= R ( {right arrow over (x)}+{right arrow over (v)} )+ K ( {right arrow over (v)} )| {right arrow over (v)}−{right arrow over (x)}|. (4)
FIG. 2( b ) is a view of the vessel cross-section with radius {right arrow over (r)}. Voxels are shown voting for a centerpoint of the vessel. The gray region 21 contains the most popular candidates. In the corresponding radius image, R({right arrow over (x)}), point {right arrow over (a)}, receives weighted increments of value r for all three points {right arrow over (x)} 1 , {right arrow over (x)} 2 ,{right arrow over (x)} 3 . At point {right arrow over (b)}, on the other hand, the weighted increments will be different from r: less r than for {right arrow over (x)} 2 and {right arrow over (x)} 3 , greater than r for {right arrow over (x)} 1 .
At step 103 , the sum of the weights is stored in Σ({right arrow over (x)}) for normalization:
Σ( {right arrow over (x)}+{right arrow over (v)} )=Σ( {right arrow over (x)}+{right arrow over (v)} )+ K ( {right arrow over (v)} ) (5)
Finally, at step 104 , the radius image is divided by the sum image Σ({right arrow over (x)}) to create a normalized radius image R′({right arrow over (x)}).
A second stage begins by initializing a second vote image, V′({right arrow over (x)}) to zero: V′({right arrow over (x)})=0, ∀{right arrow over (x)}. At step 105 , for each {right arrow over (x)} in V({right arrow over (x)}), one finds the voxel, {right arrow over (v)} max , which has the maximum number of votes within the cone-shaped region emanating from {right arrow over (x)}:
v → max = { v → i : V ( x → + v → i ) ≥ V ( x → + v → ) , ∀ v → ∈ C ( x → , α max , h , ∇ I ( x → ) ∇ I ( x → ) ) } ( 6 )
If, at step 106 , the distance between {right arrow over (x)} and {right arrow over (v)} max , is approximately equal to the normalized radius image value for that point, |R′({right arrow over (v)})−∥{right arrow over (v)} max −{right arrow over (x)}∥|<ε 1 for a positive ε 1 ≈0, then a vote is cast for it in the second vote image:
V ′( {right arrow over (x)}+{right arrow over (v)} max )= V ′( {right arrow over (x)}+{right arrow over (v)} max )+ K ( {right arrow over (v)} max )log(|∇ I ( {right arrow over (x)} )|). (7)
FIG. 3( b ) illustrates the role of the normalized radius image, R′({right arrow over (x)}). Although the point shown will have several votes from the gradient edges in the first vote image, each edge corresponds to a different radius in R′({right arrow over (x)}). This point will not be selected as a centerpoint. Once all votes are tallied, V′({right arrow over (x)}) is normalized at step 107 by dividing by Σ({right arrow over (x)}) to form an axial symmetry image, A({right arrow over (x)}). High values in A({right arrow over (x)}) indicate increased likelihood of a point being a centerpoint.
The subregion I({right arrow over (x)}) is next formulated at step 108 as an undirected graph where voxels, {right arrow over (x)}, correspond to nodes pεP. A 26-connected neighborhood system N of edges, E comprising pairs {p,q}εN connects these nodes. Two additional nodes, {s,t} representing source and sink respectively are included and linked to the nodes pεP forming edges E s,t . A labeling, f, is sought distinguishing vessel (f=1) from non-vessel (f=0) on the graph which minimizes an energy of the form:
E ( f ) = ∑ p ∈ P D p ( f p ) + ∑ p , q ∈ N V p , q ( f p , f q ) . ( 8 )
The V p,q term represents the consistency between neighboring nodes p, q (n-links):
V p , q , ∈ N = C 1 exp ( ( ( I ( p ) - I ( q ) ) 2 + cos - 1 ( ∇ I ( p ) ∇ I ( p ) · ∇ I ( q ) ∇ I ( q ) ) ) 2 σ 2 ) , ( 9 )
penalizing the differences in intensity and gradient direction. The D p term represents the confidence that a node should be labeled as vessel (t-links):
D p =C 2 A ( p ) for { p,s}εE s,t ; (10a)
and D p =C 2 (1 −A ( p )) for { p,t}ε=E s,t . (10b)
The constants C 1 and C 2 may be determined empirically.
At step 109 , to find the globally optimal partitioning of the graph, a maxflow/mincut algorithm is used. Exemplary maxflow/mincut algorithms include the well known Ford-Fulkerson algorithm, and its variants, such as the Edmonds-Karp algorithm. Segmentation can be accomplished in polynomial time as each node is connected only to its nearest neighbors.
Once the vessel is segmented within the subregion, the intersections between the segmentation and the subregion boundaries are detected at step 110 . In image coordinates, this is
X
s
=
{
x
→
f
=
1
❘
(
x
i
=
d
2
)
⋂
(
x
i
=
d
2
)
,
i
∈
0
,
1
,
2
}
.
(
11
)
A connected component analysis is performed on X s and components with size above a threshold are designated as vessel endpoints. These endpoints serve as seeds for extracting a new subregion in a next iteration of the segmentation, returning to step 100 . Each successive new subregion serves to track the vessel's path. FIG. 3( a ) illustrates a tracking scheme for an algorithm according to an embodiment of the invention, where intersections of the segmentation with the subregion boundaries define new starting points.
For aorta extraction, a graph G={V, E} is created based on the axial symmetry image A({right arrow over (x)}) which will be searched to find the aorta. The vertices V={B,H,U} are: B={{right arrow over (x)}:∇T({right arrow over (x)})>ε 2 }, the aorta surface points, where T({right arrow over (x)}) is the aorta mask; H={{right arrow over (x)}:A({right arrow over (x)})>ε 3 }, the axial symmetry voxels over a threshold; and U={{right arrow over (u)}}, a user supplied distal endpoint. The thresholds ε 2 , ε 3 may be determined empirically from the aorta. The edges, E, are created between any two vertices which are less than or equal to a predetermined distance apart in world coordinates, to facilitate bridging occlusions shorter than that length. According to an embodiment of the invention, this predetermined distance is about 2 centimeters. Edge weights are computed as the line integral (again in world coordinates) between two vertices through the multiplicative inverse of the axial symmetry volume,
w ( E ij ) = ∫ C ij 1 A ′ ( s ) ⅆ s , ( 12 )
where C ij is the line segment connecting vertex v i and v j .
According to an embodiment of the invention, Dijkstra's algorithm for finding a shortest path between 2 nodes on a graph is applied on G starting from {right arrow over (u)}, the user supplied endpoint, to any point on the aorta surface to recover the vessel of interest. The point on the aorta will be an ostium if the segmentation is correct. It is to be understood that the use of Dijkstra's algorithm is exemplary and non-limiting, and any algorithm for finding a shortest path between 2 nodes on a graph is within the scope of an embodiment of the invention.
Results
A vessel segmentation algorithm according to an embodiment of the invention was validated on 70 coronary trees (left and right), using coronary CT angiography datasets from 35 patients, with seeds placed at the ostium of the Left Main and Right Coronary Arteries. Exemplary parameters for this embodiment were: subregion size=48×48×48, α max =π/10, h=4 mm, σ=32, C 1 =10, C 2 =200. All vessels were manually segmented by experts for ground truth comparisons. Algorithms according to embodiments of the invention were tested on all vessels of radius greater than 0.6 mm. The sensitivity was 90.1%±9.3% (mean±standard deviation), i.e., on average ˜90% of the voxels labeled as ground truth were detected, while the positive predictive value was 95.4%±7.6%, i.e., ˜95% of vessel voxels were correctly classified. FIG. 4 presents exemplary views from two patients showing results for both the left and right trees. FIGS. 5( a )-( b ), FIGS. 6( a )-( b ), FIGS. 7( a )-( b ), and FIGS. 8( a )-( b ) each depict a vessel tree segmented by a method according to an embodiment of the invention in the (a) view, and a manually segmented ground truth vessel tree in the (b) view. Average execution time was 95 s using a dual core 2.6 Ghz CPU, with 2 gigabytes of RAM. This execution time is relatively fast because the axial symmetry calculation is only performed on the small cubical subregion extracted in a first step of a method according to an embodiment of the invention. The vessel is tracked from the initial subregion, and subsequent small cubical subregions are extracted as the vessel is tracked. Thus, only a small fraction of an entire image is processed.
An axial symmetry based vessel extraction algorithm when applied to a whole image volume is computationally expensive. In this case, an automatic cardiac extraction algorithm can be applied to isolate the heart. Then, the image volume is subdivided into sub-cubes. Any cube which contains some part of the heart is included in the processing. Even so, the creation of the axial symmetry image typically takes up to five minutes. Once this is calculated, however, extraction of a vessel, once an endpoint is selected, can be performed in a few seconds.
A coronary artery centerline tracking method according to an embodiment of the invention can be compared to manually annotated centerlines in cardiac CTA datasets. For this purpose, the centerline of a coronary artery in a CTA scan may be defined as the curve that passes through the center of gravity of the lumen in each cross-section of an image volume. The start point of a centerline is defined as the center of the coronary ostium (i.e. the point where the coronary artery originates from the aorta) and the end point as the most distal point where the artery is still distinguishable from the background. The centerline is smoothly interpolated if the artery is partly indistinguishable from the background, e.g. in case of a total occlusion or imaging artifacts.
The CTA data used for the comparison was acquired in the Erasmus MC, University Medical Center Rotterdam, The Netherlands. Thirty-two datasets were randomly selected from a series of patients who underwent a cardiac CTA examination between June 2005 and June 2006. Twenty datasets were acquired with a 64-slice CT scanner and twelve datasets with a dual-source CT scanner (Sensation 64 and Somatom Definition, Siemens Medical Solutions, Forchheim, Germany).
FIG. 10 presents 2 tables of test results of a coronary artery centerline tracking method according to an embodiment of the invention on sixteen datasets as compared with manually annotated results. The upper table presents several overlap and accuracy measurement results for each of the datasets, and the lower table presents summary results for each measurement. The overlap and accuracy measures are explained next.
Quality measures for extracted centerlines are based on a labeling of points on the centerlines as true positive, false negative or false positive. This labeling, in turn, is based on a correspondence between the reference standard annotated centerline and an evaluated centerline. A point of the reference standard is marked as true positive TPR ov , if the distance to at least one of the connected points on the evaluated centerline is less than the annotated radius and false negative FN ov otherwise. A point on the evaluated centerline is marked as true positive TPM ov if there is at least one connected point on the reference standard at a distance less than the radius defined at that reference point, and it is marked as false positive FP ov otherwise.
Three different overlap measures are used.
Overlap (OV) represents the ability to track the complete vessel annotated by the human observers. It is defined as:
OV
=
TPM
ov
+
TPR
ov
TPM
ov
+
TPR
ov
+
FN
ov
+
FP
ov
.
Overlap until first error (OF) determines how much of a coronary artery has been extracted before making an error. It is defined as the ratio of the number of true positive points on the reference before the first error (TPR of ) and the total number of reference points (TPR of +FN of ):
OF = TPR of TPR of + FN of .
The first error is defined as the first FN ov , point when traversing from the start of the reference standard to its end while ignoring false negative points in a beginning segment of the reference standard. The threshold for the beginning segment is based on the average diameter annotated at the beginning of all the reference standard centerlines.
Overlap with the clinically relevant part of the vessel (OT) gives an indication of how well the method is able to track a section of the vessel that is assumed to be clinically relevant. The point closest to the end of the reference standard with a radius larger than or equal to predetermined threshold is determined. Only points on the reference standard between this point and the start of the reference standard are taken into account and only points on the (semi-)automatic centerline connected to these reference points are used when defining the true positives (TPM ot and TPR ot ), false negatives (FN ot ) and false positives (FP ot ). The OT measure is calculated as follows:
OT
=
TPM
ot
+
TPR
ot
TPM
ot
+
TPR
ot
+
FN
ot
+
FP
ot
.
Three different measures are used to assess the accuracy of coronary artery centerline extraction algorithms.
Average distance (AD) is the average distance between the reference standard and the automatic centerline. The average distance is defined as the summed length of all the connections between the two equidistantly sampled centerlines, divided by the number of connections.
Average distance inside vessel (AI) represents the accuracy of centerline extraction, provided that the evaluated centerline is inside the vessel. The measure is calculated in the same way as AD, except that connections that have a length larger than the annotated radius at the connected reference point are excluded.
Average distance to the clinically relevant part of a vessel (AT) represents how well the method can track vessels segments that are clinically relevant. The difference with the AD measure is that the lengths and scores for the connections that connect TPM ot , TPR ot , FN ot , and FP ot points are averaged.
System Implementations
It is to be understood that embodiments of the present invention can be implemented in various forms of hardware, software, firmware, special purpose processes, or a combination thereof. In one embodiment, the present invention can be implemented in software as an application program tangible embodied on a computer readable program storage device. The application program can be uploaded to, and executed by, a machine comprising any suitable architecture.
FIG. 9 is a block diagram of an exemplary computer system for implementing a method for segmentation of vascular structures in volumetric image datasets according to an embodiment of the invention. Referring now to FIG. 9 , a computer system 91 for implementing the present invention can comprise, inter alia, a central processing unit (CPU) 92 , a memory 93 and an input/output (I/O) interface 94 . The computer system 91 is generally coupled through the I/O interface 94 to a display 95 and various input devices 96 such as a mouse and a keyboard. The support circuits can include circuits such as cache, power supplies, clock circuits, and a communication bus. The memory 93 can include random access memory (RAM), read only memory (ROM), disk drive, tape drive, etc., or a combinations thereof. The present invention can be implemented as a routine 97 that is stored in memory 93 and executed by the CPU 92 to process the signal from the signal source 98 . As such, the computer system 91 is a general purpose computer system that becomes a specific purpose computer system when executing the routine 97 of the present invention.
The computer system 91 also includes an operating system and micro instruction code. The various processes and functions described herein can either be part of the micro instruction code or part of the application program (or combination thereof) which is executed via the operating system. In addition, various other peripheral devices can be connected to the computer platform such as an additional data storage device and a printing device.
It is to be further understood that, because some of the constituent system components and method steps depicted in the accompanying figures can be implemented in software, the actual connections between the systems components (or the process steps) may differ depending upon the manner in which the present invention is programmed. Given the teachings of the present invention provided herein, one of ordinary skill in the related art will be able to contemplate these and similar implementations or configurations of the present invention.
While the present invention has been described in detail with reference to a preferred embodiment, those skilled in the art will appreciate that various modifications and substitutions can be made thereto without departing from the spirit and scope of the invention as set forth in the appended claims. | A method for segmenting tubular structures in digital medical images includes extracting a subregion from a 3-dimensional (3D) digital medical image volume containing a vessel of interest, identifying potential vessel centerpoints for each voxel in the subregion by attaching to each voxel a tip of a 3D cone that is oriented in the direction of the voxel's image gradient and having each voxel within the cone vote for those voxels most likely to belong to a vessel centerline, selecting candidates for a second vote image that are both popular according to a first vote image, as well as being consistently voted upon by a radius image, reconfiguring the subregion as a graph where each voxel is represented by a node that is connected to 26 nearest neighbors by n-link edges, and applying a min-cut algorithm to segment the vessel within the subregion. | 6 |
PRIORITY
This application is a continuation in part of U.S. patent application Ser. No. 12/077,430, filed Mar. 19, 2008, titled “Modular Utility Light,” which was issued on Dec. 22, 2009 as U.S. Pat. No. 7,635,208, the disclosure of which is incorporated herein by reference, which claims priority of U.S. Provisional Patent Application Ser. No. 60/919,265, filed Mar. 21, 2007, titled “Modular Utility Light,” the disclosure of which is incorporated herein by reference.
TECHNICAL FIELD
Embodiments of the present invention relate to an improved hand held utility light. More particularly embodiments relate to a modularly constructed handle for the utility light which allows for design of individual hand hold configurations, as requested by given customers, without the need for separate UL testing and approval for each individually configured light.
BACKGROUND
Hand held utility lights may comprise two half-shells which when assembled encapsulate therebetween the light bulb receptacle, the light on-off switch, and any other desired brass circuitry. For example see U.S. Pat. No. 5,833,357, issued to Ting on Nov. 10, 1998.
However, when manufacturing such utility lights for differing customers, each customer may require that the hand-hold portion of the utility light be uniquely different from their competitors. Thus manufacturing suppliers of such utility lights must individually submit each uniquely designed utility light for UL testing and approval even though the electrical portions of each utility light may be identical to that of previously approved utility lights.
In the event that a given customer desires to reconfigure their particular utility light handle, the entire newly configured utility light must be UL tested and approved even though the redesign is superficial and incorporates previously approved electrical components and circuitry.
Thus for manufacturers supplying multiple customers, such individual UL testing and approvals becomes costly and generally unnecessary.
BRIEF SUMMARY
A uniquely configured utility light is taught which may not require separate UL testing and approval when the overall appearance of the hand hold portion of the utility light is the only portion of the utility light that is reconfigured.
Embodiments of the present invention disclose a unique hand held utility light having a modular construction wherein the light includes an electrical module and a separately constructed hand hold module, thereby compressing a separate hand hold module connected to an electrical module to complete the light structure.
By this modular construction the utility light manufacturer need only submit the electrical module for UL testing and approval. Once UL tested and approved, the electrical module may be used with any uniquely designed hand hold module without separate UL testing and approval. Of the complete utility light
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 presents a pictorial view of a typical utility light embodying the present invention.
FIG. 2 presents an exploded pictorial view of the utility light illustrated in FIG. 1 .
FIG. 3 presents a detailed, exploded pictorial view illustrating the assembly of the lower portion of the utility light illustrated in FIG. 1 .
FIG. 4 presents a reverse and inverted pictorial view of FIG. 3 .
FIG. 5 presents a cross-sectional view taken along line 5 - 5 in FIG. 1 .
FIG. 6 presents a cross-sectional view taken along line 6 - 6 in FIG. 1 .
FIG. 7 presents a perspective view of an alternate embodiment of a utility light comprising an articulation mechanism.
FIG. 8 presents a detailed, cross-sectional front view of the lower portion of the utility light in FIG. 7 .
FIG. 9 presents an exploded assembly view of the articulation mechanism of the utility light in FIG. 7 .
FIG. 10 presents a perspective view of an alternate embodiment of a utility light comprising an alternate articulation mechanism.
FIG. 11 presents a detailed, cross-sectional front view of the lower portion of the utility light in FIG. 10 .
FIG. 12 presents an exploded assembly view of the articulation mechanism of the utility light in FIG. 10 .
FIG. 13 presents a perspective view of an alternate embodiment of a utility light comprising a storage strap.
FIG. 14 presents a detailed rear view of the lower portion of the utility light in FIG. 13 .
FIG. 15 presents a detailed side view of the lower portion of the utility light in FIG. 13 .
DETAILED DESCRIPTION
FIG. 1 illustrates a utility light 10 comprising a handle module 12 , an electrical module 14 , and a cord 22 . As illustrated in FIGS. 2 , 3 and 4 handle module 12 comprises half shells 12 A and 12 B that when placed together, as illustrated in FIG. 6 , and fastened with fasteners 15 , complete the assembly of handle module 12 .
Similarly, as illustrated in FIG. 2 , electrical module 14 comprises two opposing shells 14 A and 14 B that permanently, combine to form an outer housing for electrical module 14 . As illustrated, shells 14 A and 14 B, when assembled, encapsulate any desired brass electrical components 20 and the light bulb receptacle 25 .
When assembled electrical module 14 includes a cylindrical shaped extension 18 which receives thereon handle shells 12 A and 12 B thereby forming the completed utility light as illustrated in FIG. 1 . Post like protrusions 23 A and 23 B extend through an opening in extension 18 , as illustrated in FIGS. 3 and 4 , and are fastened by a screw 15 . Two additional screws 15 extend through shell 12 B and cord lock 22 B, within shell 12 B, and are received within cord lock 22 A inside shell 12 A as illustrated in FIGS. 2 , 3 and 4 .
Shells 12 A and 12 B, when assembled, further inter lock with extension 18 of electrical module 14 as illustrated in FIG. 5 .
Once the electric module 14 has been designed, tested, and approved by UL, the module 14 may be joined with various handle configurations, thereby forming utility lights of various appearances and designs without undergoing individual UL testing and approval.
By way of example only, FIGS. 7-14 depict various embodiments of alternate handle module configurations that may be joined with electric module 14 . Specifically, FIGS. 7-12 depict two different handle modules, each comprising an articulation mechanism, and FIGS. 13-14 depict a handle module comprising a strap 350 and locking mechanism 360 .
As shown in FIGS. 7-9 , handle module 112 comprises a first half shell 112 a , a second half shell 112 b and an articulation mechanism 150 . In this version, handle module 112 is configured to provide a side entry aperture 124 to receive cord 122 within handle module 112 . Of course the side entry aperture 124 may be positioned on either side of handle module 112 . As shown, articulation mechanism 150 comprises a ball and socket joint comprising a socket 114 formed by first half shell 112 a and second half shell 112 b and a base assembly 160 . In this example, base assembly 160 comprises a sphere 162 and a support portion 164 . The components of base assembly 160 may be configured to interlock with each other to provide a secure attachment between the components, although other suitable methods of construction may be utilized in place of or in addition to the interlocking design. Sphere 162 may comprise two spherical halves 162 a , 162 b , as shown in FIG. 9 , or, alternatively, sphere 162 may have a unitary or other suitable construction. Socket 114 may be sized and shaped to receive at least a portion of sphere 162 such that upon assembly utility light 110 may be rotated about base assembly 160 in at least one direction. Because utility light 110 is rotatable, a user can manipulate the direction of the light provided by utility light 110 to illuminate a desired area.
As shown, the bottom of support portion 164 comprises a hexagonal shape. By way of example only, the bottom of support portion 164 may be hexagonal, square, circular, triangular, or have any other suitable shape. Of course, support portion 164 may be any suitable shape and size depending on the particular application intended by the user. Support portion 164 may be configured to provide adequate support to allow utility light 110 to be placed in a vertical orientation on a support surface. In the illustrated version, support portion 164 further comprises a magnet 166 which may be of sufficient shape, size, and strength to allow utility light 110 to be releasably mounted to a support surface, such as a metal surface, in any desired orientation. Alternatively, support portion 164 may comprise an adhesive instead of a magnet to allow utility light 110 to be fixedly or releasably attached to any suitable support surface in any desired orientation. Of course, neither the magnet nor the adhesive is required.
In the embodiment shown in FIGS. 10-12 , handle module 212 comprises first half shell 212 a , a second half shell 212 b and an articulation mechanism 250 . Similar to the embodiment shown in FIGS. 7-9 , handle module 212 is configured to provide a side entry aperture 224 to receive cord 222 within handle module 212 . Of course, side entry aperture 224 may be positioned on either side of handle module 212 . As shown in FIGS. 10-12 , articulation mechanism 250 comprises a base assembly 260 that includes both a ball and socket joint 270 and a ratcheting mechanism 280 . In the illustrated embodiment, ball and socket joint 270 and ratcheting mechanism 280 of articulation mechanism 250 provide two discrete pivot points or points of rotation. Of course, the ball and socket joint is not required, and an alternate embodiment (not shown) may comprise an articulation mechanism that includes a ratcheting mechanism engaged with the handle module without a ball and socket joint. Base assembly 260 further comprises a support portion 264 . The components of base assembly 260 may be configured to interlock with each other to provide a secure attachment between the components, although other suitable methods of construction may be utilized in place of or in addition to the interlocking design. In this example, ball and socket joint 270 comprises a sphere 262 and a socket 214 formed by first half shell 212 a and second half shell 212 b . Sphere 262 may comprise two spherical halves 262 a , 262 b , as shown in FIG. 12 , or, alternatively, sphere 262 may have a unitary or other suitable construction. Socket 214 may be sized and shaped to receive at least a portion of sphere 262 such that, upon assembly, utility light 110 may be rotated about base assembly 260 in at least one direction. Ratcheting mechanism 280 may comprise any suitable ratcheting device known to those skilled in the art. Ratcheting mechanism 280 may comprise two substantially spherical halves 280 a , 280 b , as shown in FIG. 12 , or, alternatively, ratcheting mechanism 280 may have a unitary or other suitable construction. In the illustrated embodiment, ratcheting mechanism 280 is positioned between sphere 262 and support portion 264 , although other arrangements may be apparent to those of ordinary skill in the art. Ratcheting mechanism 280 may be configured to provide an additional range of motion for adjusting the orientation of utility light 210 . Because utility light 210 is rotatable due to ball and socket joint 270 and further adjustable due to ratcheting mechanism 280 , a user can manipulate the direction of the light provided by utility light 210 to illuminate a desired area.
As shown, the bottom of support portion 264 comprises a circular shape. By way of example only, the bottom of support portion 264 may be hexagonal, square, circular, triangular, or have any other suitable shape. Support portion 264 may be any suitable shape and size depending on the particular application intended by the user. Support portion 264 may be configured to provide adequate support to allow utility light 210 to be placed in a vertical orientation on a support surface. In the illustrated version, support portion 264 further comprises a magnet 266 which may be of sufficient shape, size, and strength to allow utility light 210 to be releasably mounted to a support surface, such as a metal surface, in any desired orientation. Alternatively, support portion 164 may comprise an adhesive instead of a magnet to allow utility light 210 to be fixedly or releasably attached to any suitable support surface in any desired orientation. Of course, neither the magnet nor the adhesive is required.
FIGS. 13-14 depict a handle module 312 comprising a first half shell 312 a , a second half shell 312 b , and a strap 320 . In the illustrated embodiment, strap 320 comprises a fixed end 322 and a free end 324 . Fixed end 322 is attached to handle module 312 , and free end 324 is configured to be inserted into a slot 314 formed by first half shell 312 a and second half shell 312 b . It will be appreciated that the slot may be formed entirely within either first half shell 312 a or second half shell 312 b or formed jointly by both first half shell 312 a and second half shell 312 b (as shown in FIGS. 13-14 ). Upon insertion into slot 314 , free end 324 may be releasably engaged by a locking mechanism 330 . Locking mechanism 330 may comprise a rotating friction lock or any other device configured to adequately secure free end 324 . Locking mechanism 330 is configured to transition between an engaged configuration and a released configuration. When free end 324 is inserted into slot 314 and locking mechanism 330 is placed in the engaged configuration, then free end 324 is fixedly engaged with locking mechanism 330 and free end 324 may not be removed. When free end 324 is inserted into slot 314 and locking mechanism is placed in the released configuration, then free end 324 is releasably engaged with locking mechanism 330 and free end 324 may be removed from slot 314 . When strap 322 is in the loop configuration, as shown in FIG. 14 , strap 322 may be used to help manage or store the power cord 340 . Alternatively, a user may hang utility light 310 in an inverted orientation above or adjacent to a work area by placing strap 322 in the loop configuration and placing the loop around a support member.
Although a specific embodiment of the invention has been disclosed, there is no intent to thereby limit the invention to the specific embodiment illustrated herein. On the contrary, the intention herein is to cover all modifications, alternatives, embodiments, and/or equivalents of the subject invention as may fall within the spirit and scope of the invention as disclosed. | A modularly constructed hand held, utility light is described and taught having a sealed electrical module and a separately attached handle module. In one embodiment. module includes two half shells that when assembled and attached to the electric module. Various embodiments of the handle module may comprise an articulation mechanism configured to allow the user to manipulate the direction of the light provided by the utility light by rotating the utility light in at least one direction. The articulation mechanism may comprise one or more of a ball and socket joint, a ratchet mechanism, or any other suitable device configured to allow a user to manipulate the direction of the light provided by the modular utility light. In another embodiment, the handle module may comprise a strap configured to facilitate cord management and/or allow a user to hang the modular utility light above a work area. | 5 |
FIELD OF THE INVENTION
The present invention relates generally to a toilet flushing mechanism that allows a user to chose between a partial flush and a full flush. In particular, the present invention relates to a dual flushing assembly having two concentric handles operable to either partially or fully flush a toilet.
BACKGROUND OF THE INVENTION
Water conservation is becoming increasing more important. A significant source of water consumption is the water used in flushing toilets. As is well known in the art, several problems and difficulties are encountered in providing suitable means for flushing controlled amounts of water from a toilet water tank.
One of the most common flushing apparatuses in use today utilizes a ball cock supply valve that controls the inlet of water into the toilet tank. A buoyant float ball is connected to the ball cock by means of a trip lever and as the toilet tank is filled with water, the buoyant ball rises. The upward motion of the buoyant ball is transmitted to the ball cock supply valve through the trip lever until, at a predetermined water level, the ball cock shuts off the water inlet to the toilet tank. In most toilets, the water level in the tank may be adjusted by means of a screw-set mechanism located in the ball cock supply valve. Once the water level in the tank is set, further adjustment is not required and a consistent volume of water will be discharged each time the toilet is flushed.
In addition to the ball cock supply valve, a second valve means is needed for controlling the flushing of the toilet, namely a flush valve. Typically the flush valve comprises a flapper that seals water into the toilet tank. When the trip lever or handle on the outside of the toilet tank is depressed to initiates the flush of the toilet, the trip lever activities a trip arm to lift the flapper and allow water to exit the tank into the toilet bowl for the flush cycle.
Finally, a tank refill tube is commonly integrated with the water supply valve and the flush valve to ensure that the toilet trapway refills with water after the flush is completed.
A flush valve mechanism for controlling the flushing action of water through the water outlet of a toilet tank is taught in U.S. Pat. No. 4,305,163. The valve taught in U.S. Pat. No. 4,305,163 is a dual activity flush valve having a float assist, the operation of which permits the complete drainage of the water in the tank for a full flush. The flush valve operates by means of a pair of lever arms whereby one arm operates to lift up a vertical tube for limited flushing and the other arm operates to lift both the vertical tube and an ancillary float assist that extends the opening time of the valve until the entire water volume is depleted. Such a valve system is manufactured by Plasson Maagan Michael Industries Ltd. (“Plasson”).
The present invention provides a dual flushing assembly comprising dual handles for use with currently available components such as conventional ball cock supply valves and flushing valves as taught in U.S. Pat. No. 4,305,163 and manufactured by Plasson. Thus, when one wishes to flush only liquid waste, one of the dual handles will be responsible for a partial flush and when one wishes to flush both solid and liquid waste, a second handle will operate to effect a full flush.
SUMMARY OF THE INVENTION
The present invention has been accomplished to provide a double trip handle type flush control assembly, which operates to allow either a full volume of water to be drawn out of the toilet tank or a partial volume of water to be drawn out of the tank. In particular, the double trip handle type flush control assembly of the present invention is adaptable for use in any size toilet tank. Further, the flush control assembly of the present invention has been adapted to accommodate a refill tube, which directs water from the ball cock valve into an overflow tube to refill the toilet trapway after flushing.
The present invention provides a dual flushing apparatus, mountable through an aperture in a wall of a toilet tank, for use with a dual flushing valve assembly comprising a vertical tube having a first float means attached thereto and a float assist arm having a second float attached thereto, said flushing apparatus comprising:
a rotatable first handle means comprising a first handle and a first shaft having an annulus therethrough; a rotatable second handle means comprising a second handle and a second shaft, said second shaft adapted to be slideably received in said annulus of said first shaft such that the second handle nests with the first handle; a first flush lever arm have two ends, a first end operably attached to said first shaft and a second end operably attached to said float assist arm; and a second flush lever arm having two ends, a first end operably attached to said second shaft and a second end operably attached to said vertical tube, said second end further having a bore therethrough and a nipple member in communication with said bore for attaching a refill tube such that when said second flush lever arm is operably attached to said vertical tube, said bore is directly over said vertical tube;
whereby said first flush lever arm supports said second flush lever arm such that when said second handle is depressed only said vertical tube is lifted for a partial flush but when said first handle is depressed both said vertical tube and said assist arm are lifted for a full flush.
In a preferred embodiment, the first flush lever and the second flush lever arm are adjustable in length so as to fit in any size toilet tank.
In another preferred embodiment, the first flush lever arm further comprises a first arm portion and a second arm portion, whereby each arm portions have male ends, and the second flush lever arm further comprises a first arm portion and a second arm portion, each arm portions having male ends. The male ends of the first and second arm portions of the first flush lever arm are interconnected by means of a first tube. The male ends of the first and second arm portions of said second flush lever arm are also interconnected by means of a second tube. The first and second tubes can be made in a variety of lengths, or can be of one length that can be cut to adapt to a particular size toilet tank.
In another preferred embodiment, the present invention provides a dual flushing apparatus comprising:
a rotatable first handle means comprising a first handle and a first shaft having an annulus therethrough; a rotatable second handle means comprising a second handle and a second shaft, said second shaft adapted to be slideably received in said annulus of said first shaft such that the second handle nests with the first handle; means for securing said second handle means to said first handle means; a first flush lever arm operably attached to said first shaft, said first flush lever arm having a first arm portion and a second arm portion and each arm portion having an annulus therethrough; a second flush lever arm operably attached to said second shaft, said second flush lever arm having a first arm portion and a second arm portion, each arm portion having an annulus therethrough; a first rod member for insertion into said annulus of said first and second arm portions of said first flush lever arm to interconnect said first and second arm portions; and a second rod member for insertion into said annulus of said first and second arm portions of said second flush lever arm to interconnect said first and second arm portions.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows the dual flushing apparatus of the present invention installed in a toilet tank.
FIG. 2 a is a perspective view of the dual flushing apparatus of the present invention.
FIG. 2 b is a side view of the dual flushing apparatus of the present invention.
FIG. 3 shows a perspective of the individual parts of the dual flushing apparatus and how they fit together.
FIG. 4 a is a perspective view of the dual flushing apparatus of the present invention showing the adjustable flush lever arms.
FIG. 4 b is a side view of the dual flushing apparatus of the present invention showing the adjustable flush lever arms.
DETAILED DESCRIPTION OF THE INVENTION
In FIG. 1 , an embodiment of the dual flushing assembly 10 of the present invention has been installed through a mounting hole 12 in a wall 14 of a toilet tank 16 . In addition to the dual flushing assembly 10 , the toilet tank 16 comprises a ball cock valve assembly 18 , a dual acting flush valve assembly 22 and a refill tube 20 , wherein one end of refill tube 20 is attached to ball cock valve assembly 18 and the other end is attached to flush valve assembly 22 . The dual acting flush valve assembly 22 is preferably constructed of a thermoplastic material and manufactured by Plasson.
Dual acting flush valve assembly 22 is used in place of conventional flush valves such as a flapper valve or ball type valve because it has been designed to either partially or fully release water from the tank into the toilet bowl, as the need arises. Dual acting flush valve assembly 22 comprises a water outlet valve 24 and a buoyant valve engaging assembly which assembly comprises a float assist 28 attached to one end of a float assist arm 30 . Float assist arm 30 further comprises a ring 40 attached to the opposite end from float assist 28 . Float assist arm 30 operates to release float assist 28 .
Water outlet valve 24 comprises vertical tube 25 having a toilet mounting means 70 at one end for mounting said dual flush valve assembly 22 to water outlet 34 . Vertical tube 25 further comprises a flushing valve seal 100 , which seals the water outlet valve when water outlet valve is not in the lifted position. When vertical tube 25 of the water outlet valve 24 is lifted, flushing valve seal 100 is also lifted thereby releasing water through water outlet 34 into the toilet bowl (not shown).
Vertical tube 25 further comprises an aperture 38 at the opposite end and a partial float 26 . In operation, dual acting flush valve assembly 22 releases a full tank of water when both the float assist arm 30 and vertical tube 25 are simultaneously lifted. However, when vertical tube 25 is lifted alone, only a partial amount of water is released from the tank. Dual acting flush valve assembly 22 is described in more detail in U.S. Pat. No. 4,305,163, incorporated herein by reference.
To ensure that the toilet trapway is refilled after flushing, refill tube 20 , having first end 102 and second end 104 is provided. First end 102 is connected to ball cock valve assembly 18 , which supplies water to refill tube 20 . Second end 104 of refill tube 20 is posited directly over flush valve assembly 22 for supplying water through vertical tube 25 and water outlet 34 .
Dual flushing assembly 10 of the present invention has been adapted to be used with such dual acting flushing valve assemblies as shown in FIG. 1 . One embodiment of dual flushing assembly 10 is illustrated in FIGS. 2 a and 2 b. FIG. 3 provides details of the interconnection of the various components of dual flushing assembly 10 . A rotatable first handle means 42 is provided, said first handle means 42 comprising a handle 72 (“first handle”) having a hollow shaft 76 (“first shaft”) at one end. End 78 of shaft 76 comprises a plurality of splines 80 arranged for mating with the correspondingly shaped hub 82 of first flush lever arm 46 . This ensures proper orientation of said first lever arm 46 relative to first handle means 42 .
A rotatable second handle means 44 , having a handle 84 (“second handle”) and a shaft 86 (“second shaft”), said shaft 86 located at one end of said handle 84 , is shown in FIGS. 2 a and 2 b with second shaft being inserted into first shaft such that second shaft is free to rotate concentrically within first shaft. Thus, second handle is resting on first handle to give the appearance of a single handle.
Shaft 86 further comprises a plurality of splines 88 at end 90 of shaft 86 , said splines 88 being discontinuous across the length of end 90 because of depressed ridge 92 , said ridge 92 being continuous around the circumference of shaft 86 . Splines 88 are arranged for mating with the correspondingly shaped hub 94 of second flush lever arm 48 .
FIGS. 2 a and 2 b show second handle means 44 nested within first handle means 42 . Retainer means 50 fittingly attaches to ridge 92 and is designed to ensure that first and second handle means remain nested. Retainer means 50 is shown in FIG. 3 as a simple clip, which clips over ridge 92 .
First flush lever arm 46 further comprises end 52 adapted to be mounted into ring 40 of float assist arm 30 as shown in FIG. 1 . First flush lever arm 46 is bent such that it is positioned beneath second flush lever arm 48 . Second flush lever arm 48 further comprises end 54 adapted to penetrate aperture 38 of vertical tube 25 of water outlet valve 24 as shown in FIG. 1 .
Second flush lever arm 48 further comprises a bore 98 therethrough and nipple 96 , said nipple adapted to snugly receive refill tube 20 as shown in FIG. 1 . As previously mentioned, first end 102 of refill tube 20 is connected to ball cock valve assembly 18 and second end 104 of refill tube 20 is posited directly over the vertical tube 25 of dual acting flush valve assembly 22 for supplying water through vertical tube 25 and water outlet 34 . In the prior art, the refill tube had an elbow tube connected at its end, and said elbow tube simply hooked to the lip of the vertical tube of a dual acting flush valve assembly. However, such an attachment means of the refill tube to the vertical tube proved to be unsatisfactory as the refill tube was constantly being “knocked off” the lip of the vertical tube. As well, the movement of the vertical tube of the dual flush valve assembly, in response to the movement of the second flush lever arm is partially restricted due to the pull or drag of the elbow tube on the refill tube.
In the present invention, second end 104 of refill tube 20 snugly attaches on to nipple 96 located at end 54 of second flush lever arm 48 such when end 54 penetrates aperture 38 of vertical tube 25 , bore 98 and nipple 96 are located directly over the opening 106 of vertical tube 25 . Once bore 98 and nipple 96 are positioned directly over opening 106 , refill tube 20 can be fitted thereon to supply water through vertical tube 25 and through water outlet 34 in order to refill the toilet trapway (not shown) once flushing has occurred. Thus, by snugly fitting the refill tube 20 on second flush lever arm 48 , refill tube 20 will be less likely to be knocked off, and will always be positioned directly above the vertical tube. Further, by being positioned on the second flush lever arm 48 , there is no drag or pull on vertical tube 25 .
In a preferred embodiment first and second flush lever arms 46 and 48 are adjustable in length. Such adjustability is desirable due to the variety of different tank sizes and shapes on the market today. Adjustability is achieved in a preferred embodiment as follows.
With reference now to FIGS. 4 a and 4 b, first flush lever arm 46 is comprised of two separate sections 58 and 60 , each having male ends 66 and 67 , respectively. Tube 36 , which can be made in any length, or, in the alternative, can be cut to any length, snugly fits over male ends 66 , 67 of sections 58 and 60 , thereby connecting the two sections 58 and 60 to form a contiguous arm. Similarly, second flush lever arm 48 is comprised of two separate sections 62 and 64 , each having male ends 68 and 69 , respectively. Tube 56 , which again can be made in any length or cut to any length, snugly fits over male ends 68 , 69 of sections 62 and 64 to form a contiguous arm.
In an alternative embodiment (not shown), each arm section could have an annulus partially therethrough and a dowel could be inserted into each annulus to form a contiguous arm.
With reference again to FIG. 1 , the dual flushing assembly of the present invention operates as follows. When the handle 84 of second handle means 44 is depressed, second flush lever arm 48 is lifted, which in turn lifts vertical tube 25 of water outlet valve 24 and flushing valve seal 100 thereby releasing water through water outlet 34 into toilet bowl (not shown). However, partial float 26 is positioned on vertical tube 25 such that the water outlet valve 24 will close water outlet 34 when only part of the water in the tank 14 is released. This results in only a partial flush. In a preferred embodiment, partial float 26 can be adjustable along the length of vertical tube 25 to control the amount of water released during partial flushing.
When handle 72 of first handle means 42 is depressed, first flush lever arm 46 is lifted, which in turn lifts both second flush lever arm 48 and float assist arm 30 . Second flush lever arm 48 in turn lifts vertical tube 25 as described above. Float assist arm 30 in turn releases float assist 28 . When float assist 28 is released, it operates to keep the vertical tube 25 in the lifted position for a longer period of time. Hence, water outlet valve 24 will remain in the lifted position longer thereby allowing all of the water in the tank 14 to be released through water outlet 34 into toilet bowl (not shown). This results in a full flush.
While various embodiments in accordance with the present invention have been shown and described, it is understood that the same is not limited thereto, but is susceptible to numerous changes and modifications as known to those skilled in the art, and therefore the present invention is not to be limited to the details shown and described herein, but is intended to cover all such changes and modifications as are encompassed by the scope of the appended claims. | A double trip handle type flush control assembly is disclosed, which operates to allow either a full volume of water to be drawn out of the toilet tank or a partial volume of water to be drawn out of the tank. In particular, the double trip handle type flush control assembly of the present invention is adaptable for use in any size toilet tank. Further, the flush control assembly of the present invention has been adapted to accommodate a refill tube, which directs water from a ball cock valve into an overflow tube to refill the toilet trapway after flushing. | 4 |
TECHNICAL FIELD
The present invention relates to a gas generator, in particular for airbag modules in motor vehicles, comprising two generator stages each of which includes in its own pressure housing at least one igniter, at least one propellant charge and at least one combustion chamber.
BACKGROUND OF THE INVENTION
Such multi-stage gas generators are already known from the prior art. One or more generator stages can be ignited depending on the respective demands. The same gas generator can thus be used in vehicle applications for different airbag modules and different vehicle types. However, with the aid of a corresponding control, a decision can also be made with a gas generator installed with an airbag module in a vehicle in dependence on the magnitude of the impact, on different accident conditions or on the situation of use, e.g. the manner of seat occupation, which generator stages are ignited at which time.
With such multi-stage gas generators, it must be prevented by the geometrical arrangement and the design of the individual generator stages that, when one generator stage is ignited, the propellant charge of the other generator is also unintentionally ignited (sympathetic ignition). The pressure housings of the individual generator stages must therefore be correspondingly insulated from one another, with the weight of the gas generator, however, simultaneously being kept as low as possible. Since such gas generators are mass products produced in very high volumes, the manufacture of the generator should moreover be as simple as possible despite these aforementioned demands. As few different parts as possible should in particular be used.
SUMMARY OF THE INVENTION
It is the object of the present invention to provide a gas generator of the initially named kind which is as light and as compact as possible in which the aforesaid problem of cross-ignition does not occur and which can nevertheless be produced in as simple and as cost-favorable manner as possible in high volumes.
This object is satisfied in accordance with the invention in that an inner generator stage is arranged at least substantially inside an outer generator stage and in that the two generator stages are arranged at least partly, in a common filter housing together with a common filter unit arranged outside a pressure housing of the outer generator stage.
The arrangement of the two generator stages inside one another (so-called “stage-in-stage” design) saves room and permits an arrangement overall which is as symmetrical as possible. An additional chamber, which the gases have to flow through, can be provided outside the combustion chambers at the interior of the filter housing due to the arrangement of the two generator stages in a common filter housing including the filter unit. Said gases are not only filtered in this process, so that a gas as free of particles as possible can enter into the airbag, but can also cool down. Since the two generator stages each have their own pressure housing and a common housing with a separating wall is, for instance, not provided, the gas generator can be made up in modular form of different housing modules. For example, a pressure housing of always the same type for the outer generator housing can be combined with different pressure housings for the inner generator stage so that the costs for the manufacture of different gas generators can be reduced. Due to the arrangement of the filter unit outside the outside pressure housing, the latter can be made relatively small, whereby material and weight are saved. It was recognized that it is not necessary to arrange the filter unit inside the outer pressure housing, but that it is rather sufficient to provide a comparatively thin-walled filter housing which can then moreover advantageously be used to satisfy specific additional functions.
Advantageous embodiments of the invention are described in the dependent claims and in the description in conjunction with the enclosed drawings.
In accordance with an embodiment of the invention preferred due to its simplicity, the pressure housing of the outer generator stage is cylindrical and the igniters of the two generator stages are arranged at least approximately symmetrically with respect to a central axis of this pressure housing. This arrangement of the igniters permits an at least largely symmetrical weight distribution inside the pressure housing. The cylindrical shape of the outer pressure housing moreover permits a rotationally symmetrical outflow of the gases generated in the generator.
The two generator stages are preferably cylindrical.
An outflow behavior which is symmetrical to a high degree can be obtained when the central axes of the two igniters and the central axes of the housings and of the filter unit lie in a common plane.
In accordance with a further advantageous embodiment of the invention, the inner generator stage almost completely fills the outer generator stage. This provides an optimum space utilization since a region above the inner stage and belonging to the outer generator stage would not be utilized ideally for technical flow reasons. The probability is moreover reduced that, on an ignition of only the outer generator stage, the inner generator stage is unintentionally ignited as well, since at least the upper wall of the inner generator stage is not directly heated by the combusting propellant charge.
The utilization of the space present can furthermore be optimized in that the filter unit and the two generator stages at least substantially fully fill the filter housing.
In accordance with a further preferred embodiment of the invention, the filter unit is in ring shape and surrounds the outer generator stage. Such an arrangement is again characterized by its symmetry. A ring-shaped filter unit is moreover comparatively simple to assemble.
The filter ring preferably has a smaller axial length than the outer generator stage. Installation space and weight can thereby be saved overall when it is not necessary due to the respectively desired filter effect for a filter ring to extend over the whole axial length of the outer generator stage.
To guide the gas from the outer generator stage through the filter and, finally, out of the gas generator into the airbag to be inflated, in accordance with a preferred embodiment of the invention, outflow openings are provided in the pressure housing of the outer generator stage which are arranged at the level of the lower end of the filter unit and open into a space receiving the filter unit. This space is bounded from the outside by the filter housing and does not have to be completely filled by the filter unit. The generated gas inside this space can cool inside the same due to the expansion before exiting the gas generator. Outflow openings arranged at the level of the lower end of the filter unit in conjunction with skillfully arranged outflow openings of the filter housing permit a relatively long filter path and thus a particularly reliable filtering and a particularly effective cooling of the gas.
It is particularly advantageous for the mentioned outflow openings of the pressure housing of the outer generator stage to be lower than outflow openings of the filter housing. The gas flowing out of the outer generator stage through the lower lying outflow openings of the pressure housing in this case flows upwardly through the filter before exiting the filter housing. Since it is generally more advantageous to arrange the outflow openings through which the gas exits the gas generator as far upwardly as possible, a long filter path can be realized in a particularly elegant manner with such an arrangement, without the dimensions of the gas generator being unnecessarily enlarged.
In order to generate a flow path for the gas flowing out of the inner generator stage which is as long as possible, outflow openings of the inner pressure housing are preferably disposed approximately at the level of the outflow openings of the filter housing. With outflow openings of the filter housing arranged relatively far upwardly and with outflow openings of the outer pressure housing disposed comparatively far downwardly, the gas of the inner generator stage must therefore first move downwardly from the outflow openings of the inner generator stage to the outflow openings of the outer generator stage, from where it then again moves upwardly through the filter and then exits the filter housing approximately at the level of the outflow openings of the inner generator stage.
The outflow openings of the inner generator stage are preferably likewise aligned radially.
In accordance with a further preferred embodiment of the invention, the filter housing has a radially widened portion at the level of the filter unit. Overall, the filter housing can fit snugly substantially from the outside to the pressure housing of the outer generator stage in order to minimize the space requirement, with the said radially widened portion being able to be made to receive the filter unit of in particular ring shape in the region in which the filter unit is arranged.
The igniters of the two generator stages can be secured to a common base plate, which simplifies the manufacture of the gas generator. The mechanical stability of the total generator is moreover increased.
It is very particularly advantageous to form weld connections between the components forming the pressure housings in each case by the same welding process in order to simplify the manufacturing process. In particular capacitor discharge welding, laser welding or friction welding can be considered. The use of the same welding process for all connections saves time and thus costs in the manufacture of the gas generator in accordance with the invention. Depending on the process used and on the geometry of the generator stages, optionally even a plurality of weld connections can be formed in one workstep.
The filter housing is preferably secured to the previously manufactured assembly of the two generator stages with the aid of a reshaping operation, for example, a rolled joint or a beaded joint. Such a fastening can be realized in a simple manner. Alternatively or additionally, the filter housing can, however, also be welded to the base plate and/or to the generator stages.
The filter housing is preferably made as an outer housing of the generator. An additional outer housing of the generator is therefore not necessary, which saves material and thus costs, weight and installation space.
In accordance with a preferred further development of the invention, the filter housing can have a securing flange to attach the gas generator to an airbag module. The filter housing can thus be used as an outer housing of the generator without an additional connection piece being necessary for the attachment to the airbag module.
It is particularly advantageous for outflow openings of the filter housing to be provided in an upper region of the filter unit. Such an arrangement is in particular to be preferred when the filter housing also forms the outer housing of the generator, since the gas should flow out of the gas generator as far toward the top as possible, but still in a radial direction, for an optimum unfolding of the airbag.
In accordance with a further preferred embodiment of the invention, the filter housing can be expanded by the gas pressure generated by means of the generator stages so that it can assist a pressure buffer function. The pressure of the gas flowing out can be reduced by such an expansion of the filter housing such that the airbag is inflated with a lower force than with a filter housing of a less resilient design. This is above all of particular importance at high environmental temperatures, in comparison with lower environmental temperatures, which have the consequence of a higher maximum pressure which would have a full effect on the inflation behavior of the airbag without a pressure buffer. The dilatability of the filter housing can be set such that the inflation behavior is less dependent on the environmental temperature, that is such that the airbag does not behave too “aggressively” in summer and behaves sufficiently “dynamically” in winter. It must also be taken into account here that current regulations require a problem-free function and a simultaneous observation of safety requirements over a temperature range from −35° C. to +85° C., i.e. the gas generator must also be designed for very low temperatures. The pressure buffer function of the filter housing in particular ensures that the increased pressure development does not result in a bursting of the filter housing at very high temperatures.
In accordance with an advantageous further development of the invention, this filter housing can be made so that it surrounds the generator stages, the filter unit and a base plate common to the generator stages like a clamp. This clamp form can be established, for example, by a roll at the lower side of the filter housing. The stability of the total gas generator is increased and the filter housing provided with an additional function by such an arrangement.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be explained in more detail in the following with reference to a preferred embodiment and to the two enclosed Figures. The Figures show in detail:
FIG. 1 is an axial section through a gas generator in accordance with the invention; and
FIG. 2 is a radial section through the gas generator of FIG. 1 in a partly simplified representation.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 2 illustrates the basic design of the two-stage gas generator which has a substantially cylindrical shape overall. An inner generator stage 20 , which is bounded by a cylindrical pressure housing 26 , is arranged asymmetrically inside a larger cylindrical outer generator stage 30 .
The interior space of the pressure housing 26 of the inner generator stage 20 forms a combustion chamber 24 in which a propellant charge not shown in the Figures is stored in the form of pressed fuel pellets. As can better be recognized in FIG. 1 , the outer generator stage 30 has a cylindrical pressure housing 36 whose inner space forms a combustion chamber 34 in which a second propellant charge, which is likewise not shown, of the same type is disposed. The outer pressure housing 36 has a much larger wall thickness than the pressure housing 26 of the inner generator stage 20 since, due to the lower wall surface of the pressure housing 26 of the inner generator stage 20 , a lower wall thickness is sufficient to withstand the pressures which occur.
As is easily recognizable in FIG. 2 , two igniters 22 , 32 each having a circular cross-section are arranged approximately symmetrically to a central axis of the pressure housing 36 of the outer generator stage 30 . The igniter 32 disposed at the right in the two Figures belongs to the outer generator stage 30 , whereas the igniter 22 shown at the left belongs to the inner generator stage 20 and is arranged centrally in its pressure housing 26 .
The inner generator stage 20 substantially lies in the half of the gas generator or of the outer generator stage 30 disposed at the left in the Figures. The pressure housing 26 of the inner generator stage 20 extends in height, as can be recognized in FIG. 1 , almost up to the upper side of the pressure housing 36 of the outer generator stage 30 .
A collection grating 42 extending at a low spacing from the side wall of the pressure housing 36 of the outer generator stage 30 lies regionally between the inner generator stage 20 and the pressure housing 36 . The fuel pellets of the propellant charges are prevented by the collection grating 42 from clogging outflow openings 38 formed in the pressure housing 36 and described further below.
As can easily be recognized in FIG. 2 , a filter housing 56 is arranged coaxially around the pressure housing 36 of the outer generator stage 30 . Both generator stages 20 , 30 lie completely inside the filter housing 56 which is provided at the top and bottom with a relatively large opening to save material and weight and thus practically represents a housing ring which radially completely surrounds and upwardly and downwardly engages around the arrangement of pressure housing 36 and a base plate 46 described in more detail in the following. The space 54 , which is bounded outwardly by the filter housing 56 and inwardly by the pressure housing 36 of the outer generator stage 30 , serves i.a. for the reception of a filter unit 50 explained in the following.
The filter unit 50 , which is not shown in FIG. 2 for reasons of simplicity, is arranged in ring-shape between the pressure housing 36 of the outer generator stage 30 and the filter housing 56 . The filter ring 50 extending around the pressure housing 36 does not extend beyond the total height of the pressure housing 36 , but rather has an axial extent which only amounts to approximately two thirds of the total axial extent of the gas generator.
The filter housing 56 having a substantially lower wall thickness than the pressure housing 36 of the outer generator stage 30 fits snugly to it from the outside, as shown in FIG. 1 , with a radially widened portion being formed in the region of the filter unit 50 which extends, like the filter unit 50 , around the pressure housing 36 in the manner of a ring and serves for the reception of the filter unit 50 . The contour of the filter housing 56 thus substantially corresponds to the outer contour of the pressure housing 36 with the filter ring 50 surrounding it.
As in particular FIG. 2 shows, the central axes of the housings 26 , 36 , 56 , of the ring-shaped filter unit 50 , of the collection grating 42 and of the igniters 22 , 32 lie in a common plane, with the housings 36 , 56 , the filter unit 50 and the collection grating 42 being arranged concentrically and their central axes consequently coinciding.
It can be recognized in FIG. 1 that the outer generator stage 30 is fitted with a booster container 40 which is pushed over the igniter 32 and likewise has a cylindrical shape. This booster container 40 , just like the remaining space of the combustion chamber 34 , is filled with fuel pellets and only opens when a specific threshold pressure has built up such that a very high pressure can be built up very quickly in the combustion chamber 34 . Due to the lower volume of the inner generator stage 20 , it can do without such a booster container; optionally, however, a booster container can likewise be pushed over the igniter 22 of the inner generator stage 20 .
Volume compensation pieces 25 and 35 are provided in both the smaller inner generator stage 20 and in the outer generator stage 30 respectively. They prevent a movement of the fuel pellets of the propellant charges so that these cannot be damaged by friction which occurs and so that an unwanted noise development is avoided.
The pressure housing 26 of the inner generator stage 20 terminates at its upper side at a cover 23 having a circular cross-section which has a peripheral double fold 21 U-shaped in section at its outer rim. This improves the sealing of the pressure housing 26 at its upper rim and gives the cover 23 a certain flexibility. After ignition of the inner generator stage 20 , the cover 23 is presses upwardly by the pressure prevailing in the pressure housing 26 until it abuts the pressure housing 36 of the outer generator stage 30 after overcoming the axial intermediate space which is present. This movement of the cover 23 is made possible by its double fold 21 providing the required path length, without the sealing of the housing 26 being impaired due to the upwardly pressed cover 23 . In contrast, on an ignition of the outer generator stage 30 , the cover 23 is pressed onto the pressure housing 26 of the inner generator stage 20 by the pressure acting from the outside in particular due to the axial intermediate space so that the inner generator stage 20 is or remains reliably sealed.
The pressure housing 26 of the inner generator stage 20 has radial outflow openings 28 which are arranged in an upper region of the pressure housing 26 . The outflow openings 28 are covered by an insulating film 29 at the inner side of the pressure housing 26 . The insulating film 29 can either be made as a film ring and extend around the total periphery of the pressure housing 26 , or every outflow opening 28 is covered by a separate insulation film 29 . The insulation film 29 tears at a certain minimum pressure and thus has a similar effect to the booster container 40 described above: only when a certain minimum pressure has been built up can the gas flow out of the inner generator stage 20 . The outflow openings 28 are covered by a reverse flow protection 29 a from the outside. It can, for example, be a steel band which prevents a flowing of gas from the outer generator stage 30 into the inner generator stage 20 (reverse flow protection). It is avoided in this way that, after an ignition of the outer generator stage 30 , the inner generator stage 20 is unintentionally ignited (“sympathetic ignition”).
The already mentioned outflow openings 38 of the pressure housing 36 of the outer generator stage 30 are likewise radially aligned and lie approximately at a level with the lower end of the filter ring 50 in a lower region of the pressure housing 36 . As can be seen in FIG. 2 , the outflow openings 38 of the pressure housing 36 are distributed at uniform intervals over the total periphery of the cylindrical pressure housing 36 . The outflow openings 38 are covered on the inner side of the pressure housing 36 by an insulating film 39 which has the same effect as the insulating film 29 described above for the outflow openings 28 of the inner generator stage 20 .
The filter housing 56 likewise has outflow openings 58 which are located in the region of the upper end of the filter 50 and thus clearly above the outflow openings 38 of the pressure housing 36 . The outflow openings 28 of the pressure housing 26 of the inner generator stage 20 are located approximately at the same level as the outflow openings 58 of the filter housing 56 .
The two generator stages 20 , 30 have a common, circular base plate 46 having cut-outs, likewise circular, intended to receive the igniters 22 , 32 . The igniters are pushed into these cut-outs and can be welded along its periphery, for example by means of a laser welding process, to the base plate 46 .
The filter housing 56 engaging around the pressure housing 36 at the upper side moreover engages around the base plate 46 and thus forms an outer envelope surrounding the total gas generator like a clamp. The rim engaging around the base plate 46 can be established by a reshaping such as a rolling process or a flanging.
A flange 44 which serves for the attachment of the gas generator to an airbag module, is attached to the filter housing 56 , which also forms the outer housing of the gas generator in the embodiment shown, whereby the filter housing 56 satisfies a further additional function.
The components which form the pressure housings of the two generator stages 20 , 30 are welded together, with the same welding process being able to be used for all welding spots 60 . The outer pressure housing 36 , the collection grating 42 an the pressure housing 26 of the inner generator stage 20 are welded to the base plate 46 . First, the pressure housing 26 of the inner generator stage 20 is preferably filled with a propellant charge and welded to the base plate 46 already provided with the igniters 22 , 32 . An assembly is formed by welding the collection grating 42 and the pressure housing 36 of the outer generator stage 30 to the base plate 46 over which the filter unit 50 and the filter housing 56 are then pushed. The filter housing 56 is secured to the base plate 46 in a last step by reshaping, for example by rolling. Alternatively or additionally, it can also be welded to the base plate 46 . A connection of the components by means of capacitor discharge welding, laser welding or friction welding is in particular especially advantageous
Different ignition sequences are now feasible for the described two-stage gas generator. On the one hand, only one stage, namely the outer generator stage 30 , can be ignited, which is for example advantageous when it is a question of a driver airbag for a comparatively small driver sitting closely behind the steering wheel. Alternatively, both generator stages 20 , 30 can be ignited offset in time or simultaneously. The time span between the first ignition and the second ignition can in particular lie in the range from 0 to 10 ms. The time for the maximum degree of filling of the airbag and the rate of the pressure increase can be matched to different conditions by a corresponding choice of this time span. Generally, with the described arrangement, the outer generator stage 30 is ignited first and then the inner generator stage 20 . It would also be feasible first to ignite the inner generator stage 20 , with the outer generator stage 30 then likewise being ignited shortly thereafter by the gas flowing in via the outflow openings 28 as a consequence of the heat development. However, the individual components can be strained comparatively greatly due to the pressure relationships prevailing in this case so that the reverse ignition order is preferred.
In particular on the ignition of both generator stages 20 , 30 , the common expansion space outside the pressure housing 36 serves not only for filtering, but also for the cooling down and mixing of the gases generated by the two generator stages 20 , 30 . | The present invention relates to a gas generator, in particular for airbag modules in motor vehicles, comprising two generator stages each of which includes in its pressure housing at least one igniter, at least one propellant charge and at least one combustion chamber. An inner generator stage is arranged at least substantially inside an outer generator stage and the two generator stages are arranged at least partly in a common filter housing together with a common filter unit arranged outside a pressure housing of the outer generator stage. | 1 |
FIELD OF THE INVENTION
The invention is directed to packet switching communication networks, and in particular to improvements to Inverse Multiplexing over ATM logical links having inactive IMA sub-links.
BACKGROUND OF THE INVENTION
Asynchronous Transfer Mode (ATM) is a protocol used in telecommunication systems to transport voice and data at high speed. Inverse Multiplexing over ATM (IMA) is used to aggregate the bandwidth of several lower speed links (IMA sub-links) such as, for example, T1 or E1 cables, to effectively provide a single higher speed link (IMA logical link). IMA logical link is also referred to as IMA bundle or IMA group. IMA is described in ATM Forum standard (Inverse Multiplexing for ATM (IMA) Specification Version 1.1; AF-PHY-0086.001). As illustrated in FIG. 1 , ATM cells of a traffic flow 102 to be carried over the IMA logical link are distributed across the lower speed IMA sub-links 112 , 114 , 116 at the transmitting end of the IMA logical link. ATM cell insertion happens in a round-robin fashion 108 among all the IMA sub-links 112 , 114 , 116 in the IMA link. IMA Control Protocol (ICP) cells are used to control the operation of the inverse multiplexing function. ICP cells need to be transmitted periodically on all IMA sub-links. In some cases, one or more of these lower speed sub-links may go into an inactive state 116 e.g. because of a fault, or may have simply been provisioned but left in an inactive state until needed at some future time. Active and inactive sub-links are sometimes referred to as usable or unusable sub-links respectively. When the transmit end of the IMA link has a pending ATM cell 104 to send, it must use a round-robin approach 108 to find the first available active sub-link on which to send the cell. However, if during that process the transmit end encounters an inactive sub-link ( 116 ), it must first send a filler cell 122 (or an ICP cell) over the inactive sub-link ( 116 ) before continuing to search for an active sub-link on which to send the current cell. Generally, if most of the IMA sub-links in an IMA logical link are active, the additional delay and processing resources taken by this process of dealing with inactive sub-links does not adversely impact the transmit end of the IMA link. However, when an IMA logical link has a large number of sub-links (e.g. 16 to 32) and majority of those sub-links are inactive, performance of the line card at the transmit end of the IMA logical link can be seriously degraded especially on a scaled system.
Therefore, a means of providing improved performance for IMA links having inactive sub-links is highly desirable.
SUMMARY OF THE INVENTION
One aspect of an embodiment of the present invention is directed to a method of transmitting filler cells on inactive sub-links of an Inverse Multiplexing over Asynchronous Transfer Mode (IMA) system having an IMA transmitter. The method comprises, for each pending ATM data cell, steps of: selecting a current IMA sub-link via a sub-link ID counter; determining if the current IMA sub-link is active; and responsive to a determination that the current IMA sub-link is not active: adding the current sub-link ID to a list of identified inactive IMA sub-links; incrementing the sub-link ID counter.
Some embodiments of the present invention further comprise steps of: responsive to a determination that the current sub-link is active: instructing the IMA transmitter to transmit a pending ATM data cell on the current sub-link; instructing the IMA transmitter to transmit a predefined IMA filler cell on each inactive sub-link identified in the list of identified inactive IMA sub-links; and incrementing the sub-link ID counter.
Some embodiments of the present invention further comprise a step of clearing the list of identified inactive IMA sub-links after instructing the IMA transmitter to transmit the predefined IMA filler cell.
In some embodiments of the present invention the IMA transmitter comprises a Field Programmable Gate Array (FPGA).
In some embodiments of the present invention the predefined filler cell is stored on the FPGA.
In some embodiments of the present invention the step of instructing the IMA transmitter to transmit a predefined filler cell on the identified inactive IMA sub-links comprises steps of: sending a message to the IMA transmitter comprising: an instruction to transmit the predefined filler cell on each inactive sub-link identified in the list; and a list of IMA sub-link IDs representing the list of identified inactive IMA sub-links.
Some embodiments of the present invention further comprise, prior to the step of determining if the IMA sub-link is active, steps of: determining if an IMA Control Protocol (ICP) cell should be transmitted on the current sub-link; and responsive to a determination that the ICP cell should be transmitted, transmitting the ICP cell on the current sub-link.
Another aspect of an embodiment of the present invention is directed to a system for transmitting filler cells on inactive sub-links of an Inverse Multiplexing over Asynchronous Transfer Mode (IMA) interface. The system comprises: a network processor configured to: receive pending ATM data cells; select a current IMA sub-link via a sub-link ID counter determine whether a current IMA sub-link is active; responsive to a determination that the current IMA sub-link is not active: add the current sub-link ID to a list of identified inactive IMA sub-links; increment the IMA sub-link ID counter.
In some embodiments of the present invention the network processor is further configured to: responsive to a determination that the current sub-link is active: instruct the IMA transmitter to transmit a pending ATM data cell on the current sub-link; instruct the IMA transmitter to transmit a predefined IMA filler cell on each inactive sub-link identified in the list of identified inactive IMA sub-links; and increment the sub-link ID counter.
In some embodiments of the present invention the IMA transmitter comprises a Field Programmable Gate Array (FPGA).
In some embodiments of the present invention the predefined filler cell is stored on the FPGA.
In some embodiments of the present invention, instructing the IMA transmitter to transmit a predefined IMA filler cell on each inactive sub-link identified in the list of identified inactive IMA sub-links comprises: sending a message to the IMA transmitter comprising: an instruction to transmit the predefined filler cell on each inactive sub-link identified in the list; and a list of IMA sub-link IDs representing the list of identified inactive IMA sub-links.
In some embodiments of the present invention the network processor is further configured to: prior to the step of determining if the IMA sub-link is active: determine if an IMA Control Protocol (ICP) cell should be transmitted on the current sub-link; and responsive to a determination that the ICP cell should be transmitted, transmit the ICP cell on the current sub-link.
Another aspect of an embodiment of the present invention is directed to a program storage device readable by a machine, tangibly embodying a program of instructions executable by the machine to perform the method steps described above.
BRIEF DESCRIPTION OF THE DRAWINGS
Some embodiments of apparatus and/or methods in accordance with embodiments of the present invention are now described, by way of example only, and with reference to the accompanying drawings in which:
FIG. 1 illustrates a prior art representation of filler cells transmitted on inactive IMA sub-links;
FIG. 2 illustrates a representation of filler cells transmitted on inactive IMA sub-links according to an embodiment of the present invention; and
FIG. 3 illustrates a system for transmitting filler cells on inactive IMA sub-links according to an embodiment of the present invention; and
FIG. 4 illustrates the flowchart of a method for transmitting filler cells on inactive IMA sub-links according to an embodiment of the present invention.
In the figures like features are denoted by like reference characters.
DETAILED DESCRIPTION
Embodiments of the present invention continually monitor which sub-links of the IMA logical link are in an inactive state, and immediately after (or before) an ATM data cell is transmitted on the IMA logical link, send a filler cell or ICP cell in parallel to all such inactive sub-links. Filler cells are sent on non-active links on which a data cell can not be transmitted. In effect, the filler cells are multicast to all the inactive sub-links at the same time ( 226 , 232 of FIG. 2 ) instead of sending them to the sub-links serially ( 122 of FIG. 1 ). This can provide advantages of reducing delays in sending the next ATM cell while processing filler cells to be sent on inactive IMA sub-links. Note that filler cells also need to be transmitted on active sub-links when there are no ATM data cells in the queue at the time of transmission in order to maintain synchronization between the transmitter at the near end and the receiver at the far end of the IMA sub-link.
As illustrated in FIG. 3 , a transmit line card 206 includes a network processor (NP) 238 , which distributes the cells 204 in the transmit queue 202 in a round robin manner 208 . When an ATM data cell is to be transmitted over the IMA link, the NP 238 selects the current IMA Sub-link via an IMA sub-link ID and if the current IMA sub-link is active, it sends the ATM data cell 217 (or 221 ) with the current IMA sub-link ID over signal bus 244 to a Field Programmable Gate Array (FPGA) 240 . Note that messages from the NP 238 to FPGA 240 are shown on individual lines representing the destination IMA sub-links. The messages are actually sent on a common bus 244 , with an address in the message header indicating the destination IMA sub-link. Persons skilled in the art will recognize that other methods of forwarding the ATM data cells to the FPGA or other transmitter portion of the system could also be used. The FPGA handles link-level input/output (I/O) procedures and synchronization for each of the IMA sub-links, and transmits the ATM cell 218 (or 222 ) on the appropriate physical IMA sub-link.
The NP 238 determines if the current IMA Sub-link is active by retrieving a list of the active/inactive status of the IMA sub-links stored on a database maintained by the host central processor. The active/inactive list can be in the form of a mask, wherein the status of each sub-link is represented by a binary bit. The database can be local to the network processor 238 . If the current IMA sub-link is inactive the NP 238 adds the current sub-link ID to a list of identified inactive IMA sub-links. This list can be in the form of a message that is populated with a list of destination IMA sub-links on to which a filler cell will be sent, but it does not send the Filler Cell List message to the FPGA until the next active IMA sub-link is found. The NP 238 then increments the IMA sub-link ID to select the next IMA sub-link. If subsequent IMA sub-links are also inactive, their sub-link IDs are added to the list of identified inactive IMA sub-links or filler message.
TABLE 1
Format of Filler Cell List message
0
Filler hdr(chan c1)
chan c2
chan c3
1
chan c4
chan c5
chan c6
chan c7
2
chan c8
chan c9
chan c10
chan c11
3
chan c12
chan c13
chan c14
chan c15
4
chan c16
chan c17
chan c18
chan c19
5
chan c20
chan c21
chan c22
chan c23
6
chan c24
chan c25
chan c26
chan c27
7
chan c28
chan c29
chan c30
chan c31
Table 1 above illustrates a format of the Filler Cell List message, for instructing FPGA 240 to generate IMA filler cells on IMA sub-links. The Filler Cell List message header, “Filler Hdr” is a unique header recognizable by the FPGA and also contains the first sub-link ID (“chan C1”) and a filler cell generation count. The filler cell generation count is used by the FPGA to determine the number of IMA filler cells to generate. The sub-link ID of each sub-link that requires an IMA filler cell is stored in subsequent blocks “chan c2” to “chan c31”. Note that this message format is variable length and can accommodate up to 31 sub-link IDs.
When a subsequent IMA sub-link is found to be active, the NP 238 sends the ATM data cell 223 to the FPGA 240 and also sends Filler Cell List message 225 , to the FPGA 240 . The NP 238 then clears the list of identified inactive IMA sub-links in preparation for the next pending ATM data cell in queue 202 . The Filler Cell List message 225 contains the list of identified inactive IMA sub-links and instructs the FPGA to send a predefined filler cell 242 to each inactive IMA sub-link identified in the Filler Cell List message 225 simultaneously as illustrated at 226 . Note that in other embodiments NP 238 could be implemented in an FPGA, or NP 238 and FPGA 240 could be implemented in a single device.
An embodiment of a method 400 of the present invention will now be described with reference to FIG. 4 . The method starts at step 402 . At steps 404 , 406 the NP 238 retrieves the current sub-link ID and the inactive/active status of each IMA sub-link, from a database for this IMA logical link or group, maintained by the central processor. At step 407 , NP 238 retrieves the Cells in Frames (CIF) position from the same database. At step 408 , NP 238 determines if an ICP cell is required to be sent on the current sub-link. This can be calculated as a function of the Cells in Frames (CIF) position and current sub-link ID. ICP cells need to be transmitted on IMA sub-links periodically to manage the IMA interface, to maintain IMA framing on an IMA sub-link, irrespective if the current IMA sub-link is active or not. ICP cells are generated individually by the NP on each link.
If at step 408 , the NP 238 determines that an ICP cell is not required to be sent, then at step 410 , the NP 238 determines if the current sub-link is active by comparing the current sub-link ID against a status mask retrieved at step 406 . If the NP 238 determines that the current link is inactive, then at step 412 NP 238 adds the current sub-link ID to a local list of identified inactive IMA sub-links. If the local list of identified inactive IMA sub-links does not exist, then the list is initialized before the current sub-link ID is added to the list. At each subsequent pass through step 412 , additional sub-link IDs are added to the list for later transmission. This avoids the time delay and cost of NP processor cycles to build and send a filler cell on each inactive IMA sub-link while there is a pending ATM data cell in the ATM queue 202 . At step 414 , the sub-link ID is incremented locally to point at the next current IMA sub-link.
At step 416 the NP 238 determines if the sub-link ID has wrapped around to the first sub-link. If the sub-link ID has not wrapped around, the process loops back to step 410 . If the NP 238 determines that the sub-link ID has wrapped around to the first sub-link, then the process continues to step 418 where the CIF position is incremented. The process then loops back to step 408 .
If the NP 238 determines at step 410 , that the current sub-link is active, then at step 420 , the NP 238 sends an ATM message to the FPGA 240 to transmit the pending ATM cell on the interface of the current IMA sub-link. The ATM message can be in the form of an ATM data cell, with a header prepended to the cell containing the destination IMA sub-link ID. At step 422 the NP 238 determines if there are sub-link Ds in the local list of identified inactive IMA sub-links, and if there are, the NP 238 then sends Filler Cell List message 225 (or 231 ) to the FPGA 240 . If there are no sub-link IDs in the local list, or if the local list does not exist or is not initialized, this means that there are no inactive links on which filler cells need to be sent.
A filler cell can also be sent when there are no ATM data cells present in the transmit queue 202 , which could occur frequently. In this case, filler cells could be sent on active sub-links as well as inactive sub-links and the Filler Cell List Message could contain sub-link IDs for active sub-links. The Filler Cell List message 225 contains the list of identified inactive IMA sub-links and instructs the FPGA to send a predefined filler cell 242 to each inactive IMA sub-link identified in the Filler Cell List message 225 simultaneously as illustrated at 226 . In one embodiment, the Filler Cell List message is tagged with the address of the first inactive sub-link.
At step 424 , the NP 238 then clears the list of identified inactive IMA sub-links in preparation for the next pending ATM cell in queue 202 . Note that the pending ATM cell could be a data cell or a filler cell. The Filler Cell List message 225 contains the list of identified inactive IMA sub-links and instructs the FPGA to send a predefined IMA filler cell 242 to each inactive IMA sub-link identified in the Filler Cell List message 225 simultaneously as illustrated at 226 . The process then moves to step 430 described below.
If at step 408 , the NP 238 determines that an ICP cell is required to be sent, at step 428 , the NP 238 sends a message to the FPGA 240 on bus 244 to transmit the appropriate ICP cell on the current IMA sub-link. The ICP message can be in the form of an ATM ICP cell, with a header prepended to the cell containing the destination IMA sub-link ID. Alternatively, the destination IMA sub-link ID could be appended to the cell instead of prepended. The process the proceeds to step 430 .
At step 430 , the sub-link ID is incremented and at step 432 , the NP 238 determines if the sub-link ID has wrapped around to the first sub-link. If the sub-link ID has not wrapped around, the process skips to step 438 . If the sub-link ID has wrapped around, it means that all of the sub-links have been accessed and the next CIF should be considered. The CIF position is incremented at step 434 . At step 436 , the newly updated CIF position is written to the database, and at step 438 the current sub-link ID is written to the database, so that the host processor of the line card can maintain an accurate status of the IMA interface. The process then stops at step 440 , ready to process the next pending ATM cell in queue 202 .
Alternatively, steps 420 and 422 could be executed in reverse sequence. In both embodiments, filler cells are assembled by the FPGA and transmitted only in conjunction with transmission of an ATM data cell. Simultaneous transmission of filler cells on each inactive IMA sub-link is managed by the FPGA.
Note that there are other circumstances in which filler cells need to be generated, independently of the reception of ATM cells. If there are no ATM cells or not enough ATM cells, in the ATM queue 202 , filler and ICP cells still need to be transmitted on all the IMA sub-links on a regular basis to maintain IMA sub-link integrity or synchronization. The generation of filler cells in these circumstances could be based on the output of a traffic shaper or based on a timer.
A person of skill in the art would readily recognize that steps of various above-described methods can be performed by programmed computers. Herein, some embodiments are also intended to cover program storage devices, e.g., digital data storage media, which are machine or computer-readable and encode machine-executable or computer-executable programs of instructions, wherein said instructions perform some or all of the steps of said above-described methods. The program storage devices may be, e.g., digital memories, magnetic storage media such as a magnetic disks and magnetic tapes, hard drives, or optically readable digital data storage media. The embodiments are also intended to cover computers programmed to perform said steps of the above-described methods.
The description and drawings merely illustrate the principles of the invention. It will thus be appreciated that those skilled in the art will be able to devise various arrangements that, although not explicitly described or shown herein, embody the principles of the invention and are included within its spirit and scope. Furthermore, all examples recited herein are principally intended expressly to be only for pedagogical purposes to aid the reader in understanding the principles of the invention and the concepts contributed by the inventor(s) to furthering the art, and are to be construed as being without limitation to such specifically recited examples and conditions. Moreover, all statements herein reciting principles, aspects, and embodiments of the invention, as well as specific examples thereof, are intended to encompass equivalents thereof.
The functions of the various elements shown in the Figures, including any functional blocks labeled as “processors”, may be provided through the use of dedicated hardware as well as hardware capable of executing software in association with appropriate software. When provided by a processor, the functions may be provided by a single dedicated processor, by a single shared processor, or by a plurality of individual processors, some of which may be shared. Moreover, explicit use of the term “processor” or “controller” should not be construed to refer exclusively to hardware capable of executing software, and may implicitly include, without limitation, digital signal processor (DSP) hardware, network processor, application specific integrated circuit (ASIC), field programmable gate array (FPGA), read only memory (ROM) for storing software, random access memory (RAM), and non volatile storage. Other hardware, conventional and/or custom, may also be included. Similarly, any switches shown in the FIGS. are conceptual only. Their function may be carried out through the operation of program logic, through dedicated logic, through the interaction of program control and dedicated logic, or even manually, the particular technique being selectable by the implementer as more specifically understood from the context.
It should be appreciated by those skilled in the art that any block diagrams herein represent conceptual views of illustrative circuitry embodying the principles of the invention. Similarly, it will be appreciated that any flow charts, flow diagrams, state transition diagrams, pseudo code, and the like represent various processes which may be substantially represented in computer readable medium and so executed by a computer or processor, whether or not such computer or processor is explicitly shown.
Numerous modifications, variations and adaptations may be made to the embodiment of the invention described above without departing from the scope of the invention, which is defined in the claims. | The invention is directed to a method and system for efficiently distributing Inverse Multiplexing over ATM (IMA) filler cells on IMA logical links having inactive or unusable IMA sub-links. Inactive IMA sub-links are identified during round-robin distribution of ATM data cells to active IMA sub-links. Predefined IMA filler cells are transmitted simultaneously on the identified inactive IMA sub-links when an ATM data cell is transmitted on an active IMA sub-link, thereby reducing the delay between transmitting ATM data cells. | 7 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. application Ser. No. 14/594,940 (now U.S. Pat. No. 9,214,230), filed Jan. 12, 2015, which is a continuation of U.S. application Ser. No. 14/050,720 (now U.S. Pat. No. 8,934,285), filed Oct. 10, 2013, which claims the benefit of U.S. Provisional Application No. 61/713,894, filed on Oct. 15, 2012. The entire disclosures of the applications referenced above are incorporated herein by reference.
FIELD
[0002] The present disclosure relates generally to resistive random access memory (RRAM) cells and more particularly to techniques for forming a contact in a RRAM cell to reduce a voltage required to program the RRAM cell.
BACKGROUND
[0003] A resistive random access memory (RRAM) array includes RRAM cells arranged at intersections of word lines and bit lines. A RRAM cell includes an insulating material (e.g., a dielectric) as a resistive element. The resistance of the insulating material increases when current is passed through the insulating material in one direction, and decreases when current is passed through the insulating material in an opposite direction. Accordingly, a RRAM cell can be programmed to (i) a high resistance state by passing current through the RRAM cell in one direction, and (ii) a low resistance state by passing current through the RRAM cell in an opposite direction. The high resistance state can be used to denote logic high (binary 1), and the low resistance state can be used to denote logic low (binary 0), or vice versa.
[0004] RRAM cells that are programmed to high and low resistance states using currents of opposite polarities are called bipolar RRAM cells. Alternatively, RRAM cells can be programmed to high and low resistance states by passing currents of two different magnitudes in the same direction through the insulating material of the RRAM cells. RRAM cells that are programmed to high and low resistance states using currents of two different magnitudes in the same direction are called unipolar RRAM cells.
[0005] Each RRAM cell includes an access device such as a diode or a transistor. The access device is connected in series with the resistive element. Using the access device, the RRAM cells in the RRAM array can be selected and deselected during read and write operations.
SUMMARY
[0006] A cell of a resistive random access memory comprises a resistive element and an access device. The resistive element includes (i) a first electrode and (ii) a second electrode. The access device is configured to select and deselect the cell. The access device includes (i) a first terminal connected to a first contact and (i) a second terminal connected to a second contact. The second contact is connected to the second electrode of the resistive element via a third contact. The third contact includes (i) a first surface in contact with the second contact and (ii) a second surface in contact with the second electrode. The first surface defines a first surface area, and the second surface defines a second surface area. The first surface area is greater than the second surface area.
[0007] In another feature, the third contact has a shape of a pyramid or a cone.
[0008] In another feature, the cell further comprises an interface metal layer between the second contact and the first surface of the third contact.
[0009] In another feature, the third contact is partially etched to reduce a volume of the third contact.
[0010] In other features, the resistive element comprises a first layer of transitional metal oxide arranged adjacent to the second electrode, and a second layer of a reactive metal arranged adjacent to (i) the first layer of transitional metal oxide and (i) the first electrode.
[0011] In another feature, the first layer of transitional metal oxide is thinner near a center of the first layer relative to a remainder of the first layer.
[0012] In other features, the first electrode of the resistive element is connected to a fourth contact, and the first contact connected to the first terminal of the access device is connected to a bit line via fifth contact.
[0013] In other features, a sixth contact is arranged between (i) the first contact connected to the first terminal of the access device and (ii) the fifth contact, and the sixth contact has a structure of the third contact.
[0014] In another feature, the resistive element is configured to have (i) a first resistance in response to applying a first voltage across the first electrode and the second electrode and (ii) a second resistance in response to applying a second voltage across the first electrode and the second electrode.
[0015] In another feature, the access device further includes a control terminal connected to a word line.
[0016] In still other features, a method for connecting elements of a cell of a resistive random access memory, where the elements of the cell include (i) an access device and (ii) a resistive element, the access device includes (i) a first terminal and (ii) a second terminal, the resistive element includes (i) a first electrode and (ii) a second electrode, and the access device is used to select and deselect the cell. The method comprises connecting (i) the first terminal and (ii) the second terminal of the access device respectively to (i) a first contact and (ii) a second contact and connecting the second contact of the access device to the second electrode of the resistive element via a third contact. The third contact includes (i) a first surface in contact with the second contact and (ii) a second surface in contact with the second electrode. The first surface defines a first surface area, and the second surface defines a second surface area. The first surface area is greater than the second surface area.
[0017] In another feature, the third contact has a shape of a pyramid or a cone.
[0018] In another feature, the method further comprises arranging an interface metal layer between the second contact and the first surface of the third contact.
[0019] In another feature, the method further comprises partially etching the third contact to reduce a volume of the third contact.
[0020] In other features, the method further comprises forming the resistive element by arranging a first layer of transitional metal oxide adjacent to the second electrode, and by arranging a second layer of a reactive metal adjacent to (i) the first layer of transitional metal oxide and (i) the first electrode.
[0021] In another feature, the first layer of transitional metal oxide is thinner near a center of the first layer relative to a remainder of the first layer.
[0022] In other features, the method further comprises connecting the first electrode of the resistive element to a fourth contact, and connecting the first contacted to the first terminal of the access device to a bit line via fifth contact.
[0023] In another feature, the method further comprises arranging a sixth contact between (i) the first contact connected to the first terminal of the access device and (ii) the fifth contact, where the sixth contact has a structure of the third contact.
[0024] In other features, the method further comprises applying a first voltage across the first electrode and the second electrode to program the cell to a first resistance state, and applying a second voltage across the first electrode and the second electrode to program the cell to a second resistance state.
[0025] In other features, the method further comprises connecting a control terminal of the access device to a word line, and selecting and deselecting the cell using the word line.
[0026] Further areas of applicability of the present disclosure will become apparent from the detailed description, the claims and the drawings. The detailed description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the disclosure.
BRIEF DESCRIPTION OF DRAWINGS
[0027] FIG. 1A shows a schematic of an example of a resistive random access memory (RRAM) cell.
[0028] FIG. 1B shows a schematic of a resistive element of the RRAM cell shown in FIG. 1A .
[0029] FIG. 1C shows creation of multiple conducting paths in a transitional metal oxide layer due to movement of oxygen ions from the transitional metal oxide layer to a reactive metal layer of the resistive element shown in FIG. 1B .
[0030] FIG. 1D shows resetting of the multiple conducting paths in the transitional metal oxide layer due to return of the oxygen ions from the reactive metal layer to the transitional metal oxide layer of the resistive element shown in FIG. 1B .
[0031] FIG. 2 shows an example of a RRAM cell, where all the layers of the resistive element are flat.
[0032] FIG. 3 shows an example of a sharp contact grown on the surface of a drain contact of an access device of a RRAM cell.
[0033] FIG. 4 shows an example of a sharp contact grown on an interface metal layer pre-grown on the surface of a drain contact of an access device of a RRAM cell.
[0034] FIG. 5 shows an example of a sharp contact that is etched back.
[0035] FIG. 6A shows an example of a RRAM cell with the sharp contact and a resistive element created by growing layers of the resistive element around the sharp contact.
[0036] FIGS. 6B-6D illustrate a process of thinning the transitional metal oxide layer of the resistive element shown in FIG. 6A at the tip of the transitional metal oxide layer by bombarding the tip during reactive metal layer formation.
[0037] FIG. 7 shows an example of a RRAM cell including all the features of the RRAM cell shown in FIG. 6A , and additionally including a sharp contact grown on the surface of the source contact of the access device.
[0038] FIG. 8 is a flowchart of a method for creating the sharp contact(s) and the resistive element shown in FIGS. 3-7 .
[0039] In the drawings, reference numbers may be reused to identify similar and/or identical elements.
DESCRIPTION
[0040] FIG. 1A shows an example of a resistive random access memory (RRAM) cell 100 . The RRAM cell 100 includes an access device 102 and a resistive element 104 . In the example shown, the access device 102 includes a transistor. Alternatively, diodes or other suitable switching elements can be used as the access device 102 .
[0041] FIG. 1B shows the resistive element 104 . The resistive element 104 includes a top electrode 106 , a bottom electrode 108 , a dielectric layer 110 , and a reactive metal layer 112 . For example, the dielectric layer 110 includes a layer of a transitional metal oxide (e.g., HfO 2 ). The dielectric layer 110 acts as a donor of oxygen ions. For example, the reactive metal layer 112 includes a layer of titanium (Ti).
[0042] FIG. 1C shows flow of oxygen ions 113 from the dielectric layer 110 to the reactive metal layer 112 when a positive voltage is applied to the top electrode 106 relative to the bottom electrode 108 . The flow of oxygen ions 113 from the dielectric layer 110 to the reactive metal layer 112 creates a plurality of conducting paths 114 . Consequently, the resistive element 104 has a low resistance, and the RRAM cell 100 has a low resistance state.
[0043] FIG. 1D shows flow of oxygen ions 113 from the reactive metal layer 112 to the dielectric layer 110 when a negative voltage (or a less positive voltage than that applied in FIG. 1C ) is applied to the top electrode 106 relative to the bottom electrode 108 . The oxygen ions 113 return to the dielectric layer 110 through the plurality of conducting paths 114 . Consequently, the resistive element 104 has a high resistance, and the RRAM cell 110 has a high resistance state.
[0044] FIG. 2 shows an example of the RRAM cell 100 . For example, the access device 102 is shown as a metal-oxide semiconductor field-effect transistor (MOSFET) having a source terminal, a drain terminal, and a gate terminal. Throughout the present disclosure, while certain aspects are described with specific references to the drain and source terminals, the source and drain terminals are interchangeable. The source terminal is connected to a bit line via a contact. The gate terminal is connected to a word line via a contact. The drain terminal is connected to the bottom electrode 108 of the resistive element 104 via a contact.
[0045] Each of the bottom electrode 108 , the dielectric layer 110 , the reactive metal layer 112 , and the top electrode 106 is a flat layer of respective material. The flatness of these layers causes the formation of the plurality of conducting paths shown in FIG. 1C . The plurality of conducting paths makes programming of the RRAM cell 100 difficult. Particularly, when programming the RRAM cell 100 from the low resistance state to the high resistance state, a sufficiently high voltage must be applied to ensure that each of the plurality of conducting paths is reset.
[0046] The present disclosure relates to creating a novel contact between the drain contact of the access device and the bottom electrode of the resistive element. The novel contact is a sharp, pointed structure. The present disclosure further relates to a novel resistive element structure. Specifically, the resistive element is created by arranging layers of the bottom electrode, the dielectric layer, the reactive metal layer, and the top electrode of the resistive element around the sharp contact. Additionally, the thickness of the dielectric layer at the tip of the sharp contact is made less than the thickness of the remainder of the dielectric layer. This structure allows formation of a single conducting path in the dielectric layer, which is easy to program with a voltage lower than the voltage normally used to program the RRAM cell.
[0047] Compared to the traditional flat contact, this novel structure strengthens the field and current densities at the center of the resistive element. The localized programming enables the new RRAM cell with better writability and device matching compared to the traditional RRAM cell. The new approach does not add a mask layer to the manufacturing process.
[0048] FIG. 3 shows an example of a RRAM cell 200 according to the present disclosure. The RRAM cell 200 includes the access device 102 . A sharp contact 202 is created between a drain contact 204 of the access device 102 and the bottom electrode of the resistive element (not shown). The sharp contact 202 can be realized by employing nanotechnologies such as quantum dots growth on the surface of the drain contact 204 of the access device 102 . Using these methods, a lightning-rod-like sharpened structure is grown with precision on the surface of the drain contact (e.g., tungsten) 204 to form the sharp contact 202 .
[0049] FIG. 4 shows an example of an alternate embodiment of a RRAM cell 210 according to the present disclosure. Instead of growing the sharp contact 202 directly on the surface of the drain contact (e.g., tungsten) 204 of the access device 102 , initially, a suitable interface metal material 212 may be selectively grown on the surface of the drain contact 204 . Subsequently, the sharp contact 202 is grown on the interface metal material 212 .
[0050] FIG. 5 shows an example of another alternative embodiment of a RRAM cell 220 according to the present disclosure. Optionally, for better contact resistance, the sharp contact 202 may be etched back to expose part of the original surface of the drain contact (e.g., tungsten) 204 of the access device 102 . The result is a smaller sharp contact 202 - 1 in a middle portion of the surface of the drain contact 204 of the access device 102 .
[0051] FIG. 6A shows a cross-section of an example of a RRAM cell 300 according to the present disclosure. The RRAM cell 300 includes the access device 102 and a new resistive element 302 according to the present disclosure. The sharp contact 202 (or 202 - 1 shown in FIG. 5 ) is grown on the surface of the drain contact (e.g., tungsten) 204 of the access device 102 (or on the interface metal material 212 shown in FIG. 4 ) as explained before.
[0052] The resistive element 302 includes a bottom electrode 304 , a dielectric layer 306 , a reactive metal layer 308 , and a top electrode 310 grown around the sharp contact 202 as shown. For example, the dielectric layer 306 includes a layer of a transitional metal oxide (e.g., HfO 2 ). The dielectric layer 306 acts as a donor of oxygen ions. For example, the reactive metal layer 308 includes a layer of titanium (Ti).
[0053] As shown in FIGS. 6B and 6D , during the formation of the reactive metal layer 308 , a process such as physical vapor deposition (PVD) may be tuned to be initially more bombarding. For example, the tip of the transitional metal oxide layer (i.e., the dielectric layer 306 ) may be bombarded with an inert gas (e.g., Ar). Due to the bombarding, the transitional metal oxide layer (i.e., the dielectric layer 306 ) may become slightly thinner at the tip than at the slopes. In FIG. 6C , the distance d 1 between the tip of the dielectric layer 306 and the tip of the bottom electrode 304 is less than the distance d 2 between the dielectric layer 306 and the bottom electrode 304 elsewhere. The thinness of the dielectric layer 306 at the tip will ensure that programming of the RRAM cell 300 is more likely to occur (i.e., to be localized) at the tip via a single conducting path. Optionally, after bottom electrode, transition metal oxide, reactive metal, and top electrode deposition, planarization may be utilized to create a smoother surface for later patterning steps.
[0054] The top electrode 310 of the resistive element 302 is connected to a contact 312 . The contact 312 provides a connection to other circuitry (e.g., a voltage generator used to program the RRAM cell 300 ). The source terminal of the access device 102 is connected to a source contact 314 . The source contact 314 is connected to a bit line via a contact 316 .
[0055] FIG. 7 shows another embodiment of a RRAM 350 according to the present disclosure. When the sharp contact 202 is grown on the surface of the drain contact 204 , a sharp contact 352 is also grown on the source contact 314 . The sharp contact 352 may be of the same dimensions as the sharp contact 202 or may be smaller than the sharp contact 202 . The sharp contact 352 may be etched away if the resistivity of the sharp contact 352 is high or can be left on top of the source contact 314 if the resistivity of the sharp contact 352 is low.
[0056] In general, the sharp contacts 202 , 202 - 1 , and 352 can have the shape of a pyramid or a cone, where the base of the pyramid or the cone connects to the drain contact 204 (and the source contact 314 ), and an apex of the pyramid or a vertex of the cone connects to the bottom electrode of the resistive element. A pyramid is a polyhedron formed by connecting a polygonal base to a point called an apex of the pyramid. For example, depending on the shape of the drain contact 204 (and the source contact 314 ), the pyramid can be a square pyramid, a pentagonal pyramid, a hexagonal pyramid, or a tetrahedron. Alternatively, for example, if the shape of the drain contact 204 (and the source contact 314 ) is round or oval, the shape of the sharp contacts 202 , 202 - 1 , and 352 may be conical. In some implementations, regardless of the shape of the drain contact 204 (and the source contact 314 ), the sharp contacts 202 , 202 - 1 , and 352 can have a shape that has a greater surface area at the point of contact with the drain contact 204 (and the source contact 314 ) than at the point of contact with the bottom electrode of the resistive element. Typically, the shape of the sharp contacts 202 , 202 - 1 , and 352 converges to a point having infinitesimal dimensions at the point of contact with the bottom electrode of the resistive element.
[0057] FIG. 8 shows a method 400 for creating a sharp contact between a drain contact of an access device and a bottom electrode of a resistive element and for creating a resistive element according to the present disclosure. At 402 , a sharp contact is grown on a surface of a drain contact or on a surface of an interface metal layer pre-grown on the surface of the drain contact. At 404 , the sharp contact is optionally etched back. At 406 , a resistive element is created on top of the sharp contact by growing layers of a bottom electrode, a transitional metal oxide, a reactive metal, and a top electrode around the sharp contact. At 408 , during reactive metal layer formation, the process is tuned to be initially more bombarding so that the transitional metal oxide layer is thinner at the tip than at the slopes. At 410 , a sharp contact also formed on the surface of the source contact can be etched away if the resistivity of the sharp contact is high or can be preserved if the resistivity of the sharp contact is low. At 412 , the top electrode of the resistive element is connected to another contact for connection to other circuitry, and the source contact (with or without the associated sharp contact) is connected to a bit line via another contact.
[0058] The foregoing description is merely illustrative in nature and is in no way intended to limit the disclosure, its application, or uses. The broad teachings of the disclosure can be implemented in a variety of forms. Therefore, while this disclosure includes particular examples, the true scope of the disclosure should not be so limited since other modifications will become apparent upon a study of the drawings, the specification, and the following claims. As used herein, the phrase at least one of A, B, and C should be construed to mean a logical (A or B or C), using a non-exclusive logical OR. It should be understood that one or more steps within a method may be executed in different order (or concurrently) without altering the principles of the present disclosure. | A system including a resistive element of a memory cell and a device to access the resistive element of the memory cell. The resistive element includes (i) a first electrode, and (ii) a second electrode. The device includes (i) a first terminal connected to a first contact, and (i) a second terminal connected to a second contact. One or more of the first contact and the second contact of the device is respectively connected to one or more of the first electrode and the second electrode of the resistive element via a third contact. A size of the third contact decreases from the one or more of the first contact and the second contact of the device to the one or more of the first electrode and the second electrode of the resistive element of the memory cell. | 8 |
BACKGROUND OF THE INVENTION
The present invention relates to a glider, and more particularly to a glider having preassembled bench panels.
Gliders, also referred to as swings, are lawn or porch furniture providing single or multiple person seating that is generally suspended so that it may rock or swing. Conventionally, gliders are sold to consumers in an unassembled condition because it is impractical to package, store and transport these bulky items in an assembled condition.
A particularly popular form of gliders include a bench with seat and back portions each having a plurality of horizontal wooden slats. This type of glider often includes a frame fabricated from solid metal or metal tube stock, or cast from metal. As compared to wooden frames, such metal frames are durable, lightweight and relatively inexpensive to manufacture.
Assembly of such a glider involves individually attaching each wooden slat to the metal frame using two or more screws, nuts and bolts, or similar fasteners. This is inconvenient for a purchaser of the glider since it is a very tedious and time consuming task. Further, such an involved assembly procedure by an unskilled consumer often leads to improperly assembled gliders.
Thus, it is desirable to produce a glider with wooden seat slats that is easy to assemble and can be provided to the consumer in a compact package.
SUMMARY OF THE INVENTION
The present invention provides a partially assembled glider for final assembly by a purchaser comprising: a stationary frame; a bench frame for suspended attachment to the stationary frame; a preassembled bench back panel for attachment to the bench frame, the preassembled bench back panel comprising a first plurality of slats secured to a first support; and a preassembled bench seat panel for attachment to the bench frame, the preassembled bench seat panel comprising a second plurality of slats secured to a second support.
According another aspect, the present invention provides a glider comprising: a stationary frame formed from metal; a bench frame formed from metal, the bench frame being movably suspended from the stationary frame; a bench back panel comprising a first plurality of wooden slats attached to a first wooden support, the bench back panel being attached to the bench frame; and a bench seat panel comprising a second plurality of wooden slats attached to a second wooden support, the bench seat panel being attached to the bench frame.
According to a further aspect, the present invention provides a method for manufacturing a partially assembled glider for final assembly by a purchaser, the method comprising steps of: assembling a bench back panel by securing a first plurality of slats to a first support; assembling a bench seat panel by securing a second plurality of slats to a second support; fabricating a plurality of frame members for constructing a bench frame and a stationary frame; and packaging the bench back panel, the bench seat panel and the frame members unassembled in a package for storage, shipping and sale to a consumer.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
FIG. 1A is an exploded perspective view of a bench for a glider assembly according to a first embodiment of the present invention;
FIG. 1B is a perspective view of a frame for a glider assembly according to the first embodiment of the present invention;
FIG. 1C is a detail view of a lap joint of the bench of FIG. 1A;
FIG. 2 is a perspective view of a bench for a glider assembly according to a second embodiment of the present invention;
FIG. 3 is a bottom perspective view of the bench of FIG. 2; and
FIG. 3A is a detail view of a joint of the bench of FIG. 2 .
DETAILED DESCRIPTION OF THE INVENTION
According to a first embodiment of the present invention, as shown in FIGS. 1A and 1B, a glider assembly in a partially assembled condition comprises a bench 10 and a frame 12 . The bench 10 comprises a preassembled bench back panel 14 and a bench seat panel 16 .
The bench back panel 14 comprises a left side support member 18 , an intermediate support member 20 , a right side support member 22 , and a plurality of slats 24 attached to the support members 18 - 22 . Likewise, the bench seat panel 16 comprises a left side support member 26 , an intermediate support member 28 , a right side support member 30 , and a plurality of slats 32 attached to the support members 26 - 30 .
The support members 18 - 22 , 26 - 30 and the slats 24 , 32 are each fabricated from wood. The slats 24 , 32 are attached to the respective support members 18 - 22 , 26 - 30 by a manufacturer using nails, brads, rivets, screws, adhesive or other known means of attachment. Thus, the bench back panel 14 and the bench seat panel 16 are provided to a purchaser of the glider in an individually preassembled condition.
The glider assembly is provided to a purchaser by the manufacturer or retailer in the form of a packaged kit, which includes the preassembled bench back panel 14 , the preassembled bench seat panel 16 , the frame 12 , and a variety of fasteners and other hardware necessary for final assembly of the glider by the purchaser.
The bench back panel 14 and the bench seat panel 16 are each provided with means of attachment for attaching the panels 14 , 16 to each other. The means of attaching the bench back panel 14 comprises notched ends 34 , 36 , 38 provided respectively to each of the support members 18 - 22 . Likewise, the means of attaching the bench seat panel 16 comprises notched ends 40 , 42 , 44 provided respectively to each of the support members 26 - 30 .
To assemble the bench 10 , the purchaser of the glider attaches the notched ends 34 - 38 of the bench back panel 14 to the respective and complementary notched ends 40 - 44 of the bench seat panel 16 using nuts 46 and bolts 48 . The resulting joint is similar to that commonly referred to as a square shoulder joint or lap joint. As shown in FIG. 1C, each pair of complementary notched ends 34 , 40 ; 36 , 42 ; 38 , 44 are engaged such that relative rotation is prevented by the abutment of pairs of shoulders or facing surfaces 50 , 52 .
The glider frame 12 comprises a stationary frame 54 and a bench frame 56 . In the disclosed embodiment, the frames 54 , 56 are fabricated from bent metal tube stock. Alternatively, other material could be used to fabricate the frames 54 , 56 , such as solid metal stock. The bench frame 56 is movably suspended from the stationary frame 54 by a plurality of glider bands or straps 58 attached between the frames 54 , 56 . This attachment can be achieved by a bushing and fastener assembly, or similar, utilized at each point of attachment of the glider straps 58 . The straps 58 of the present embodiment are in the form of metallic straps, however, other suitable materials or other suitable configurations can be utilized. For example, although the glider frame 12 of the present embodiment is shown to utilize two straps 58 on each side of the frame 12 , a lesser or greater number can be used and/or the straps 58 can be formed from an elastomeric material.
The glider frame 12 can be provided to the consumer in various stages of assembly. For example, each of the stationary frame 54 , the bench frame 56 and the glider straps 58 can be provided as separate parts to be assembled by the purchaser. As a further example, the stationary frame 54 and/or the bench frame 56 can be provided as smaller sections of metal tubing (not shown) which must be fastened together by the purchaser to form the frames 54 , 56 .
Each of the stationary frame 54 and the bench frame 56 has a pair of armrests 60 attached thereto. The armrests 60 can be provided pre-attached to the purchaser or as separate parts which must be attached using fasteners. Alternatively, one or more of the armrests 60 can be eliminated. As a further alternative, other structures can be substituted for the armrests 60 , such as side tables.
To enable the purchaser to attach the assembled bench 10 to the frame 12 , each side of the bench 10 is provided with a plurality of holes: a first attachment hole 62 and a second attachment hole 64 in each of the left and right side support members 18 , 22 of the bench back panel 14 , and a third attachment hole 66 in each of the left and right side support members 26 , 30 of the bench seat panel 16 . A screw, bolt or other fastener (not shown) is used to secure each of these attachment holes 62 - 66 to corresponding holes 68 , 70 , 72 in the bench frame 56 by the purchaser.
FIGS. 2, 3 and 3 A show a glider bench 110 according to a second embodiment of the present invention. Like the bench 10 of the first embodiment, the bench 110 comprises a bench back panel 114 and a bench seat panel 116 . Support members 118 , 120 , 122 , 126 , 128 , 130 are respectively provided with curved support surfaces 119 , 121 , 123 , 127 , 129 , 131 , resulting in a curved arrangement of the attached slats 124 , 132 . This curved arrangement of the slats 124 , 132 is provided to enhance the comfort and aesthetic appeal of the bench 110 .
As shown in FIGS. 2 and 3, the left side support members 122 , 130 overlap at their respective ends 138 , 144 and are attached to each other by means of two screws, bolts or other fasteners 146 , 147 . The use of two fasteners 146 , 147 , unlike the single fastener 46 of the first embodiment, prevents relative rotation of the support members 122 , 130 . Similarly, the right side support members 118 , 126 overlap at their respective ends 134 , 140 and are attached to each other by means of two fasteners 146 , 147 .
As best shown in FIG. 3A, the intermediate support members 120 , 128 abut at their respective ends 136 , 142 and are attached to each other by means of a bolt 174 and cylindrical nut 176 . This type of joint is commonly referred to as a butt joint. Other means of attachment, such as a wood screw or peg, could be used in place of the bolt 174 and cylindrical nut 176 .
It should be evident that this disclosure is by way of example and that various changes may be made by adding, modifying or eliminating details without departing from the fair scope of the teaching contained in this disclosure. The invention is therefore not limited to particular details of this disclosure except to the extent that the following claims are necessarily so limited. | A metal frame glider having preassembled wooden seat panels. A bench back panel and a bench seat panel each include three vertical wooden support members to which a plurality of horizontal wooden slats are attached. | 0 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of under 35 USC §120 to, commonly owned, U.S. application Ser. No. 09/853,356, filed May 11, 2001, now U.S. Pat. No. 6,433,614 which is a continuation of U.S. application Ser. No. 09/798,008, filed Mar. 2, 2001, now abandoned the entire contents of which are hereby incorporated by reference.
BACKGROUND
This invention relates to transistor switches, and more particularly to metal oxide semiconductor field-effect transistor (MOSFET) switches.
In power management ICs having a monolithically integrated MOSFET power train, the on-chip field-effect transistor (FET) not only accounts for most of the power dissipation, but also consumes a significant amount of silicon area, and very often is the major concern regarding the long-term reliability of the chip.
FIG. 1 shows a cross-sectional view of a conventional asymmetric high-voltage NMOS transistor, compatible with standard CMOS processes, with N deep drain (NDD) implantation. Although implementations of the inventions are described with reference to an asymmetrical device, the invention applies to all MOSFET devices.
A N+ source 104 is formed within a P substrate 102 . Also formed in the substrate is a NDD region 106 that includes a N+ drain implant 108 , and a N lightly doped drain (LDD) implant 1 12 . Formed upon substrate 102 is a LDD that includes a gate 114 .
Two important dimensions in this device structure are the length L G of gate 114 and the spacing L D between the drain N+ implant 108 and gate 114 . The design rules for these two dimensions are set to meet two specifications punch-through breakdown voltage, and hot-carrier lifetime.
Quite often, it is the reliability specification, also referred to as the hot-carrier lifetime specification, instead of the punch-through breakdown voltage specification, that determines the design rule, which dictates the minimum allowed dimensions of L G and L D .
In other words, in the applications where hot-carrier degradation is not of concern, a more aggressive design rule can be used to design a transistor such as that shown in FIG. 1 while still meeting the same punch-through breakdown voltage specification. A FET structure with smaller dimensions on L G or L D is preferred because it not only reduces the overall chip area, but also reduces the on resistance and the junction capacitance of the FET, thus improving the overall system efficiency.
It is known that hot-carrier injection (HCI) occurs at the overlapping period between the transitions of the gate voltage and drain voltage of the FET, with the injection peaking when the gate voltage is approximately one half of the drain voltage. As a result, the typical inverter application turns out to be a stressful operation for the FET in terms of hot-carrier degradation. HCI is discussed in greater detail in W. Weber, C. Werner and A. V. Schwerin, “Lifetimes and substrate current in static and dynamic hot-carrier degradation, ” IEDM 86, pp 390-393, 1986.
FIG. 2 is a conceptual time t versus voltage v plot of voltage waveforms for a conventional N-FET during the switching transitions of a typical inverter mode operation. During the turn-on transition, the drain voltage V D goes low and the gate voltage V G goes high. During the turn-off transition, V P goes high and V G goes low. The area between times t 1 and t 2 and t 3 and t 4 shows the transition period during which a strong hot-carrier injection occurs. Hot-carrier degradation results in threshold voltage shift and transconductance degradation for the N-FET. Due to the hot-carrier degradation concern, the conventional design of a FET switch typically involves trade-offs between electrical performance, such as on resistance, and reliability performance, such as hot-carrier lifetime. In general, making a conventional device more resilient to hot carrier degradation involves increasing one or both of L G and L D , while improving electrical performance (and minimizing device area) involves minimizing L G and L D .
SUMMARY
In general, in one aspect, the invention features a method and computer program product for use with a switch having a field-effect transistor (FET). It includes restricting the drain-source voltage of the FET to a predetermined range; and then switching the FET.
Particular implementations can include one or more of the following features. It includes delaying switching for a predetermined period of time after restricting. It includes delaying switching for a period of time after restricting that is determined by the drain-source voltage of the FET. It includes releasing the drain-source voltage of the FET after switching. The switch includes a further FET having a drain coupled to the drain of the FET and a source coupled to the source of the FET, and restricting includes controlling the further FET. Restricting includes turning on the further FET; and switching includes turning on the FET. Restricting includes keeping the further FET on; and switching includes turning off the FET. It includes keeping the FET, off when the current at the drain is below a predetermined threshold current.
In general, in one aspect, the invention features a circuit having source, drain and gate terminals. It includes a first field-effect transistor (FET) having a first drain coupled to the drain terminal and a first source coupled to the source terminal; a second FET having a second drain coupled to the drain terminal and a second source coupled to the source terminal; and a control circuit coupled to the gate terminal, the first gate, and the second gate.
Particular implementations can include one or more of the following features. The control circuit is coupled to the drain terminal. The control circuit is configured to turn on the second FET before turning on the first FET. The control circuit is configured to impose a fixed delay between turning off the first and second FETs. The control circuit is configured to impose a delay between turning on the first and second FETs, the duration of the delay determined by the voltage between the drain and source terminals. The control circuit is configured to turn off the second FET after turning off the first FET. The control circuit is configured to impose a fixed delay between turning on the first and second FETs. The first FET is designed for superior electrical performance. The second FET is designed for superior reliability performance. The first and second FETs are implemented as a single monolithic device. The first and second; FETs and the control circuit are implemented as a single monolithic device. The circuit includes a current sensing circuit configured to keep the first FET off when the current at the drain terminal is below a predetermined threshold current.
Advantages that can be seen in implementations of the invention include one or more of the following. Implementations of the invention provide cost reduction, efficiency improvement and reliability enhancement in switching applications. Because the helper FET only accounts for a small percentage of the total FET switch size, designers can cut the overall FET switch area while improving overall switching efficiency. This approach successfully overcomes the tradeoff between electrical performance and reliability performances of conventional MOSFET switches.
The details of one or more embodiments of the invention are set forth in the accompanying drawings and the description below. Other features, objects, and advantages of the invention will be apparent from the description and drawings, and from the claims.
DESCRIPTION OF DRAWINGS
FIG. 1 shows a cross-sectional view of a conventional asymmetric high-voltage NMOS transistor.
FIG. 2 is a time t versus voltage v plot of voltage waveforms for a conventional N-FET during the turn-on transition of a typical inverter mode operation.
FIG. 3 is a block diagram of a FET switch according to one implementation.
FIG. 4 depicts a circuit for use in an FET control circuit according to one implementation.
FIG. 5 shows a timing diagram for three of the voltage waveforms for a switch according to one implementation.
FIG. 6 depicts a circuit for use in an FET control circuit according to another implementation.
FIG. 7 depicts a circuit for use in an FET control circuit according to still another implementation.
FIG. 8 depicts a circuit for use in an FET control circuit according to yet another implementation.
FIG. 9 depicts a circuit for use in an FET control circuit according to another implementation.
Like reference symbols in the various drawings indicate like elements.
DETAILED DESCRIPTION
FIG. 3 is a block diagram of a FET switch 302 according to one implementation. Switch 302 includes a main FET F M , a helper FET F H , and a control circuit 304 . Control circuit 304 controls the timing of the operation of the main and helper FETs. The main FET is designed for superior electrical performance, while the helper FET is designed for superior reliability performance. The helper FET controls the drain voltage of the main FET during the switching transition of the main FET.
The drain D M of the main FET is coupled to the drain D H of the helper FET to form the drain D of switch 302 . The source S M of the main FET is coupled to the source S H of the helper FET to form the source S of switch 302 . Control circuit 304 receives the signals applied to the gate G of switch 302 . In some implementations, control circuit 304 also receives the signals applied to the drain D of switch 302 .
Control circuit 304 controls the timing of the gate signal G M for the main FET and the gate signal G H for helper FET such that the main FET operates at a stress-free biasing condition under any switching scenario.
FIG. 4 depicts a circuit 400 for use in control circuit 304 according to one implementation. The inputs of a NAND gate 402 are coupled to terminals G and G H . The inputs of a NOR gate 404 are coupled to terminals G and G M . The output of NAND gate 402 is coupled to the input of an inverter 406 . The output of inverter 406 is coupled to terminal G M . The output of NOR gate 404 is coupled to the input of an inverter 408 . The output of inverter 408 is coupled to terminal G M .
FIG. 5 shows a timing diagram for three of the voltage waveforms for switch 302 according to one implementation. V D is the voltage appearing at terminal D. V G (F H ) is the voltage applied to terminal G H by control circuit 304 . V G (F M ) is the voltage applied to terminal G M by control circuit 304 . V G is the voltage appearing at terminal G. V G is substantially similar to V G (F H ) during the turn-on transition, and is substantially similar to V G (F M ) during the turnoff transition. Therefore, for clarity, V G is not shown.
A turn-on transition is shown from time t 1 to time t 5 . At t 1 , V G begins to rise. Switch 302 responds by turning on the helper FET. Control circuit 304 turns on the helper FET by asserting a high voltage V G (F H ) at terminal G H . Consequently, V G (F H ) begins to rise, and V D begins to drop. At time t 2 , the helper FET is on, so V G (F H ) is high and V D is clamped at V C .
At time t 3 , switch 302 turns on the main FET. The main FET can be turned on before the helper FET is completely on, as long as the drain voltage has dropped to a level at which HCI is no longer a concern. Control circuit 304 turns on the main FET by asserting a high voltage V G (F M ) at terminal G M . At time t 4 , V D begins to fall from V C to V ON . At time t 5 , the main FET is on, so V G (F M ) is high and V D has reached V ON . As can be seen, control circuit 304 delays the main FET transition for a fixed delay time T D1 =t 3 −t 1 . Delay time T D1 can be increased by adding more buffer stages to control circuit 304 .
A turn-off transition is shown from time t 6 to time t 10 . At time t 6 , V G begins to fall. Switch 302 responds by turning off the main FET. Control circuit 304 turns off the main FET by asserting a low voltage V G (F M ) at terminal G M . Consequently, V G (F M ) begins to fall.
Depending on load conditions, V D may rise. The portion of the V D curve shown from time t 6 to time t 10 represents the maximum voltage V D is allowed to reach. Switch 302 keeps V D at or below this maximum.
At time t 7 , V D is restricted to at or below V C . At time t 8 , the main FET is off.
At time t 9 , switch 302 turns off the helper FET. The helper FET can be turned off before the main FET is completely off, as long as the drain voltage remains at a level at which HCI is no longer a concern. Control circuit 304 turns off the helper FET by asserting a low voltage V G (F H ) at terminal G H . Consequently, V D is no longer clamped at or below V C , and so V D may rise. At time t 10 , the helper FET is off, so V G (F H ) is low and V D can be high. As can be seen, control circuit 304 delays the helper FET transition for a fixed delay time T D2 =t 9 −t 6 . Delay time T D2 can be increased by adding more buffer stages to control circuit 304 .
As can be seen from FIG. 5, in the static state, the main FET and helper FET operate in parallel. However, their operations differ during the switching transient period. The helper FET turns on before the main FET turns on, thereby lowering the voltage across the main FET during its turn-on transition. The helper FET also turns off after the main FET turns off, thereby limiting the voltage across the main FET during its turn-off transition. Therefore, the main FET experiences no HCI stress.
Because the main FET is now free of the reliability design constraint, it can be designed for optimal electrical performance. For example, the main FET can use more aggressive design rules than the conventional FET not only to reduce the silicon area, but also to improve the efficiency of switch 302 . On the other hand, because the helper FET sustains all the HCI stress, it is designed for robust and reliable performance. The helper FET can use conventional or even more conservative design rules to achieve this performance.
The magnitude of the benefits of switch 302 is a function of the relative size (or channel width) of the main FET and the helper FET. Only the main FET portion contributes in terms of area saving and efficiency improvement. Therefore the smaller the helper FET is relative to the main FET, the greater the benefit.
The overall size of switch 302 , including both the main FET and the helper FET, is a function of the on-state voltage drop (V ON ) requirement. In switching applications, V ON typically is a very low voltage level. The helper FET alone is on to clamp the drain of the main FET at a voltage lower than the blocking voltage that it will otherwise sees in conventional switching. Blocking voltage is the voltage that the switch sustains in the off state. The relative size of the helper FET to the size of the helper FET and the main FET combined is inversely proportional to the ratio of clamped voltage (V C ) to V ON .
Hot-carrier injection quickly subsides as V C decreases from the blocking voltage. Therefore, V C can be much higher than zero while still being low enough to protect the main FET from hot-carrier stress. Indeed, V C in switch 302 actually has a much greater voltage range than conventional switching modes.
FIG. 6 depicts a circuit 600 for use in control circuit 304 according to another implementation. The inputs of a NAND gate 602 are coupled to terminals G and G H . The input of an inverter 604 is coupled to terminal G. The input of an inverter 606 is coupled to the output of NAND gate 602 . The output of inverter 606 is coupled to terminal G M . The output of inverter 604 is coupled to the input of an inverter 608 . The output of inverter 608 is coupled to terminal G H . As can be seen, circuit 600 delays the main FET transition for a fixed delay time T D1 =t 3 −t 1 . Circuit 600 implements the timing of FIG. 5 only for the turn-on transition of switch 302 .
FIG. 7 depicts a circuit 700 for use in control circuit 304 according to still another implementation. The input of an inverter 702 is coupled to terminal G. The inputs of a NOR gate 704 are coupled to terminals G and G M . The input of an inverter 706 is coupled to the output of inverter 702 . The output of inverter 706 is coupled to terminal G M . The output of NOR gate 704 is coupled to the input of an inverter 708 . The output of inverter 708 is coupled to terminal G H . Circuit 700 implements the timing of FIG. 5 only for the turn-off transition of switch 302 .
FIG. 8 depicts a circuit 800 for use in control circuit 304 according to yet another implementation. The input of an inverter 802 is coupled to terminal G. The inputs of a NOR gate 804 are coupled to terminals G and G M . The inputs of a NOR gate 806 are coupled to terminal D and the output of inverter 802 . The input of an inverter 808 is coupled to the output of NOR gate 804 . The output of inverter 808 is coupled to terminal G H . Circuit 800 implements the timing of FIG. 5 only for the turn-on transition of switch 302 .
Circuit 800 implements a variable delay T DV =t 3 −t 1 during the turn-on transition of switch 302 , when the effects of HCI are more severe than during the turn-off transition. The turn-on of the main FET is delayed until the drain voltage V D falls below a predetermined voltage. In this implementation, V C is designed to be within the range of an effective logic “low.” Circuit 800 implements a fixed delay T D2 =t 9 −t 6 during the turn-off transition of switch 302 .
In one implementation 304 includes a current sensing circuit. When the load current falls below a predetermined threshold, 304 shuts off main FET F M . Switching is then accomplished by helper FET F H alone.
For a given size for switch 302 , the conduction loss of switch 302 decreases with decreases in DC load current. When switch 302 is operated at light load current condition, the power losses incurred by charging up the gate capacitance of switch 302 (including both the main FET and the helper FET) may dominate the overall loss of switch 302 . Therefore the conduction loss of switch 302 becomes negligible, and the overall efficiency of switch 302 improves due to the dramatic reduction of gate capacitance and charging loss associated with the gate capacitance. In this situation, it is useful to disable the main FET and use the helper FET only.
FIG. 9 depicts a circuit 900 for use in control circuit 304 according to this implementation. The inputs of a NAND gate 902 are coupled to terminals G and G H ., and to the output of a current sensing circuit 910 . The inputs of a NOR gate 904 are coupled to terminals G and G M . The output of NAND gate 902 is coupled to the input of an inverter 906 . The output of inverter 906 is coupled to terminal G M . The output of NOR gate 904 is coupled to the input of an inverter 908 . The output of inverter 908 is coupled to terminal G H .
Current sensing circuit 910 outputs a logic high level when the drain current (that is, the current at drain D) is greater than a predetermined threshold current (indicating a normal load). Current sensing circuit 910 outputs a logic low level when the drain current is less than the predetermined threshold current (indicating a light load). Such current sensing circuits are well-known in the relevant arts. Circuit 900 thus operates in a manner similar to circuit 400 in FIG. 4 under normal loads. However, under light loads, circuit 900 keeps the main FET shut off at all times, while the helper FET is free to carry out the function of switch 302 .
The invention can be implemented in digital electronic circuitry, or in computer hardware, firmware, software, or in combinations of them. Apparatus of the invention can be implemented in a computer program product tangibly embodied in a machine-readable storage device for execution by a programmable processor; and method steps of the invention can be performed by a programmable processor executing a program of instructions to perform functions of the invention by operating on input data and generating output. The invention can be implemented advantageously in one or more computer programs that are executable on a programmable system including at least one programmable processor coupled to receive data and instructions from, and to transmit data and instructions to, a data storage system, at least one input device, and at least one output device. Each computer program can be implemented in a high-level procedural or object-oriented programming language, or in assembly or machine language if desired; and in any case, the language can be a compiled or interpreted language. Suitable processors include, by way of example, both general and special purpose microprocessors. Generally, a processor will receive instructions and data from a read-only memory and/or a random access memory. Generally, a computer will include one or more mass storage devices for storing data files; such devices include magnetic disks, such as internal hard disks and removable disks; magneto-optical disks; and optical disks. Storage devices suitable for tangibly embodying computer program instructions and data include all forms of non-volatile memory, including by way of example semiconductor memory devices, such as EPROM, EEPROM, and flash memory devices; magnetic disks such as internal hard disks and removable disks; magneto-optical disks; and CD-ROM disks. Any of the foregoing can be supplemented by, or incorporated in, ASICs (application-specific integrated circuits).
A number of embodiments of the invention have been described. Nevertheless, it will be understood that various modifications may be made without departing from the spirit and scope of the invention. For example, switch 302 can be implemented monolithically, or as two or more discrete components. The main FET, the helper FET, or both can be implemented as a single FET or as many FETs operating together. Switch 302 can be implemented using N-type MOSFETs or P-type MOSFETs. Switch 302 can be implemented to affect only the turn-on transition, only the turn-off transition, or both. Switch 302 can be implemented to drive capacitive, resistive or inductive loads. Accordingly, other embodiments are within the scope of the following claims. | A circuit, and a method and computer program product for use with a switch having a field-effect transistor (FET). The method and computer program product include restricting the drain-source voltage of the FET to a predetermined range; and then switching the FET. In general, in one aspect, the invention features a circuit having source, drain and gate terminals. The circuit includes a first FET having a first drain coupled to the drain terminal and a first source coupled to the source terminal; a second FET having a second drain coupled to the drain terminal and a second source coupled to the source terminal; and a control circuit coupled to the gate terminal, the first gate, and the second gate. | 7 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The invention is related to concentric casings and strings in wellheads wherein it is necessary to effect a seal between concentric members of the wellhead and is specifically directed to a seal system wherein the sealing members are activated via an external, non-invasive seal energizing system.
[0003] 2. Discussion of the Prior Art
[0004] In oil and gas wells, it is conventional to pass a number of concentric tubes or casings down the well. An outermost casing is fixed in the ground, and the inner casings are each supported from the next outer casing by casing hangers which take the form of inter-engaging internal shoulders on the outer casing and external shoulders on the inner casing.
[0005] Typically, such casing hangers are fixed in position on each casing. There are however applications where a fixed position casing hanger is unsatisfactory, because the hang-off point of one casing on another may require to be adjusted. Such drilling wellheads have to accommodate a casing with an undetermined hang-off point, it has been known to use casing slip-type support mechanisms.
[0006] Wellheads are used in oil and gas drilling to suspend casing, seal the annulus between casing strings, and provide an interface with the BOP. The design of a wellhead is generally dependant upon the location of the wellhead and the characteristics of the well being drilled or produced. One specific type of wellhead is a unitized wellhead for platform or land applications.
[0007] Unitized wellheads are composed of several individual components, including a wellhead housing that is used to support a number of casing hangers and tubing hangers. The hangers support the weight of the casing and tubing, and pass loads back to the wellhead housing. Annulus seals seal the annular spaces between casing and tubing strings.
[0008] Conventional land or platform wellheads are either slip-type conventional wellheads or through-the-BOP multi-bowl wellheads.
[0009] Slip-type wellheads use casing slips to support casing strings. These slips are friction wedges that “grip” the top of a casing string and use slip teeth to bite into the casing. Wellheads of this type require higher-risk operations, as they require lifting the BOP to install casing slips and annulus seals. The seals that are used with slip-type casing hangers must be actively maintained throughout the field life of the well.
[0010] Multi-bowl type wellheads feature reduced-risk operations, as the BOP does not need to be lifted to set casing slips. Instead of using slips, a multi-bowl wellhead uses a fixed landing shoulder in the wellhead housing to support the first casing hanger. All other casing hangers are stacked on top of this initial casing hanger. The seals installed on multi-bowl wellheads can be more dependable than those installed in slip-type wellheads, but are still often unreliable, due to eccentricities in the casing hanger/wellhead alignment and unreliability in the seal setting mechanisms. As the initial load shoulder must support the weight of all casing strings and any loads due to test pressures, this load shoulder must intrude into the bore of the wellhead quite a bit. This can create an operational restriction that limits operations through this well.
[0011] Various sealing devices are known and employed in such wellheads. One example of a sealing assembly is shown and described in U.S. Pat. No. 4,913,469, wherein a wellhead slip and seal assembly includes a slip assembly with slips supported within a slip bowl and a seal assembly positioned above the slip assembly and interconnected thereto for supporting the slip assembly, the seal assembly includes two segments connected to form the seal ring and each of the segments includes arcuate elements embedded in a resilient material which forms an inner seal in an inner groove. The segments of the slip bowl include segments interconnected by toe nails and the seal ring includes pin and recess connection for connecting the two segments together.
[0012] It is also known from European Patent No. 0 251 595 to use an adjustable landing ring on a surface casing hanger to accommodate a space-out requirement when the casing is also landed in a surface wellhead.
[0013] More recently, and as shown and described in my U.S. Pat. Nos. 6,092,596 and 6,662,868, an external clamp for clamping two concentric tubes, typically two concentric tubes in an oil or gas well, has two axially movable tapered components which can be pulled over one another in an axial direction to provide a contraction of internal diameter which grips the smaller diameter tube.
[0014] Another example of a sealing system is shown and described in U.S. Pat. No. 5,031,695, wherein a well casing hanger with a wide temperature range seal element is energized by axial compression with a pre-determined initial portion of the casing hang load, the remaining portion of that hang load then being transferred to the wellhead or other surrounding well element without imposition on the seal element.
[0015] U.S. Pat. No. 6,488,084 shows and describes a casing hanger adapted for landing on a load shoulder in a wellhead to seal and support a string of casing. The casing hanger has a lower ring for landing on the load shoulder, the lower ring having an upward facing surface. A plurality of circumferentially spaced recesses are in the upward facing surface of the lower ring, each of the recesses having a base. A seal is located on the lower ring and has a plurality of holes that register with the recesses in the upward facing surface of the lower ring. A slip assembly bowl has a wedging surface that carries a plurality of slip members. The slip members grip the casing and cause the bowl to transmit downward forces from the casing to the seal to axially compress and energize the seal. Fasteners extend from the lower ring through apertures provided in the seal into threaded apertures provided in a downward facing surface of the bowl to secure the lower ring to the slip assembly but allow relative axial movement between the bowl and the lower ring. A plurality of substantially cylindrical stop members are located in the holes in the seal and in the recesses of the lower ring. The stop members are secured into threaded holes formed in the shoulder ring and contact the bases of the recesses to limit the compression of the seal to a predetermined amount.
SUMMARY OF THE INVENTION
[0016] The subject invention is directed to a method and apparatus for a seal assembly for a unitized wellhead system for land or platform applications utilizing a friction grip technology to create maintainable metal-to-metal seals with finely-controlled contact stresses, lock-down casing and tubing hangers, support test loads to minimize the size of landing shoulders required, and to rotationally lock casing hangers to provide simplified running procedures.
[0017] The subject invention that combines the benefits of a slip-type wellhead and a multi-bowl type wellhead and is able to provide numerous advantages by using radial compression of the wellhead to create seals and support load.
[0018] In its simplest form, the invention provides the apparatus and method for accomplishing a circumferential seal between two substantially concentric members by externally activating the seal once the two members are in position. In a typical configuration, a wellhead housing accommodates and supports a concentric tubing hanger. The tubing hanger may be supported within the wellhead in any of the conventional ways.
[0019] One suitable method for supporting the tubing hanger in the well is the clamping mechanism shown and described in my previously mentioned U.S. Pat. Nos. 6,092,596 and 6,662,868, incorporated herein by reference. Using the system there described, a friction fit is provided between the inner diameter of the wellhead housing and the outer diameter of the tubing hanger. Once properly positioned, a compressor system mounted on the exterior of the wellhead housing is activated, whereby the a cam or ramp surface on the compressor system is moved axially relative to a mated cam surface on outer circumference of the wellhead housing to compress the wellhead housing radially inward for engaging and clamping the tubing hanger along coextensive surfaces.
[0020] The present invention is directed to a sealing mechanism comprising a compression system such as that shown in my aforementioned patents, metal-to-metal sealing members, and where desired, redundant resilient seals. In the preferred embodiment the sealing members are integral, machined surface on the outer circumferential wall of the tubing hanger and inner circumferential wall of the wellhead housing.. The sealing surface extends circumferentially about the walls. The sealing surface of the tubing hanger is best designed to clear the inner diameter of the wellhead housing, i.e., there is not any radial interference between the sealing surface of the tubing hanger and the interior wall of the wellhead housing. This preserves the integrity of the seal during assembly. Once the tubing hanger is positioned in the wellhead housing, the seal is activated by the compressor system., compressing the wellhead housing radially inward to engage the seal.
[0021] The sealing assembly of the subject invention provides for a flexible design that can be used for a variety of specific applications, as will be described herein. The simple design promotes dependability and reduces size of the overall architecture of the well. The resulting wellhead assembly has near-zero eccentricity between hangers and housing with near-zero torque and minimal axial setting load required to energize metal-to-metal annular seals The sealing assembly may include external test capability for metal-to-metal annular seals.
[0022] It is an important aspect of the invention that the sealing mechanism is activated by external lockdown and sealing activation. The rigid lockdown eliminates annular seal fretting, with contact stress evenly distributed around seal perimeter.
[0023] The sealing assembly permits controlled and monitored application of seal loading.
[0024] The annular seals are maintainable throughout field life.
[0025] A minimal number of running tools are required since hangers are locked in place torsionally. A high-torque connection, e.g., a standard casing coupling on the end of a standard casing string, can be used to run the hangers.
[0026] It is an important feature of the design that the primary load shoulder can be smaller than conventional multi-bowl load shoulders, as much of the load is supported through the various friction-grip interfaces. This smaller load shoulder means that the bore through the wellhead is increased, allowing the first casing string run through the wellhead to be larger in size. Alternately, a smaller load shoulder can allow the outer diameter of the wellhead to be decreased while maintaining the diameter of the casing, resulting in a smaller overall size.
[0027] The friction and gripping areas function over a length. Therefore, if the first casing hanger is landed high, subsequent casing/tubing hangers can tolerate this stack-up error by landing and sealing at slightly different places along the functional bore length.
[0028] The tubing hanger can be nested to reduce the work-over stack dimension.
[0029] The friction grip area supports test loads on the tubing hanger permitting the tubing hanger load shoulder to be smaller than it prior art configurations. More space is then available in the tubing hanger to maximize the number of control line penetrations through the tubing hanger.
[0030] The design of the subject inventions minimizes the number of wellhead penetrations. All contingency procedures can be performed through the blow out preventers (BOP's).
[0031] Due to minimizing stress and torque, the system is a fatigue resistant design for dynamic applications. The flexible design allows incorporation of tensioned casing and tubing hangers.
[0032] In the preferred compression system, the use of hydraulic pistons and lock nuts to activate and lock the flanges allows for a simplified flange design.
[0033] The push-through wear bushing does not need to be retrieved, saving an operation.
[0034] Internal tubing hanger lockdown can be accomplished without a dedicated handling tool and without potential control line damage Improved safety, with tubing back-side test, is achieved without the use of a temporary seal or temporary lockdown mechanism on tubing hanger.
[0035] Other features of the invention will be readily apparent from the accompanying drawings and detailed description of the preferred embodiment.
BRIEF DESCRIPTION OF THE DRAWINGS
[0036] FIG. 1 is a simplified cross-section of a wellhead showing the seal system in detail.
[0037] FIG. 2 is a cross-section of a typical wellhead configuration incorporating the seal system of the subject invention.
[0038] FIG. 3 is an enlarged fragmentary view of the seal system of FIG. 1 , and corresponds generally to FIG. 1 .
[0039] FIGS. 4 is a cross-section of a typical wellhead configuration incorporating the seal system of the subject invention with the tubing hanger nested to reduce the work-over stack dimension.
[0040] FIG. 5 is a cross-section of the wellhead of FIG. 4 taken at a 90 degree rotation from that of FIG. 4 .
DESCRIPTION OF THE INVENTION
[0041] A simplified, diagrammatic view of the seal system to the subject invention is shown in FIG. 1 . In its simplest form, the invention provides the apparatus and method for accomplishing a circumferential seal between two substantially concentric members by externally activating the seal once the two members are in position.
[0042] With specific reference to FIG. 1 , a wellhead 1 includes having an external sealing apparatus 10 for clamping a tubular casing 4 of a first diameter within a tubular casing (here the wellhead 1 ) of larger internal diameter. The outer tubular member has an inner circumferential wall with a sealing zone 83 . The inner tubular member is adapted to be positioned substantially concentrically within the outer tubular member having an outer circumferential wall with a sealing zone 28 . The circumferential compression system 10 is mounted outwardly of the outer tubing member and operable to be activated for compressing the outer tubular member into contact with the inner tubular member for engaging the sealing zones therein and activating a seal between the outer tubular member and the inner tubular member. The sealing zone on each tubular member may be a metal sealing surface on each of said tubular members for defining a metal-to-metal seal when the compressions system is activated. Where desired, the wellhead sealing system may include one or more resilient seal members 84 , 85 in the sealing zone of one of the tubular members and extending outwardly therefrom toward the other tubular member, wherein the resilient seal member is adapted to be compressed between the two tubular members when the compression system is activated. Where multiple resilient sealing members are used, a gap 91 is created between the resilient seal members when the compression system is activated. A test port 114 may be provided for communicating the gap with the exterior of the assembly for testing the integrity of the seal when activated. In the preferred embodiment the compression system comprises a wedge surface 15 and a flange 14 adapted for engaging the wedge, one of said wedge and flange being each located on one of the outer tubular member and the compression system, whereby the tubular member is compressed radially inwardly upon relative axial movement between the wedge and the flange. The preferred method for activating the compression system is a hydraulic ram adapted for causing axial movement between the wedge and the flange. The system includes a positive lock 21 for locking the wedge and flange in position once the seal has been engaged.
[0043] In its broadest sense the invention is a method for providing an external sealing device for concentric tubular members in a wellhead. The method comprises placing sealing zones on the mated surfaces of a plurality of concentric tubular members in radial alignment with one another and compressing the outermost tubular member toward the central axis of the concentric tubular members for engaging the sealing zones with one another. As described above, in the preferred embodiment the method includes the step of locking the compressed assembly in sealing position. Where desirable, a redundant resilient seal is positioned in the sealing zone. When a plurality of axially spaced resilient seals are located in the sealing zone, the gap between the resilient seals may be ported to the exterior of the system.
[0044] As shown in FIG. 1 , and by way of example, a wellhead housing 1 accommodates and supports a concentric tubing hanger 4 . As will be further described, additional concentric tubular members may also be sealed using the system of the subject invention. The tubing hanger may be supported within the wellhead in any of the conventional ways. One suitable method for supporting the tubing hanger in the well is the clamping mechanism shown and described in my earlier U.S. Pat. No. 6,092,596, incorporated herein by reference. Using the system therein described, a friction fit is provided between the inner circumferential wall 83 of the wellhead housing and the outer circumferential wall 28 of the tubing hanger 4 . Once properly positioned, the compressor system 10 mounted on the exterior of the wellhead housing 1 is activated by the threaded driver 20 , 21 , whereby the compression flange 14 on the compressor system is moved axially relative to the compression wedge 15 on outer circumference of the wellhead housing to compress the wellhead housing radially inward for engaging and clamping the tubing hanger along the coextensive surfaces 28 and 83 . As shown in my aforementioned patents, the compression system may comprise an annular, axially tapering surface, an axially movable sleeve surrounding the outer wall of the wellhead and has a corresponding tapering surface facing the outer wall, and a driver for producing relative axial movement between the tapering surfaces to exert a radial compressive force to the outer wall of the wellhead. The means for producing relative axial movement comprises a pressure chamber between the sleeve and the wellhead, and means for pressurising the chamber with hydraulic pressure. Alternatively, the means for producing relative axial movement may comprise a flange on the sleeve, a flange on the wellhead, and means for applying a mechanical force between the flanges to move the sleeve axially along the wellhead.
[0045] The present invention is directed to the sealing mechanism comprising the compression system 10 , the metal-to-metal sealing member 29 , and where desired, redundant resilient seals 84 and 85 . In the preferred embodiment the sealing member 29 may is an integral, machined surface on the outer wall 28 of the tubing hanger. The sealing surface extends circumferentially about the outer wall of the tubing hanger. The sealing surface is best designed to clear the inner wall of 83 of the wellhead housing, i.e., there is not any radial interference between the sealing surface of the tubing hanger and the interior wall of the wellhead housing. This preserves the integrity of the seal during assembly. Once the tubing hanger 4 is positioned in the wellhead housing 1 , the seal is activated by driving the compression flange 14 of the compressor system 10 relative to the compression wedge 15 mounted on the wellhead housing 1 , forcing the wellhead housing to compress radially inward about the entire circumference and engage the seal.
[0046] In the preferred embodiment, the metal-to-metal seal includes mated and complementary sealing surfaces 29 and 90 on both the exterior wall of the tubing hanger and the interior wall of the wellhead housing.
[0047] Resilient back up seals 84 , 85 may also be provided. As shown in FIG. 1 , the exterior wall of the tubing hanger includes channels 86 , 87 , for receiving an the resilient o-ring type resilient seal 84 , 85 . The channels and o-rings could also alternatively be housed in the interior wall of the wellhead housing. The resilient seal system is also activated by the compressor system 10 .
[0048] It is also desirable to provide a seal test port 114 in communication with the seal for testing its integrity once activated.
[0049] The seals are released by decompressing the compressor system 10 to withdraw the ramp surface 14 axially downward from the ramp surface 16 via the screw drive system 21 . The drive means may be any of a number of systems which support the exertion of circumferential pressure on the outer wall of the wellhead. Examples of such systems are shown and described in my U.S. Pat. No. 6,662,868 and copending application U.S. Ser. No. 10/721,443. All of these are incorporated by reference herein.
[0050] It is, therefore, the essence of the invention to provide a sealing mechanism for sealing the annulus between two relatively concentric tubular members by activating and engaging a sealing member via an external force applied to the assembly for compressing the outer member into the inner member.
[0051] It should be noted that the seal mechanism must be distinguished from the clamping mechanism described in the aforementioned patents. As will be readily understood, sufficient clamping can be accomplished by compressing the outer member into the inner member whether or not full circumferential contact is achieved. It is the important enhancement of the subject invention that means are provided to assure complete contact along the circumferential walls of the two member to effect a seal once the compression is completed.
[0052] FIG. 2 depicts a simple configuration of a three-string wellhead system utilizing the clamping system of my aforementioned patents and the sealing system of the present invention. The main components of this system are a wellhead housing 1 , a production casing hanger 2 with annulus seal assembly 3 , and a tubing hanger 4 . The entire assembly is supported on a base plate 5 that sits on the conductor string 6 .
[0053] A load shoulder 37 on the support plate supports the wellhead housing. The wellhead housing 1 supports the weight of the intermediate casing string 7 in a traditional manner (in this case, via a threaded casing coupling connection in the bottom of the wellhead housing). The exterior of the wellhead housing features two sets of annulus access ports 8 and 9 , two clamping compression systems 10 and 11 , a control-line access port 12 , two sets of external seal test ports 113 and 114 , and a thread-on flange profile up. A thread on flange 35 attaches to this profile to interface with the tree adapter 33 .
[0054] The bore of the wellhead housing is featured with a number of sealing profiles and lockdown profiles for the casing hanger, seal assembly, and tubing hanger. These bores may be on a series of steps so that each higher bore is on a slightly larger diameter, therefore protected from operations on the smaller diameter bores. At the top of the wellhead housing bore is an index shoulder 22 for the tubing hanger neck seal and a gasket sealing profile. At the bottom of the wellhead housing bore is a load shoulder 23 that is sized to support the casing weight of the production casing string only. Any additional axial load (for instance load from other casing strings or from test pressures) passes through the friction-grip lockdown areas.
[0055] The production casing hanger 2 features a casing thread profile down for support of the production casing string 24 and a casing thread profile up to interface with the casing hanger's casing running string (not shown). The exterior of the casing hanger features a load shoulder that is slotted to allow flow-by and cement returns to pass the exterior of the casing hanger as it is being run. The external surface of the load shoulder area 25 is a controlled surface featuring a friction profile. When the casing hanger is landed, this friction surface is parallel to a mating surface in the bore of the wellhead housing. External compression of the wellhead housing provided by the lower compression cartridge 11 forces the two surfaces to be perfectly concentric and brings them into contact. Friction at this interface provides rotational and axial lock-down support for the casing hanger, as well as additional load support for production casing weight and test loads on the production casing hanger. Above the casing hanger load shoulder is a profile for the annulus seal system 3 .
[0056] The annulus seal 3 fits between the production casing hanger 2 and the inner bore of the wellhead housing 1 . The seal features two sets of seal profiles 115 , 116 on both the inner and outer diameters, respectively. The outer diameter and inner diameter seal profiles feature two pairs each of metal-to-metal seals as well as resilient seal back-ups 118 , 119 . A port 113 between the two sets of seals allows external testing of all seals created by the seal assembly. These seal profiles do not have initial radial interference with either the casing hanger or the wellhead housing. Rather, interference (and radial contact pressure) is provided by external compression of the wellhead housing through the use of the lower compression cartridge 11 . An extended neck 120 on the seal assembly protrudes above the top of the casing hanger. This extended neck features ports 122 to allow communication between the production/tubing annulus and the upper annulus access port 8 in the wellhead housing. The top of the seal assembly serves as a landing shoulder 124 for the tubing hanger 4 at load shoulder 26 .
[0057] The tubing hanger 4 supports the tubing string 27 with a threaded connection down. The thicker main body 125 of the tubing hanger provides a load shoulder 26 that lands on top of the production casing hanger annulus seal assembly on landing shoulder 124 . This load shoulder supports full tubing string weight only. Any additional axial loads (for instance, loads due to test pressure) are supported by the friction-grip lockdown area. The outer diameter of the thick section 125 of the tubing hanger features a friction-lock profile 28 below a sealing profile 29 . The friction profile is a machined surface suitable for support of friction loads. The sealing profile consists of a pair of metal-to-metal seal bumps with resilient back-ups, as described with above and shown more clearly in FIGS. 1 and 3 . Both of these profiles are parallel to mating surfaces on the wellhead housing bore, and have no initial interference. When the upper compression cartridge 10 is activated, that section of the wellhead housing is compressed inwards to contact the tubing hanger. Contact pressure along this interface forces the pieces to be concentric, provides axial and rotational lockdown of the tubing hanger, and activates the metal-to-metal seals with resilient back-ups. The friction interface supports any test pressure loads on the tubing hanger.
[0058] Hydraulic control lines 30 pass through the tubing hanger body in a conventional manner. The tubing hanger features an extended neck 126 upwards. This neck features a tubing connection box up to interface with the tubing running string (not shown). Below this threaded box is a seal profile to accept the tubing hanger neck seal.
[0059] The tubing hanger neck seal 31 sits on a support ring 32 that is carried on the tubing hanger neck and indexes on a load shoulder in the wellhead housing bore. The seal sits on the upper face of this support ring, and features metal-to-metal seal profiles on both the straight inner diameter and the tapered outer diameter. A port 127 between these seal profiles allows external testing of all seals created by the tubing hanger neck seal via an external test port 36 in the Christmas tree adapter 33 . This seal is activated as the Christmas tree adapter 33 is drawn by studs and nuts 34 down onto the wellhead housing. Movement over the tapered external surface of the tubing hanger neck seal compresses the seal inwards and creates high radial contact pressures on both the seal inner diameter and the seal outer diameter.
[0060] FIG. 3 is an enlarged a detail of the system shown in FIG. 2 , generally in the area of the upper compressor system 10 . FIG. 3 is generally of the same cross-section of FIG. 1 , but with all of the detail of the wellhead housing of FIG. 2 .
[0061] Each POS-GRIP compression system is composed of a compression flange 14 and a compression wedge 15 . The compression flanges are rings with tapered inner surfaces that mate with the tapered outer surfaces of the compression wedges. Axial movement of the compression flanges over the compression wedges compresses the compression wedges inwards, in turn compressing a portion of the wellhead housing 1 inwards (within the wellhead housing's elastic range). The compression systems may be configured with a split spacer ring 16 between the compression wedge and the wellhead housing, as shown in the top compression system 10 of FIG. 2 . The split spacer rings have minimal hoop stiffness, and simply pass the radial contact loads from the compression wedge into the wellhead housing.
[0062] The compression flanges have handling profiles 17 on the flange outer diameters. These handling profiles interface with a release tool (not shown) that can be used to push the flanges apart, releasing the compression. The compression flanges also have activation and locking profiles 18 cut into the wide end of the flanges. These profiles accept a set of small hydraulic pistons (not shown) during activation. These hydraulic pistons react against the thick section of the wellhead housing in the region of the upper annulus access port 8 , see FIG. 2 . When pressure is applied to a set of hydraulic pistons, the associated compression flange is pushed away from the thick section of the wellhead housing into the “activated” position. Once the compression flange has been moved into its activated position, mechanical lock nuts 19 replace the hydraulic pistons in the locking profiles, and are used to lock the flange in the activated position.
[0063] The lock nuts consist of a male thread member 20 and a female thread member 21 . The male thread member has a threaded length and a flat face at one end to sit on the wellhead housing. The female thread member has threads to mate with the male thread member and a flat face to react on the compression flange. Rotation of the female thread member on the male thread member allows the lock nut to adjust in length, to fill whatever gap is developed between the wellhead housing and the compression flanges during activation of the compression system. Once the lock nut has been adjusted to the necessary length, it effectively locks the compression flange in its current position, so that the hydraulic pistons may be removed.
[0064] FIGS. 4 and 5 depict two separate sections of a more involved configuration of a four-string wellhead. The main components of this system are a wellhead housing 38 , a push-through wear bushing 39 , an intermediate casing hanger 40 with annulus seal assembly 41 . The annulus seal assembly is of the same configuration as that shown in FIG. 2 and is activated in a similar manner by the lower compression system 11 . There is also a production casing hanger 42 , a seal and support sub 43 , and a tubing hanger 44 .
[0065] The assembly shown in FIGS. 4 and 5 uses an alternate means of wellhead support. In this case, the entire assembly is supported on a friction support mechanism 45 that connects the bottom of the wellhead housing to the top of a large-diameter casing string 46 . The friction support mechanism consists of a gripping sub 47 , a compression sub 49 , and a set of studs and nuts 50 . This gripping system comprising gripping sub 47 , compression sub 49 and the driver 50 , operates in accordance with the gripping system shown and described in my aforementioned patents. The gripping sub is connected to the inner diameter of the wellhead housing 38 via a threaded profile at 130 with a metal-to-metal seal. The lower portion 131 of the gripping sub consists of a friction and sealing profile on the inner diameter and a tapered surface on the outer diameter. The friction profile diameter fits as a socket around the casing string 46 . The tapered diameter mates with a tapered surface on the compression sub 49 . As the compression sub moves upwards over the taper, the gripping sub is compressed inwards. This closes the gap between the gripping sub and the outer diameter of the casing, and creates a high radial contact pressure between the two pieces. This high radial contact pressure provides a metal-to-metal seal between the gripping sub and the casing. Friction at this interface locks the pieces together axially and rotationally.
[0066] A set of studs and nuts 50 connect the compression sub 49 to the wellhead housing 38 . It is movement of the nuts along the studs that causes the compression sub to move upwards along the tapered compression sub/gripping sub interface.
[0067] The wellhead housing 38 is largely the same as that shown in FIG. 2 . The wellhead housing in FIGS. 4 and 5 features a third annulus access port 52 ( FIG. 4 ) to allow access to the additional annulus created in the four-string configuration. This annulus access port is located at 90 degrees from the production casing/intermediate casing annulus access port 51 ( FIG. 5 ). Both ports may be located at the same height as shown in these drawings. There is also one additional test port 52 ( FIG. 4 ) through the wellhead housing to test an additional set of seals 135 on the tubing hanger.
[0068] This wellhead housing also demonstrates a different means of providing a reaction point for the hydraulic activation pistons and mechanical lock nuts. Instead of having a very thick section integral to the wellhead housing (as was shown in FIG. 2 ), this wellhead housing features a series of split flange sections 54 that fit in a dovetail groove 55 in a slightly thicker portion 136 of the wellhead housing. These flanges may then be bolted into place. At locations where annulus access port passes through the wellhead housing, a flat is machined to allow an annulus access valve to be bolted in place.
[0069] This system is used with a push-through wear bushing. This wear bushing protects the wellhead bore when drilling for the intermediate casing string. The wear bushing 39 is simply a thin sleeve with a thick top section. The bottom of the thin sleeve passes through the wellhead housing minimum inner diameter. A set of resilient seals 57 at the top of the wear bushing 39 prevents fluids from entering the protected area. The wear bushing may be supported in one of two ways. First, a pin through one of the annulus access ports can latch into a profile on the outer diameter of the wear bushing. This pin can then be removed when the wear bushing is ready to be moved out of the way. Alternately, the thick upper portion of the wear bushing may be gripped by the compression system 11 . This system is released when the wear bushing is ready to be moved out of the way.
[0070] The thicker portion at the top of the wear bushing serves as a load shoulder 138 for the intermediate casing hanger. The wear bushing is released when the intermediate casing hanger is run. The load shoulder 140 on the intermediate casing hanger lands on the top of the mating load shoulder on the wear bushing and pushes the wear bushing downwards until the thick portion of the wear bushing is sandwiched between the lower load shoulder 142 on the wellhead housing and the load shoulder 140 on the intermediate casing hanger. These shoulder thicknesses are all sized to support full intermediate casing weight only. Any additional load on the intermediate casing hanger (due to loads from additional casing strings and seal test loads) is supported by the friction interface which is activated by the compression system 11 .
[0071] The intermediate casing hanger 150 and intermediate casing hanger seal assembly 41 are largely identical to the production casing hanger 2 and production casing hanger annulus seal assembly 3 as discussed in FIG. 2 . The intermediate casing hanger features a profile 58 on the inner diameter to land the production casing hanger 42 . As a hanger does not land on top of the annulus seal as one did in the configuration of FIG. 2 , the annulus seal is shorter, and does not have the requirement of ports for annulus access.
[0072] The production casing hanger 42 features a casing thread profile down for support of the production casing string 59 . At the top end of the production casing hanger, there is a casing coupling box 152 to interface with the seal and support sub 43 and an external running thread profile to interface with the casing hanger's running tool (not shown). The exterior of the production casing hanger features slots to allow flow-by and cement returns to pass as the hanger is being run.
[0073] Held in a profile on the exterior of the production casing hanger is a split-ring landing mechanism 60 ( FIG. 5 ). This outwardly biased split ring is held inwards by the casing hanger running tool while the hanger is being run. This allows the production casing hanger to pass completely through the bore of the intermediate casing hanger, and then be pulled back to the mating landing profile, thus applying tension to the production casing string. When the production casing hanger is properly located in the bore of the intermediate casing hanger, the outwardly-biased split ring is disengaged from the running tool. The split ring springs outwards and engages the mating profile in the bore of the intermediate casing hanger. This split ring supports intermediate casing string weight only. Any additional loads on the intermediate casing hanger (for instance, loads due to the tubing string or any seal test loads) are carried by the seal and support sub.
[0074] The seal and support sub 43 has a casing coupling pin down. This threaded and sealing connection is made up to the mating box 152 in the top of the production casing hanger 150 . On the inner diameter above this coupling is a running profile 61 to mate with a running tool (not shown). Above this running profile, ports 62 ( FIG. 4 ) pass from the seal and support sub inner diameter to the outer diameter to allow communication between the production casing/tubing annulus and the annulus access port 156 .
[0075] At the outer diameter of the seal and support sub, these ports pass between a pair of metal-to-metal seals at seal assembly 160 . The outer diameter of the seal and support sub features four sets of metal-to-metal seals 162 with resilient backup 63 . The annulus access ports pass between the middle set of seals. The set of seals on either side of the annulus access port straddle external test ports in the wellhead housing wall, enabling testing of all sets of seals. Below all of these sealing profiles is a friction profile 64 , consisting of a machined surface suitable for support of friction loads.
[0076] Both of these profiles are parallel to mating surfaces on the wellhead housing bore, and have no initial interference. When the upper compression cartridge 165 is activated, that section of the wellhead housing is compressed inwards to contact the seal and support sub. Contact pressure along this interface forces the pieces to be concentric, provides axial and rotational lockdown of the seal and support sub, and activates the metal-to-metal seals with resilient back-ups. The friction interface supports any test pressure loads on the seal and support sub and any weight from the tubing hanger.
[0077] The inner diameter of the support sub is a bowl that serves as a landing shoulder 170 for the tubing hanger 65 . Above this landing shoulder is a bore with both a friction grip profile 66 and a sealing profile 67 for the tubing hanger.
[0078] The tubing hanger 65 is very similar to the tubing hanger 4 shown in FIG. 2 . The tubing hanger 65 has a reduced outer diameter, allowing it to be run through a smaller blow out preventer (BOP) . This smaller tubing hanger is landed, locked down, and sealed inside the seal and support sub rather than inside the wellhead housing bore. In order to have capability to test the metal-to-metal seals on the tubing hanger outer diameter, a port 68 in the tubing hanger passes from the top face to intersect a test port that passes between the two sets of seals on the tubing hanger outer diameter.
[0079] To activate the seals and friction grip inside the seal and support sub requires a two-stage operation of the upper compression system 165 . The first stage of activation compresses the wellhead housing inwards to grip, support, and seal the seal and support sub. During the second stage of activation, the compression system is activated further. This additional activation compresses through the seal and support sub, compressing the inner diameter of the seal and support sub inwards to grip the tubing hanger. This second-stage compression provides the force necessary to activate the metal-to-metal seals and the friction-grip support. The tubing hanger neck seal is identical to that shown FIG. 2 . From the foregoing description it will be readily understood that the platform wellhead design of the subject invention has numerous enhancements and features providing substantial advantages over the wellhead designs of the prior art. The wellhead as described herein achieves these advantages by moving load support and seal energization functions to the exterior to the wellhead housing. This results in maximization of useable bore space and excellent control of annular seal loading. These improvements result in the following advantages and features, among others:
flexible design can be used for a variety of specific applications. Simple design promotes dependability and reduces size. Zero eccentricity between hangers and housing. Zero torque and minimal axial setting load required to energize metal-to-metal annular seals. External test capability for metal-to-metal annular seals. External lockdown and sealing activation Rigid lockdown eliminates annular seal fretting. Contact stress evenly distributed around seal perimeter. Controlled and monitored application of seal loading. Annular seals maintainable throughout field life. Minimal number of running tools required-since hangers are locked in place torsionally, a high-torque connection (in this case a standard casing coupling on the end of a standard casing string) can be used to run the hangers. The primary load shoulder can be quite a bit smaller than conventional multi-bowl load shoulders, as much of the load is supported through the various friction-grip interfaces. This smaller load shoulder means that the bore through the wellhead is increased, allowing the first casing string run through the wellhead to be larger in size. Alternately, a smaller load shoulder can allow the outer diameter of the wellhead to be decreased, resulting in a smaller overall size. The friction and gripping areas function over a length. Therefore, if the first casing hanger is landed high, subsequent casing hangers/tubing hangers can tolerate this stack-up error by landing and sealing at slightly different places along the bore length. As shown in FIG. 4 , the tubing hanger can be nested to reduce the work-over stack dimension. Due to the fact that the friction grip area supports test loads on the tubing hanger, the tubing hanger load shoulder can be smaller than it would normally be. This means that more space is available in the tubing hanger to maximize the number of control line penetrations through the tubing hanger. Minimum number of wellhead penetrations. Contingency procedures can all be performed through the BOP's. Fatigue resistant design for dynamic applications. Flexible design allows incorporation of tensioned casing and tubing hangers (for instance as shown in FIG. 4 ). Use of hydraulic pistons and lock nuts to activate and lock flanges allows simple flange design. Push-through wear bushing does not need to be retrieved, saving an operation. Internal tubing hanger lockdown without dedicated handling tool and potential control line damage Improved safety, with tubing back-side test achieved without use of temporary seal or temporary lockdown mechanism on tubing hanger.
[0102] While certain features and embodiments of the invention have bee described in detail herein, it should be understood that the invention includes all modifications and enhancements within the scope of the following claims. | A method and apparatus for a seal assembly for a unitized wellhead system for land or platform applications utilizes a friction grip technology to create maintainable metal-to-metal seals with finely-controlled contact stresses, lock-down casing and tubing hangers, support test loads to minimize the size of landing shoulders required, and to rotationally lock casing hangers to provide simplified running procedures. The system can be used in combination with a friction grip clamping assembly to greatly streamline the wellhead design. | 4 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a method for detecting hepatitis C virus using hybridomas.
[0003] 2. Description of the Background
[0004] Hepatitis C virus (HCV) is an enveloped positive strand RNA virus, recognized as the major etiologic agent of blood-borne and sporadic non-A, non-B hepatitis. Due to the propensity of this virus to cause chronic infections, and its association with liver cirrhosis and hepatocellular carcinoma, HCV is a significant world-wide health problem.
[0005] HCV has a single strand positive sense RNA genome of approximately 9,400 nucleotides in length. The virus has a lipid-containing envelope that is chloroform-sensitive and appears to be necessary for replication. HCV is similar to members of the Flaviviridae family in overall genome organization and in the presumed mechanism of replication. Particularly, HCV genome codes for a single polyprotein precursor of about 3,000 aminoacids that is cleaved into a series of proteins including capsid, two envelope proteins E1 and E2 and 7 putative non-structural proteins some of which are involved the polyprotein processing. Although the entire HCV genome has been sequenced, see Chiron patents: EP 318216, EP 388,232 and PCT WO 90/1443, and the viral proteins and their processing have been well characterized in vitro, little is currently known about the mechanism of HCV infection which leads to viral persistence despite a broad immunological response to viral structural and non-structural proteins. Current diagnoses of HCV infection are based on the detection of viral RNA in serum by polymerase chain reaction (PCR) and antibodies against HCV components by the assays involving multiple HCV recombinant proteins and/or synthetic peptides. However, there are no available diagnostic assays for detection of the structural proteins of circulating virus. The polypeptide composition, antigenic structure of the virion and number of the possible viral serotypes remain unknown.
[0006] Putative HCV virion is about 50-60 nm in diameter and is composed of a viral envelope and a 33 nm core. HCV core protein is a highly basic and is mapped to the first 191 aa residues of the HCV polyprotein. This region is well conserved between different HCV isolates and genotypes and shows high degree of homology with nucleocapsid proteins of other flaviviruses. Viral encapsulation requires the self-association and the capacity to interact with the viral RNA. The interaction sites with homologous and heterologous RNA has been mapped to the N-terminal region of the core protein, whereas the main homotypic interaction domain has been mapped to the tryptophan rich aa sequence (73-108). The hydrophobic signal sequence for translocation of El protein into the endoplasmic reticulum is located in the C-terminal part aa (170-191) and is apparently cleaved by proteases associated with cellular membranes at aa 172. Besides its role in viral replication. HCV core protein has many important biological functions, such as modulation of transcription from several cellular promoters , suppression of the HBV gene expression, interaction with the cytoplasmic tail of lymphotoxin receptor and others.
[0007] With equilibrium centrifugation and immunoprecipitation studies, it has been demonstrated that HCV populations in serum consist of low density virions associated with P-lipoproteins which are infectious in cultured cells and of the high density fraction that might contain either immune complexes or naked HCV nucleocapsids. Although, several groups have reported the detection of the core antigen by immunological methods in virus-enriched serum samples from HCV-infected individuals after detergent treatment, no free core antigen has yet been isolated from serum and characterized immunochemically.
[0008] To date, the two basic tests for HCV are i) PCR, and ii) detection of antibodies in patient serum. However, a need exists for an improved means of detecting HCV.
SUMMARY OF THE INVENTION
[0009] Accordingly, it is an object of the present invention to provide a method of directly detecting HCV in serum of a patient, which represents a surprising improvement over the conventional tests for HCV.
[0010] It is also an object of the present invention to provide a method of detecting non-enveloped nucleocapid or non-enveloped core protein of HCV in serum of a patient.
[0011] The above objects and others are provided by a method of directly detecting hepatitis C virus in serum of a patient by detecting the virus with primers corresponding to viral RNA encoding core protein which RNA is a light fraction of the total viral RNA, the light fraction being isolated after ultracentifugation in a CsCl gradient of human serum containing HCV virus, the light fraction containing most of the circulating infectious HCV virus particles, which method entails precipitating RNA, effecting reverse transcription and then effecting amplification with the primers described herein.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] [0012]FIG. 1 illustrates HCV-RNA determination by RT-PCR and b-DNA assay.
[0013] [0013]FIG. 2A illustrates the activity of monoclonal antibody (MAb)VT against HCV core protein.
[0014] [0014]FIG. 2B illustrates the activity of monoclonal antibody (MAb) 39-72 against HCV core protein.
[0015] [0015]FIG. 3A illustrates a mapping of epitopes recognized by MAb 39-72 using a panel of synthetic peptides.
[0016] [0016]FIG. 3B illustrates an epitope analysis of HCV core protein.
[0017] [0017]FIG. 4 illustrates that MAb VT and MAb 39-72 recognize different, non-overlapping epitopes of HCV core protein.
[0018] [0018]FIG. 5 illustrates the results of ELISA for HCV-core protein.
[0019] [0019]FIG. 6 illustrates lack of inhibition of MAb 39-72 used in the assay for core antigen by human globulins containing anti-core antibodies.
[0020] [0020]FIG. 7 illustrates the results of Western-Blot analysis of the anti-HCV-core IgM MAb.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0021] The present invention provides a surprisingly improved method for detecting HCV. In more detail, the present invention provides a method of detecting HCV by visualization of the presence of core protein by a double sandwich test using at least monoclonal antibodies produced by the hybridoma of the present invention.
[0022] Hereinbelow is both a general and detailed description of the present invention involving the detection and immunological characterization of the free core antigen circulating in plasma of HCV carriers. Monoclonal antibodies were prepared by immunization of mice with a natural, serum-derived HCV nucleocapsid and applied for detection of HCV core in serum and liver tissue of HCV infected chimpanzees.
[0023] Material and Methods
[0024] Measurement of HCV RNA by RT-PCR
[0025] HCV RNA in serum and fractions of the gradients was determined by nested polymerase chain reaction (PCR) based on the amplification of the cDNA from the core region of the virus. Viral RNA was isolated using a commercial Rnable reagent from Eurobio. cDNA synthesis and PCR was carried out with amplification using primers according to P. Simmons et al (J. Gen. Virol. 74,661-668, 1993) as detailed below:
[0026] RNA was reversely trans-transcribed using a primer sequence 5′-1. CATGTAAGGGTAATCGATGAC, cDNA was amplified using this primer and a primer in the 5′ NCR of the sequence 2. 5′-ACTGCCTGATAGGGTGCTTGCGAG. The second PCR used primers 3. AGGTCTCGTAGACCGTGCATCATG and 4. 5′-TTGCGGGACCTACGCCGGGGGTC.
[0027] Detailed RT-PCT Method (RT-PCR Capsid-HCV)
[0028] This technique is described according to two protocols. The first one is a normal PCR amplification, but the usual dNTP mix is replaced with a dUTP/dATP, dCTP, dGTP mix in order to perform hydrolysis of the DNA with the Uracil-DNA Glycosylase (UDG) in the event of cross contamination of the PCR products. This hydrolysis step prior to PCR amplification is described in the second protocol. The principle of this hydrolysis step relies on the digestion of DNA matrices that contain dUTP instead of dATP, by the UDG. Only DNA which contains dUTP will be digested. However, precaution which must be taken in UDG use is to check the thermosensibility thereof. Indeed, after digestion of DNA matrix, it is necessary to inactivate the enzyme by heating during at least 5 min. at 95° C. to prevent digestion of the PCR products after amplification.
[0029] Antibodies to HCV Core Protein and ELISA Test for Detection of HCV Core Protein
[0030] Monoclonal antibody VT directed to the HCV core protein was obtained from Valbiotech (Pads, France); MAb 39-72 was obtained by immunization of mice with a core peptide corresponding to the aminoacids sequence core numbers 39-72.
[0031] Analysis of the fractions of CsCl gradient with anti-core antibodies revealed the presence of the material reactive with both MAbs VT and 39-72 in fraction, defined as a “heavy fraction”, of a density of 1.32-1.36, much heavier than that of a presumed virion (1.08-1.10 g/ml) defined as the “light fraction”. This observation suggested the presence of non-enveloped nucleocapsids in plasma detectable by ELISA without any treatment. Moreover, the core epitopes detected were apparently exposed and non-covered by human immunoglobulins. Indeed, using inhibition assay no antibodies corresponding to MAb 39-72 could be were detected in a pool of human immunoglobulins prepared from sera with high titer of anti-core antibodies. See FIG. 5.
[0032] Two pools of human globulins containing anti-HCV antibodies IGIV and HG were prepared from sera of HCV carriers highly positive for anti-NS3, NS4 and core antibodies by Abbott HCV EIA were kindly provided by Dr. Ali Fattom, Nabi and A. Nowoslawski, respectively.
[0033] Western Immunoblotting
[0034] Specimens were solubilized in a Tris buffer pH 6.8, containing either 2% SDS or 2% SDS and 5% 2-mercaptoethanol for 2 min at 100° C. Bromheriol blue (0.01%) and 20% sucrose were then added to the samples, the proteins were separated on 12% polyacrylamide gels, and electroblotted to nitrocellulose membranes. The membrane strips were postcoated overnight at 4° C. with 5% skim milk, washed and reacted for 1 h at room temp with monoclonal or polyclonal antibodies diluted in 1% skim milk. HRPO-labeled anti-mouse IgG (heavy+light chains) (Fab)′ fragments, Amersham) of anti-mouse IgM (Sigma) served as a second antibody. After final rinses the blots were visualized with an enhanced chemoluminescence detection system (Amersham).
[0035] Epitope Mapping by ELISA
[0036] The wells of polyvinyl plates Maxisorb (Nunc, Denmark) were coated overnight at room temp, with 1 μg/ml of synthetic peptides corresponding to different aminoacid sequences of HCV core protein. The plates were washed with PBS containing 0.05% Tween 20 and were blocked 2 h at 37° C. with 3% BSA in PBS containing 0.05% Tween 20. Monoclonal antibodies diluted in PBS were incubated on peptide-coated plated 2 h at 37° C. Following washing as above the wells were incubated with HRPO-labeled anti-mouse IgG (heavy+light chains) (Fab)′ fragments, Amersham) of anti- mouse IgM (Sigma) as a second antibody. The reaction was developed using o-phenylenediamine as the enzyme substrate and the absorbance values were read at 492 nm with an ELISA plates reader.
[0037] Competition ELISA With Human and MAbs Anti-HCV Core
[0038] Polyvinyl plates were coated with synthetic peptides or purified recombinant proteins in a concentration of 1 μg/ml, blocked and washed as described above. 100 microliters of human globulins prepared from human sera with a high titers of anti-core antibodies or MAbs, fluids were added to the wells and incubated 24 h at 37° C. After washing, peroxidase labeled MAb 39-72 was added to the wells and incubated as before. The plates were developed and read as described above.
[0039] Preparation of Mabs to HCV Core Protein
[0040] Balb/c mice were immunized intrasplenically with 50 μl of the fraction of CsCl gradient containing HCV core antigen detectable by ELISA. The fraction was dialyzed against PBS and concentrated using Nanosep centrifugal concentrator 300K (Pall Filtron). Three days after immunization mice spleen cells were fused with Sp2/OAg-myeloma cell line. Hybridoma supernatants were screen by ELISA using purified recombinant core protein corresponding to amino acids no. 1 to 120 of the sequence of the nucleocapside. The hybridomas reactive with the recombinant protein were cloned by limiting dilution. The immunoglobulin class of MAbs was determined using anti-mouse IgG (g chain) Amersham and anti-mouse IgM (m chain) (Sigma). The epitope specificity of MAbs was determined using a series of synthetic core peptides.
[0041] Results
[0042] Fractionation of HCV in Density Gradients
[0043] Precipitation of HCV by PEG-6000, previously used for concentration of other viruses allowed the concentration of HCV without lost of viral RNA. Notably, the totality of HCV RNA present originally in the plasma was recovered in the pellet. PEG precipitated preparation was subsequently submitted to ultracentrifugation in sucrose or CsCl gradients. Analysis of distribution of HCV by PCR in sucrose and CsCl gradients after equilibrium centrifugation showed heterogeneity of viral material derived from plasma. The majority of viral RNA was detected in top fractions of a buoyant density of 1.08-1.10 g/ml CsCl and at the density of 1.08 g/ml of sucrose. This RNA could be probably attributed to the b-lipoprotein associated virions since in RNA present in the “light” (top) fractions was stable and could be precipitated 90% with both dextrin sulphate.
[0044] A part of viral RNA was localized in fractions of higher density. See FIG. 1. Interestingly, different profiles of the distribution of viral RNA in the gradient were obtained using routine PCR and a commercial b-DNA assay (Chiron) which apparently does not detect the bulk of viral RNA at the top of the gradient.
[0045] Fractionation of HCV Positive Human Plasma
[0046] Human plasma (100 ml) from a chronic HCV carrier (voluntary blood donor) seropositive for anti-HCV antibodies and containing HCV of 1a genotype (titre 10-5 by PCR) was stored at 80° C. The plasma was thawed and clarified 10 min at 10,000 rpm, PEG 6000 was then added to the clarified plasma to a final concentration of 10% and NaCl to a final concentration of 0.4 M. The mixture was incubated overnight at 4° C. and precipitated virus separated by centrifugation for 1 h at 11,000 rpm in rotor of a Centrikon centrifuge. The pellet, was resuspended in a 13 ml of a 0.01 M Tris-HCl pH 7.2 containing 0.15 M NaCl. The pellet was subjected to centrifugation in a discontinuous CsCl gradient (1.10-1.60; g/ml 1.5 ml of each solution) prepared in PBS and containing protease inhibitors-1 mM PMSF, 2 μg/ml aprotinine and 10 mM EDTA. Centrifugation was carried out in a Beckman SW 41 rotor 48 h at 40,000 rpm. Fractions (1 ml) were collected from the bottom of the tube and assayed for HCV RNA by PCR and for the presence of core antigen by ELISA.
[0047] Detection of HCV Core Antigen in Fractions of CsCl Gradient by ELISA
[0048] Two MAbs, designated as MAb VT (Valbiotech, Paris, France, immunizing antigen non-communicated by the producer) and MAb 39-72, obtained by immunization of mice with a core peptide corresponding to the aminoacids sequence core numbers 39-72 were used for the development of the assay for detection of the HCV core protein. See FIGS. 2A and 2B. The specificity of these monoclonal antibodies was ascertained by Western blot with recombinant HCV core proteins and epitopes recognized by these MAbs were delineated using a series of synthetic peptides encompassing HCV core protein: MAb VT was reactive with the epitope located in the aminoacid sequence 24-37, and MAb 39-72 was reactive with an epitope located in the aa sequence 40-54. See FIGS. 3 A- 3 B. The competitive binding assay confirmed that these two MAbs recognized two different, non-overlapping and non-adjacent epitopes. See FIG. 6.
[0049] To exclude the possibility of the interference of rheumatoid factor (RF) or other non-specific reactivity with the detection of the core antigen, the presence of RF in the gradient was tested. The RF reactivity was detected by latex test in parallel with the non-specific binding to a control (unrelated to HCV) in the fractions of the gradient located at the lower density than that of the core activity.
[0050] To evidence that, in fact, core antigen was present in the gradient, fractions exhibiting the core antigenicity were polled, concentrated by dialysis in the Nanosep centrifugal concentrator 300K (Pall Filtron). 300,000 kda and injected to Balb/c mice to produce MAbs. The hybridomas were selected by ELISA with synthetic 1-130 peptide and subsequently tested with a series of overlapping peptides corresponding to different regions of the core antigen. According to these results, it was deduced that the obtained MAb recognized a linear epitope which is localized in the aminoacid sequence (45-75) of the core region.
[0051] The development of an effective vaccine against HCV is important, but is rendered difficult because of the variability of the virus and unknown antigenic structure of the virion. Identification of the epitopes conserved among different HCV genotypes would be of importance for future development of the immunological assays for detection of the HCV proteins in serum.
[0052] The physical properties of HCV particles have been analyzed by ultracentrifugation in sucrose gradients by several groups. Two main populations of HCV particles according to their floating density were found in sera of patients with chronic HCV infection: low-density virus particles (1.06-1.12 g/ml) and high density virus particles (1.18-1.21 g/ml). Virus particles with high density has been apparently associated with immunoglobulins or was supposed to represent partially or completely naked nucleocapsids Kanto. The virus particles of low density were not associated with immunoglobulins, and accumulated base changes in the hyper variable region of the E2 envelope domain of the genome. Changes in the relative proportions of these viral populations have been observed. Kanto and Hino. The increase of the relative numbers of the high density virions correlated with the disease activity and heterogeneity in HVR1 region, whereas patients with a predominance of the low density fraction showed sustained response to interferon treatment.
[0053] Core antigen has been detected in by use of monoclonal antibodies after treatment of serum concentrates with detergents or denaturing agents. Tak, Tanaka, Kashiwakuma, Orito, and Takahashi. The core antigen was detected in sera of non-responders to IFN-a but not in patients with a sustained response and was correlated to the level of viral RNA. Tanaka. Isolated nucleocapsid-like HCV particles were observed by electron-microscopy (EM) of the detergent-treated, RNA rich fractions. Taka. Few reports suggested the presence of naked, unenveloped HCV nucleocapsids in sera of HCV carriers which could be observed by EM Trest, or detected in serum by Mabs. Kanto and Maslowa. However this population of HCV has not yet been isolated and characterized immunochemically.
[0054] In the following experiment using well-characterized MAbs, the core epitopes exposed on the native nucleocapsid protein were detected in serum. These monoclonal antibodies recognized the non-overlapping epitopes of the HCV core, located close to each other in the aminoacid sequence 24-53. Since reactive with MAbs, these epitopes were not covered by human anti-core antibodies and no corresponding specificity could be detected in a pool of antibodies from chronic HCV carriers. The core antigen was isolated from serum and was shown to be immunogenic in mice. MAbs obtained by immunization with a native serum-derived core protein bound to the linear epitope located in the aa sequence (45-68) as evidenced with synthetic peptides and recognized recombinant cone protein in Western blot. See FIG. 7. This epitope is conserved between different HCV genotypes and is adjacent to the epitopes recognized by the MAb 39-72 used for detection of the core antigen in plasma.
[0055] MAbs raised against the natural core antigen was used to detect HCV core antigen in a liver tissue of chronically infected chimpanzee. This MAb represents a new reagent for the study of HCV biology and for the immunological detection of the viral antigen in sera of patients with HCV infection.
Protocols Used
[0056] I-RNA Extraction From Serum
[0057] In a 1.5 ml Eppendorf tube, extract 100 μl, 10 μl and 1 μl of each serum sample. Add respectively 0 μl, 90 μl or 99 μl of sterile water (qsp 100 μl).
[0058] Add 1 ml of RNable® (Eurobio). Mix 20 sec. and let 5 min. on ice.
[0059] Add 100 μl (1/10 th vol.) CHCl 3 (ReadyRed, Appligene), mix and centrifuge 10 min. at 14000 rpm. Save the colorless supernatant in a new tube.
[0060] Add 500 μl of CHCl 3 , mix and centrifuge 10 min.
[0061] Save the supernatant (#500 μl) and add 50 μl 3M NaOAc pH 5.2, 2 μl of SeeDNA™ (Amersham, RPN 5200) and proceed to an ethanol precipitation with 2 vol. (1 ml) of 100% ethanol. Mix, and centrifuge 10 min. at 1400 rpm at 4° C.
[0062] Wash the RNA pellet with 1 ml of cold 70% ethanol. Centrifuge 10 min.
[0063] Remove all the supernatant, dry the walls of the tube with a Kimwipes® and resuspend the RNA pellet with 20 μl of water containing 2 mM DTT and 2 U/μl Rnasin.
[0064] Store at −80° C.
[0065] I-cDNA Synthesis (Common to Both Protocols)
[0066] In a 500 μl Eppendorf tube, add: (final conc.)
[0067] 5 μl of purified RNA
[0068] 5 μl of water
[0069] and 1 μl reverse-sense primer SIM 2R.
[0070] Recover the mix with one drop of mineral oil, centrifuge briefly and place on the thermocycler for 10 min. at 70° C. and immediately on ice. Centrifuge before the addition of 14 μl of the following mix:
[0071] 5 μl reverse-transcription buffer 5X (1X)
[0072] 1.25 μl dNTP 10 mM (0.5 mM)
[0073] 0.5 μl DTT 100 mM (2 mM)
[0074] 1 μl RNase inhibitor 40 U/μl (1.6 U/μl)
[0075] 1.25 MMLV 200U/μl (250 U)
[0076] 5 μl H 2 O (qsp 25 μl)
[0077] Centrifuge briefly before incubation 1 hour at 37° C. Inactivate the RT during 10 min. at 95° C. and dip the tubes on ice. At this step, the cDNA can be kept at −80° C.
[0078] II-PCR Amplification
A1 - Outer PCR without UDG A2 - Outer PCR with UDG hydrolysis hydrolysis Prepare a mix of these components Prepare a mix of these components in a 1 ml Eppendorf tube on ice in a 1 ml Eppendorf tube on ice (final conc.): (final conc.): 5 μl buffer 10X 5 μl buffer 10X 1.5 μl MgCl 2 50 mM (1.5 mM) 1.5 μl MgCl 2 50 mM (1.5 mM) 2.5 μl dUTP/NTP mix 4 mM 2.5 μl dUTP/NTP mix 4 mM (0.2 (0.2 mM) mM) 1 μl reverse sense primer 1 μl sense primer SIM 1S SIM 2R (50 pmole) (50 pmole) 33.5 μl H 2 O (qsp 50 μl) 1 μl reverse sense primer 0.5 μl Eurobiotaq (2.5 U) SIM 2R (50 pmole) 32.5 μl H 2 O (qsp 50 μl) 0.5 μl UDG (0.5 U) 0.5 μl Eurobiotaq (2.5 U)
[0079] Under the hood: add 5 μl of cDNA, centrifuge the tubes briefly and put them:
Under the hood: add 5 μl of cDNA, centrifuge the tubes briefly and put them: in the thermocycler block once the at 37° C. during 15 min. temperature has reached at and then, denature the UDG least 80° C. (Program No. 6) during 5 min. at 85° C. and 10 min. at 95° C. before starting the amplification (Program No. 5) Amplification cycles (Prog. 6): Amplification cycles (Prog. 5): First Cycle: 94° C.-5 min. First Cycle: 85° C.-5 min. 50° C.-1 min. 95° C.-10 min. 72° C.-1 min. 50° C.-1 min. 72° C.-1 min. 25 cycles: 94° C.-50″ 25 cycles: 94° C.-50″ 55° C.-50″ 55° C.-50″ 72° C.-50″ 72° C.-50″ Elongation: 72° C.-10 min. Elongation: 72° C.-10 min. Stop: 4° C.-5 min. Stop: 4° C.-5 min.
[0080] B—Inner PCR
[0081] This step is common to both protocol because the first amplification product must not be digested by UDG.
[0082] Prepare a mix of these components in a 1 ml Eppendorf tube on ice:
[0083] 5 μl buffer 10X
[0084] 1.5 μl MgCl 2 50 mM (1.25 mM)
[0085] 2.5 μl dUTP/NTP mix 4 mM (0.2 mM)
[0086] 1 μl internal sense primer SIM 3S (50 pmole)
[0087] 1 μl internal reverse sense primer SIM 4R (50 pmole)
[0088] 33.5 μl H 2 O (qsp 50 μl)
[0089] 0.5 μl Eurobiotaq (2.5 U)
[0090] Dispense 45 μl of this mix in each thin-walled 0.5 ml PCR tubes on ice. Add a drop of mineral oil.
[0091] Under the hood: add 5 μl of DNA, centrifuge and put the tubes on the PCR block once the temperature has reached at least 80° C.
Amplification cycles: First cycle: 94° C.-5 min. (Program No. 6) 50° C.-1 min. 72° C.-1 min. 25 Cycles: 94° C.-50″ 55° C.-50″ 72° C.-50″ Elongation: 72° C.-10 min. Stop: 4° C.-5 min.
[0092] Note: At the end of the amplification it is important to centrifuge the tubes before opening to avoid contaminations and to analyze the products immediately or maintain them at −20° C.
[0093] Preparation of dUTP/dNTP-mix
Stock solutions: 250 μl - 20 mM solution dUTP (Epicentre/TEBU) 25 μM - 100 mM dUTP solution (USB/Amersham) dNTP 25 μM - 100 mM solutions kit Pharmacia Preparation: A-TEBU 20 mM dUTP: Dilute 1/25 the 100 mM solutions of the dATP, dCTP and cGTP (4 mM final) Dilute the Epicentre/TEBU dUTP 20 mM solution 1/4 to get a 5 mM solution. Mix 1 vol. of each dNTP diluted solution to get the 4 mM solution of dUTP/dNTP mixture.
[0094] B-USB 100 mM dUTP: In a 1.5 ml tube, add 40 μl of each dATP, dCTP and dGTP 100 mM stock solutions (Pharmacia) and 50 μl of the 100 mM dUTP stock solution (USB). Complete to 1 ml (830 μl) with sterile water to obtain the 4 mM solution of dUTP/dNTP mixture.
[0095] Preparation of the Solution to Resuspend RNA Pellets
[0096] 930 μl pure sterilized water
[0097] 20 μl 0.1 M DTT
[0098] 50 μl Rnasin
[0099] Analysis of the Distribution of HCV RNA by RT-PCR and B-DNA In CsCl Gradient
[0100] The majority of viral RNA was detected by RT-PCR in top fraction (“light fraction”) of the gradient corresponding to buoyant density of 1.06-1.10 g/ml CsCl. According to the literature (and also our observation that the majority HCV RNA detectable by RT-PCR can be precipitated with dextran sulfate) this part of RNA could be attributed to the HCV virions associated to β-lipoproteins.
[0101] Only a minor part of viral RNA was detected by RT-PCR in fractions of higher density; in contrast b-DNA assay which was much more effective at higher density range and two peaks of HCV RNA could be detected by this assay at 132-36 and the second at 1.10-1.15 g/ml. Moreover, the peak of RNA detected by b-DNA at the density of 1.32-1.36 g/ml corresponded to the localization of the core antigen by ELISA.
[0102] The hybridoma described in the present application ws deposited at the C.N. C.M. in France on Apr. 14, 1999, under accession number 1-2183.
[0103] Having described the present invention, it will now be apparent that many changes and modifications may be made to the above-described embodiments without departing from the spirit and the scope of the present invention.
[0104] Finally, attached to and incorporated into this disclosure are copies of the following publications:
[0105] 1) Journal of General Virology, 74, 661-668 (1993), Simmond. et al;
[0106] 2) “Detection et Caracterisation de la Nucleocapside du Virus de L'Hepatite C (VHC) Dans le Serum des Patients Infectes”, Mailard, P. et al;
[0107] 3) “Analyse de la Structure Antigenique de Virus De L'Hepatite C (VHC)”, Budkowska et al;
[0108] 4) Archives of Virology , “Ultrastructural and physicochemical characterization of the hepatitis C virus recovered from the serum of an agammaglobulinemic patient,” 143:2241-2245 (1993), Trestard et al;
[0109] 5) Journal of Medical Virology , “Detection of Hepatitis C Virus Core protein Circulating Within Different Virus particle Populations,” 55:1-6 (1998), Masalova et al.
[0110] Listed below of additional are citations for additional background publications.
REFERENCES
Background
[0111] Hihahata M., Shimizu Y. K., Kato H., et al., “Equilibrium Centrifugation Studies of Hepatitis C Virus: Evidence for circulating Immune Complexes”, J. Virol., 67, 1953-1958, 1993;
[0112] Koshy, R. L., Inchauspe, G., “Evaluation of Hepatitis C Virus protein Epitopes for Vaccine Development, Trends in Biotechnology, 14, 364-369, 1996;
[0113] Thomssen, R., Bonk, S., Propfe C., Heerman, K. H., Kochel H. G., Uy, A., “Association of Hepatitis C Virus in Human Sera with β-lipoprotein”, Med. Microbiol. Immunol, 181, 293-300, 1992;
[0114] Takahashi K., Okamoto H., Kishimoto S., Munekata E., Tachibana K., Akahane Y., Yoshizawa H., and Mishiro S., “Demonstration of a Hepatitis C Virus Specific Antigen Predicted from the Putative Core Gene in the Circulation of Infected Host,” J. Gen. Virol., 73 667-672, 1992;
[0115] Takahaski, K., Kishimoto, S., Yoshizawa, H., Okamoto, H., Yoshikawa, A., and Mishiro, S., “p26 protein and 33 nm Particle associated with nucleocapsid of hepatitis C Virus Recovered from the Circulation of Infected Host,” Virology, 191, 431-434, 1992. | A method of directly detecting Hepatitis C virus in a fractionated or non-fractionated serum of a patient, by detecting the virus with primers corresponding to viral RNA encoding core protein which said RNA is a light fraction of the total viral RNA, the said light fraction being isolated after ultracentrifugation in a CsCl gradient of human serum containing HCV virus, said light fraction containing most of the circulating infectious HCV virus particles, the method entailing precipitating RNA, then effecting reverse transcription, and then effecting amplification with the primers described herein. | 2 |
BACKGROUND OF THE INVENTION
[0001] Cervinomycins (EP00246091; EP0054801; J.Antibiot. 1982, 35, 645-652; J.Am.Chem.Soc. 1986, 108, 6088-6089, J.Antibiot. 1987, 40, 301-308; J.Antibiot. 1994, 47, 342-348; synthetic derivatives J.Antibiot. 1986, 39, 1636-1639 and EP0259496) and citreamicins (J.Antibiot. 1989, 42, 846-851; J.Antibiot. 1990, 43, 504-512; EP0405151) are members of a family of naturally occurring antibiotics, all of which posses a xanthone based unit embedded within a larger polycyclic framework.
[0002] These compounds have demonstrated potent activity against aerobic and anaerobic bacteria and mycoplasma, but only cervinomycins have been described to display antitumour activity (EP0246091).
[0003] We have recently described also the antitumour activity of citreamicins in PCT/GB01/02148.
[0004] New anticancer drugs are still needed for treatment against many human tumours. Accordingly, a goal of the present invention is to provide new antitumour agents with a polycyclic xanthone structure.
[0005] Another objective of this invention is to provide pharmaceutical compositions for administering to a patient in need of treatment an active compound.
[0006] Yet another object is directed to the production of the polycyclic xanthone by controlled aerobic fermentation using a biologically pure culture of an organism in appropriate nutrient media, also to provide with methods for its recovery and concentration from the fermentation broth, and to the final purification of the active compound.
SUMMARY OF THE INVENTION
[0007] This invention provides a new class of active xanthone compounds founded on the discovery of a new compound IB-00208 isolated from a bacteria, useful as antitumour medicaments with the formula:
[0008] Thus, the present invention provides compounds with the general formula:
[0009] where each R 1 is the same or different and can be hydrogen, acyl, alkyl, alkenyl, aryl, benzyl, alkali metal, and/or sugar, and R 2 and R 3 can be hydrogen, alky, or together form an unsaturated bond.
[0010] This invention also provides processes for preparing such compounds including a process of obtaining IB-00208.
DETAILED DESCRIPTION OF THE INVENTION
[0011] IB-00208 and related compounds exhibits antitumour activity against mammalian tumours, such as human lung carcinoma, human colon carcinoma, human melanoma, etc. Thus, the invention includes a method of treating any mammal affected by a malignant tumour sensitive to them, which comprises administering to the affected individual a therapeutically effective amount of the compound or a pharmaceutical composition thereof
[0012] The present invention also relates to pharmaceutical preparations which contain as active ingredient compound IB-00208 or any of its derivatives, or a pharmaceutical acceptable salt thereof, as well as the processes for its preparation. A pharmaceutically acceptable carrier is employed.
[0013] Pharmaceutical compositions are typically formulated from the active compound and include any solid (tablets, pills, capsules, granules, etc.) or liquid (solutions, suspensions or emulsions) in combination with any carrier or other pharmacologically active compounds.
[0014] The correct dosage of a pharmaceutical composition of IB-00208 or its derivatives will vary according to the particular compound, formulation, mode of application, and sites of host and tumour being treated.
[0015] Others factors like age, body weight, sex, diet, time of administration, rate of excretion, condition of the host, drug combinations, reaction sensitivities and severity of the disease shall be taken into account. Administration can be carried out continuously or periodically within the maximum tolerated dose.
[0016] The acyl groups can be aliphatic acyl, aromatic acyl, or mixed aliphatic/aromatic acyl. Thus, for example, they can be of the formula RCO-, where R is an alkyl group, an alkenyl group, an aryl group, an arylalkyl group, or an alkylaryl group. Examples include benzoyl.
[0017] The alkyl groups typically have from 1 to 18 carbon atoms. Alkyl groups preferably have from 1 to about 12 carbon atoms, more preferably 1 to about 8 carbon atoms, still more preferably 1 to about 6 carbon atoms, and most preferably 1, 2, 3 or 4 carbon atoms. Methyl, ethyl and propyl including isopropyl are particularly preferred alkyl groups in the compounds of the present invention. As used herein, the term alkyl, unless otherwise modified, refers to both cyclic and noncyclic groups, although cyclic groups will comprise at least three carbon ring members. The alkyl groups may be straight chain or branched chain.
[0018] The alkenyl groups typically have from 1 to 18 carbon atoms. Preferred alkenyl groups in the compounds of the present invention have one or more unsaturated linkages and from 2 to about 12 carbon atoms, more preferably 2 to about 8 carbon atoms, still more preferably 2 to about 6 carbon atoms, even more preferably 2, 3 or 4 carbon atoms. The term alkenyl as used herein refer to both cyclic and noncyclic groups, although straight or branched noncyclic groups are generally more preferred.
[0019] The aryl groups can be carbocyclic or heterocyclic, and may have one or more fused rings. The carbocyclic aryl groups typically have 6 or 10 carbon atoms, as in phenyl or naphthyl. Heterocyclic aryl groups typically have 5 to 12 atoms, more usually 4, 5, 6, 10, 11 or 12 atoms, of which there is 1, 2, 3 or more heteroatoms usually chosen from oxygen, sulphur or nitrogen. Suitable heterocyclic aryl groups in the compounds of the present invention include coumarinyl including 8-coumarinyl, quinolinyl including 8-quinolinyl, pyridyl, pyrazinyl, pyrimidyl, furyl, pyrrolyl, thienyl, thiazolyl, oxazolyl, imidazolyl, indolyl, benzofuranyl and benzothiazol.
[0020] Notable alkali metals include sodium or potassium.
[0021] Sugars employed as substituents are typically mono-, di- or tri-saccharides or saccharide derivatives, prepferably mono- or di-saccharides. Pentose or hexose compounds are preferred. Derivatives include sugar glycosides, N-glycosylamines, O-acyl derivatives, O-methyl derivatives, sugar alcohols, sugar acids, deoxy sugars, and related compounds. Examples include the trimethyldeoxypyranose hexose of IB-00208.
[0022] This invention describes a new polycyclic xanthone IB-00208, isolated from the fermentation broth of a microorganism, preferably Actinomadura sp. PO13-046, a culture of which has been deposited in the Colección Española de Cultivos Tipo at the University of Valencia, Spain under the accession number CECT 5318. This deposit has been made under the provisions of the Budapest Treaty and all restrictions on the availability thereof to the public will be made upon the granting of a patent on this application.
[0023] The microbial strain was isolated from an unidentified marine polychaete collected at the Bay of Biscay.
[0024] While the deposited organism is clearly preferred, the present invention is not restricted or limited to any particular strain or organisms. It is the intention of the present invention to include other IB-00208 producing organisms, strains or mutants within the scope of this invention.
[0025] Actinomadura sp. PO13-046 cultured under controlled conditions in a suitable medium produces the antibiotic IB-00208. This strain is preferably grown in an aqueous nutrient medium, under aerobic and mesophilic conditions.
[0026] The antibiotic IB-00208 can be isolated from the mycelial cake by extraction with a suitable mixture of solvent such as CHCl 3 :CH 3 OH:H 2 O. The activity is concentrated in the lower layer. The extracts from two repeated extractions can be combined and evaporated to dryness in vacuo.
[0027] Separation and purification of IB-00208 from the crude active extract can be performed by the use of the proper combination of conventional chromatographic techniques.
BRIEF DESCRIPTION OF THE DRAWINGS
[0028] [0028]FIG. 1 is the proton NMR ( 1 H) spectrum of purified IB-00208;
[0029] [0029]FIG. 2 is the carbon-13 NMR ( 13 C) spectrum of purified IB-00208;
[0030] [0030]FIG. 3 is the DEPT experiment of purified IB-00208;
[0031] [0031]FIGS. 4, 5, and 6 are COSY 45, HMQC and HMBC spectra of purified IB-00208 respectively;
[0032] [0032]FIG. 7 is the IR spectrum of purified IB-00208;
[0033] [0033]FIG. 8 is the HPLC/MS chromatogram and ESI-MS spectrum of IB-00208; and
[0034] [0034]FIG. 9 is the HPLC/UV chromatogram and the UV spectrum of purified IB-00208
[0035] Fractionation can be guided by the antitumour activity of fractions, or by TLC visualised with vanillin in conc. H 2 SO 4 , or analytical HPLC with photodiode-array and MS detector. HPLC analysis is performed at room temperature using an analytical column Symmetry C18 (5 μm using as mobile phase methanol:H 2 O:Acetic acid 99:1:1 and a flow rate of 0.3 ml/min. and plotted at 325 nm, in this conditions IB-00208 retention time is 4.5 min as is shown in FIG. 9.
[0036] On the basis of detailed analysis of their various spectral characteristics, the pure compound can be identified as IB-00208 (see data reproduced in FIGS. 1 to 9 ). Therefore the deduced structure is as it appears above.
[0037] IB-00208 data are summarised in Table 1.
TABLE 1 UV spectrum absorption maxima: 225, 255 nm and 325 nm as reported in FIG. 9. 1 H, 13 C and DEPT NMR. spectra are reported in FIG. 1, FIG. 2 and FIG. 3 respectively. 2D NMR experiments COSY, HMQC and HMBC are reported in FIG. 4, FIG. 5 and FIG. 6 respectively. Infrared absorption spectrum is shown in FIG. 7. The ES-MS spectrum displayed a (M + H) − peak at 691 and (M + Na) peak at 713, as reported in FIG. 8.
[0038] Various derivatives of IB-00208 can be prepared using techniques already known in the art. As an example, these modifications can be made using chemical or biological methods. These changes can include:
[0039] preparation of the aglycone moiety;
[0040] addition to the aglycone of different sugars known and new;
[0041] modification of the aglycone.
[0042] Compounds with a hydroquinone ring may be prepared from compounds with quinone ring by reduction of the quinone with a reducing agent [for example: NaBH4 (T.Ross Kelly et al. J.Am.Chem.Soc. 1989, 111, 4522-4524), Na2S2O4 (A. V. Rama Rao et al. Tetrahedron Lett. 1991,32, 5199-5202)] in an appropriate solvent, followed (when R1≠H) by reacting the hydroquinone with an acylating or alkylating or appropriated agent in an appropriate solvent.
[0043] The present invention in reference to preferred embodiments will be further illustrated with the following examples, which will aid in the understanding of the present invention and are aimed only to illustrate it, but which are not to be construed as limitations thereof.
EXAMPLES OF THE INVENTION
[0044] All percentages reported herein, unless specified, are presented by weight. All temperatures are expressed in degrees Celsius. All incubations are carried out at 28° otherwise stated and flasks are shaken in an orbital shaker at 250 rpm. All media and recipients are sterile and all culture processes aseptic.
[0045] Examples 1 to 3 deal with the preparation of compound IB-00208 with formula shown above, and Example 4 with its biological activity.
Example 1
[0046] The Producing Organism:
[0047] The taxonomic methods utilised herein are those usually employed in classic Actinomycete taxonomy and are reported in the literature.
[0048] All cultures after incubation were studied and records of results were made weekly up to 21 days. NaCl was added when needed.
[0049] A description of the organism is as follows:
[0050] After 21 days good growth was observed in ISP 2, ISP 6, Bennet and 172 ATCC with ASW. Colonies had light brown colour. In ISP 3, ISP 5, Czapek and ISP 7 with ASW less growth was obtained and no soluble pigment was observed. No aerial mycelium was formed. Substrate mycelium was branched. Isolated spores-over the substrate mycelium may occur. Spores are elongated and scarce. No other formations were observed.
[0051] In ISP-1 brown diffusible pigments were formed, as well as in other solid media. Resistance to NaCl was over 5%. The optimum growth temperature range is between 25° and 35° C. The organism can grow on glucose, galactose, rhamnose, and xylose as the sole carbon source, however, growth on fructose, raffinose, m-inositol, sucrose, and α-melibiose is negative, and in mannitol and melezitose is doubtful.
[0052] Chemical composition studies of the organism show that meso-2,6-diaminopimelic acid is present in the whole cell hydrolysate of strain PO13-046.
[0053] Fatty acids methyl esters comparison of PO13-046 with other similar strains is described in TABLE 2.
TABLE 2 i-14:0 14:0 15:0 PO13-046 1.75 2.43 4.9 Actinomadura livida ATCC 33578 1.41 1.21 7.4 Actinomadura madurae NRRL-B 5390 1.0 2.5 6.1 Actinomadura malachitica ATCC 27888 1.4 3.4 0.7 Actinomadura vinacea ATCC 33581 1.4 1.4 6.1 Actinomadura formosensis 1 ATCC 49059 1.3 1.2 2.8 Streptomyces griseus * DSM 40236 15.1 0.8 0.9 i-16:0 16:1 16:0 PO13-046 20.2 5.16 22.6 Actinomadura livida ATCC 33578 21.8 5.5 13.7 Actinomadura madurae NRRL-B 5390 11.5 5.56 21.2 Actinomadura malachitica ATCC 27888 18.5 7.9 26.2 Actinomadura vinacea ATCC 33581 22.7 6.8 15.2 Actinomadura formosensis 1 ATCC 49059 22.5 3.4 17.8 Streptomyces griseus * DSM 40236 21.2 5.1 6.4 17:1 17:0 PO13-046 6.5 5.4 Actinomadura livida ATCC 33578 14.9 7.0 Actinomadura madurae NRRL-B 5390 10.9 7.9 Act. malachitica ATCC 27888 1.1 0.9 Actinomadura vinacea ATCC 33581 12.8 5.6 Actinomadura formosensis 1 ATCC 49059 6.9 4.6 Streptomyces griseus * DSM 40236 <1 <1 i- Cis- i-18:1 18:0 18:1 18:0 18.38 PO13-046 5.2 1.8 13.0 1.22 5.75 Actinomadura livida ATCC 33578 7.5 1.2 7.8 1.0 5.7 Actinomadura madurae NRRL- 3.0 1.6 16.5 1.1 5.3 B 5390 Act. malachitica ATCC 27888 3.7 2.7 15.8 4.5 8.7 Actinomadura vinacea ATCC 33581 6.1 1.6 10.3 0.7 5.1 Actinomadura formosensis 1 6.8 1.8 10.8 2.4 5.5 ATCC 49059 Streptomyces griseus * DSM 40236 1.1 <1 <1 <1 <1
[0054] Based on the preceding characteristics the culture is determined as a species of the genus Actinomadura, with 94% similarity to A. vinacea type strain.
Example 2
[0055] Fermentation of IB-00208:
[0056] The required steps needed for the production of IB-00208 by the preferred organism are:
[0057] Stock Culture: Whole broth of a pure culture of Actinomadura sp. strain PO13-046 is preserved frozen in 20% glycerol.
[0058] Inoculum: A frozen culture or a well grown slant culture is used to seed 100 ml of seed medium described previously in a 250 cc shake flask. The flask is incubated during 48 hrs, and used as a first stage inoculum. 500 ml of the same medium in 2 L Erlenmeyer flask are seeded with 10% of this first stage inoculum. The flask is incubated during 48 h.
[0059] Fermentation: With 2.5L of second stage inoculum seed 50 L of production medium already described in a 75 L fermentation tank. The fermentation is carried out during 96 hours with 400 rpm agitation and air flow of 0.5 V/V.M.
TABLE 3 Inoculum medium: Glucose 5 g Starch 20 g Beef extract 3 g Yeast extract 5 g Tryptone 5 g CaCO3 4 g NaCl 5 g KCl 0.5 g MgCl2 2 g Tap water to 1,000 ml Production medium: Glucose 5 g Starch 20 g Soybean meal 15 g Yeast extract 5 g Tryptone 2 g CaCO3 4 g NaCl 5 g KCl 0.5 g MgCl 2 2 g Tap water to 1,000 ml
[0060] Yield of IB-00208 can be monitored by whole broth assay against murine leukaemia P-388 or by HPLC.
Example 3
[0061] Isolation of IB-00208:
[0062] 4.5 litres of whole harvested broth were filtrated to separate the biomass and other solids. The mycelia cake was extracted twice with a mixture solvent (1.5 l) of CHCl 3 :CH 3 OH:H 2 O (2:1:1), the activity was concentrated in the lower layer. The organic solvent was concentrated and evaporated to dryness in vacuo to yield 1.2 g of crude extract.
[0063] The extract was chromatographed on silica gel using a mixture of n-hexane/ethyl acetate and ethyl acetate/methanol as eluting solvents. 110 mg of a fraction containing IB-00208 with antitumour activity were eluted with ethyl acetate/methanol 1:1.
[0064] Further purification of the fraction containing IB-00208 was achieved by column chromatography on silica gel and 18 mg of pure compound IB-00208 were eluted with chloroform/methanol 95:5.
Example 4
[0065] Biological activity:
[0066] The antitumour activities of IB-00208 have been determined in vitro in cell cultures of mouse leukaemia P-388, human lung carcinoma A-549, human colon carcinoma HT-29 and human melanoma MEL-28. The procedure was carried out using the methodology described by Bergeron et al. The IC50 found was of 0.001, 0.001, 0.001, and 0.001 μg/ml for all 4 cell lines.
REFERENCES
[0067] The following references have been cited herein:
[0068] ATCC Catalog 1996.
[0069] Bergeron et al. Biochem.Biophys. Res.Comm. 121:848, 1984
[0070] Guerrant and Moss, Anal.Chem. 56:633, 1984.
[0071] Hasegawa et al., J. Gen. Appl. Microbiol. 29:319, 1983.
[0072] Shirling and Gotlieb. Int.J.Syst.Bacteriol. 16:313, 1966.
[0073] Van der Auwera et al., J. Microbiol. Methods, 4:265, 1986.
[0074] Waksman, The Actinomycetes vol.II:331, 1961.
[0075] The present invention has been described in detail, including the preferred embodiments thereof. However, it will be appreciated that those skilled in the art, upon consideration of the present disclosure, may make modifications and/or improvements within this invention. | A novel class of antitumour compounds has been recognised based on the isolation from a new marine microbe, strain PO13-046, belonging to the genus Actinomadura sp.), of a compound designated IB-00208. The class of the formulae (I) or (II) where R 1 can be hydrogen, acyl, alkyl, alkenyl, aryl, benzyl, alkali metal, and/or sugar, and R 2 and R 3 can be hydrogen, alkyl, or together R 2 and R 3 form an unsaturated bond. Such compounds demonstrate an interesting activity several cancel cell lines and against Gram-positive bacteria. | 2 |
TECHNICAL FIELD
This invention relates to fluid guns, and specifically to fluid toy guns which utilize compressed air to launch a projectile or to propel a stream of water.
BACKGROUND OF THE INVENTION
Toy guns which shoot or launch projectiles have been very popular for many years. These guns have been designed to launch projectiles in a number of ways. A common method of launching has been by the compression of a spring which propels the projectile upon its decompression or release, as, for example, with BB guns and dart guns. These guns however usually do not generate enough force to launch projectiles with great velocity.
Toy guns have also been designed which use compressed air to launch projectiles such as foam darts. These types of guns use a reciprocating air pump to pressurize air within a pressure tank. In use, a single dart is loaded and the pump is typically reciprocated several times with each firing of the gun. Therefore, the gun must be loaded and pumped with each firing as it is not capable of firing several darts in rapid sequence. The rapid firing of a gun may be desired for those playing a mock war or other type of competition. Small children however quickly become tired due to having to actuate the pumping mechanism of these guns in a continuous manner. A child may also forget to repressurize the gun following its actuation, thereby rendering the gun inoperable at a later time when the child desires to fire a projectile. As such, the child must quickly actuate the pumping mechanism in order to fire the projectile.
Toy guns have also been designed which produce a stream of water and hence are commonly referred to as water guns. The most simple method of ejecting water has been with the actuation of a manual pump coupled to the trigger of the gun. The pump is actuated by the mere pressure exerted by one finger of an operator upon the trigger, thus the pump typically cannot generate enough pressure to eject the water a lengthy distance. Additionally, these types of pumps work on the actuation of a compression piston which create single, short bursts of water. However, many children desire the production of an extended stream of water.
Water guns have also been designed with small electric pumps which expel a stream of water from a tube coupled to the pump, as shown in U.S. Pat. Nos. 4,706,848 and 4,743,030. However, these small electric pumps typically do not generate enough force to eject the stream of water a lengthy distance.
Water guns have also been designed with a pressure tank adapted to hold water therein and a manual air pump for supplying a volume of pressurized air into the pressure tank. Again, with extended use of these guns a small child may become quite tired having to continuously actuate the pumping mechanism continuously with each firing of the gun. Furthermore, here again, a child may forget to pressurize the pressure tank and thus be unable to fire the gun at a desired time.
Accordingly, it is seen that a need remains for a toy fluid gun which may be pressurized in a quick and efficient manner. It is to the provision of such therefore that the present invention is primarily directed.
SUMMARY OF THE INVENTION
In a preferred form of the invention a compressed air gun for firing projectiles comprises an electric power source, an electrically motorized air pump coupled to the electric power source, a pressure chamber in fluid communication with the air pump, a launch tube in fluid communication with the pressure chamber, a release valve in fluid communication with the launch tube which controls the release of pressurized air from the pressure chamber to the launch tube, and trigger means for actuating the release valve. The gun also has pressure sensitive actuation means in fluid communication with the pressure chamber for sensing the air pressure associated with the pressure chamber and energizing the motorized air pump when the sensed air pressure is within a select pressure range.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a rapid fire compressed air gun embodying principles of the present invention in a preferred form.
FIG. 2 is a side view, shown in partial cross-section, of the air gun of FIG. 1 .
FIGS. 3-5 are a sequence of views showing a portion of the air gun of FIG. 1, which show in sequence, the actuation of an actuator which indexes a magazine and controls a release valve.
FIG. 6 is a perspective view of a rapid fire compressed air gun embodying principles of the present invention in another preferred form.
FIG. 7 is a rear view of portions of the air gun of FIG. 6 with the pump shown in side view for clarity of explanation.
FIG. 8 is a rear view of portions of the air gun of FIG. 6 with the pump shown in side view for clarity of explanation.
FIG. 9 is a side view, shown in partial cross-section, of interior components of the air gun of FIG. 6 and a projectile positioned within the barrel of the gun.
FIG. 10 is a side view, shown in partial cross-section, of an alternative design for the interior components of the air gun of FIG. 1, shown in a pressurizing configuration.
FIG. 11 is a side view, shown in partial cross-section, of the interior components shown in FIG. 10, shown in a firing configuration.
FIG. 12 is a schematic view of portions of an air compressed gun in another preferred form.
FIGS. 13-16 are a sequence of side views, shown in partial cross-section, of a portion of the interior components of the air gun of FIG. 12, which show in sequence, the actuation of the interior components controlling the release of pressurized air.
FIGS. 17-20 are a sequence of side views, shown in partial cross-section, of a portion of the interior components in another preferred embodiment, which show in sequence, the actuation of the interior components controlling the release of pressurized air.
FIGS. 21 and 22 are a sequence of top views of the magazine of the air gun of FIG. 12, which show in sequence, the rotation of the magazine in conjunction with the actuation of the control valve.
FIGS. 23-26 are a sequence of side views, shown in partial cross-section, of a portion of the interior components in another preferred embodiment, which show in sequence, the actuation of the fluid pulsator controlling the release of pressurized fluids.
FIGS. 27-28 are a sequence of side views, shown in partial cross-section, of a portion of the interior components in another preferred embodiment, which show in sequence, the actuation of the fluid pulsator controlling the release of pressurized fluids.
FIG. 29 is a schematic view of a toy gun shown firing a sequence of water bursts.
FIG. 30 is a cross-sectional view of a variable flow fluid valve in an alternative embodiment.
FIGS. 31-33 are a sequence of side views, shown in partial cross-section, of a portion of the interior components in another preferred embodiment, which show in sequence, the actuation of the fluid pulsator controlling the release of pressurized fluids.
FIG. 34 is a schematic diagram of a toy gun in another preferred embodiment.
FIG. 35 is a schematic diagram of a toy gun in another preferred embodiment.
FIG. 36 is a schematic diagram of a toy gun in another preferred embodiment.
FIG. 37 is a detailed view of the actuation switch of the toy gun shown in FIG. 35 .
DETAILED DESCRIPTION
With reference next to the drawings, there is shown a compressed air gun 10 having a stock or handle 11 , a barrel 12 mounted to the stock 11 , a spring biased trigger 13 , and a manual air pump 14 . The gun 10 has a pressure chamber or tank 15 in fluid communication with the air pump 14 through a pressure tube 16 and a multi-projectile magazine 18 rotationally mounted to stock 11 . The pump 14 includes a conventional cylinder 20 , a cylinder rod 21 and a handle 22 mounted to an end of the cylinder rod 21 .
The magazine 18 has a central pivot rod 24 mounted to a disk-shaped mounting plate 25 and an annular array of projectile barrels 26 extending from the mounting plate 25 in generally two concentric circles about pivot rod 24 . Each barrel 26 has a launch tube 27 therein aligned with an opening 28 extending through the mounting plate 25 . Likewise, the openings 28 are oriented in two concentric circles or annular arrays with each opening of the inner circle being positioned generally between two adjacent opening of the outer circle, so as to appear in staggered fashion, as best shown in FIGS. 3-5. Thus, each opening 28 ′ of the outer annular array of openings 28 ′ is aligned along a radius and spaced a selected distance d1 from the center of the mounting plate, and each opening 28 ″ of the inner annular array of openings 28 ″ is aligned along a radius and spaced a selected distance d2 from the center. The gun magazine is shown in FIG. 2 as having only one barrel for clarity of explanation. Mounting plate 25 has series of peripheral, outwardly extending, serrated teeth 31 each of which is aligned with a barrel 26 . The serrated teeth 31 are configured to cooperate with a pawl 32 extending from the stock 11 . The mounting plate 25 also has an annular array of L-shaped grooves 33 equal in number to the number of magazine barrels 26 .
The gun 10 has a pressure chamber 35 adapted to receive and store a supply of air at elevated pressure levels and a pressure sensitive release valve 36 mounted within the pressure chamber 35 . The pressure chamber 35 has an exit opening 37 therein. A spring biased sealing plate 38 is mounted within opening 37 . The sealing plate 38 has a central bore 39 extending into an elongated bore 40 configured to overlay the mounting plate openings 28 . It should be noted that the mounting plate openings 28 are positioned so that the sealing plate elongated bore 40 overlaps only one opening 28 at a time. A gasket 42 is mounted to the sealing plate 38 to ensure sealing engagement of the sealing plate with the mounting plate 25 . The release valve 36 has a cylindrical manifold 45 and a cylindrical plunger 46 slidably mounted within manifold 45 . Plunger 46 has a gasket 47 to ensure sealing engagement of the plunger about opening 37 .
The release valve manifold 45 is pneumatically coupled to an actuator 50 , by a pressure tube 51 extending therebetween the actuator 50 automatically and sequentially causes the actuation of the release valve 36 . Actuator 50 includes an elongated manifold 52 having an upper opening 53 in fluid communication with pressure tube 51 and a lower opening 55 in fluid communication with another pressure tube 56 extending from the pressure tank 15 and positioned so as to be pinchably closed by spring biased trigger 13 . A piston 58 is movably mounted within actuator manifold 52 . Piston 58 has a top seal 59 and a bottom seal 60 . The actuator 50 also has a pressure cylinder 62 having a vent 61 adjacent its top end. Pressure cylinder 62 is coupled in fluid communication with pressure chamber 35 by a pressure tube 63 . A piston 64 , having an elongated piston rod 65 , is mounted within the actuator pressure cylinder 62 for reciprocal movement therein between a low pressure position shown in FIGS. 2 and 3 and a high pressure position shown in FIG. 4. A coil spring 67 mounted about piston rod 65 biases the piston 64 towards its low pressure position. Piston rod 65 is coupled to piston 58 by an over center torsion spring 68 , such as that made by Barnes Group Incorporated of Corry, Pa. under model number T038180218-R. An indexing finger 69 , mounted to an end of the piston rod 65 , is configured to sequentially engage and ride within each magazine L-shaped groove 33 .
In use, an operator actuates the pump to pressurize a supply of air by grasping the handle 22 and reciprocating the cylinder rod 21 back and forth within the cylinder 20 . Pressurized air is passed through pressure tube 16 into the pressure tank 15 . Manual actuation of the trigger 13 moves the trigger to a position wherein it unpinches pressure tube 56 so as to allow pressurized air within the pressure tank 15 to pass through pressure tube 56 into actuator manifold 52 between the top and bottom seals 59 and 60 . The pressurized air then passes out of lower opening 55 and through pressure tube 51 into release valve manifold 45 .
The pressurized air within the release valve manifold 45 causes the plunger 46 to move to a forward position sealing the opening 37 . Pressurized air then flows between the plunger 46 and the release valve manifold 45 so as to pressurize the pressure chamber 35 . A portion of the pressurized air within pressure chamber 35 passes through pressure tube 63 into the actuator pressure cylinder 62 . With increased pressure within pressure cylinder 62 the piston 64 is forced upwards against the biasing force of coil spring 67 , i.e. the piston 64 is moved from its low pressure position shown in FIG. 3 to its high pressure position shown in FIG. 4 . As shown in FIG. 4, upward movement of the piston rod 65 causes compression of torsion spring 68 and the finger 69 to ride up within a mounting plate groove 33 thereby causing clockwise rotation of the magazine 18 which brings opening 28 ″ into fluid communication with seal plate 38 . All references herein to downward and upward directions is for purposes of clarity in reference to the drawings and is not meant to indicate gravity sensitivity. Upon reaching the apex of the movement of piston rod 65 the torsion spring 68 decompresses thereby forcing piston 58 downward, as shown in FIG. 5 . Downward movement of piston 58 causes the top seal 59 to be positioned between upper opening 53 and lower opening 55 . This positioning of the piston 58 isolates manifold lower opening 55 to prevent escape of pressurized air from pressure tank 15 . This positioning of the top seal 59 also allows pressurized air within pressure tube 51 to escape to ambience through the top of actuator manifold 52 . The release of air pressure causes the plunger 46 to move to a rearward position unsealing opening 37 . With the unsealing of opening 37 pressurized air within pressure chamber 35 flows through opening 37 , into the central and elongated bores 39 and 40 of sealing plate 38 , and into the launch tube 27 through mounting plate opening 28 . Pressurized air within launch tube 27 propels the projectile out of the magazine barrel 26 and through gun barrel 12 . The actuation of this type of release valve is described in more detail in U.S. Pat. No. 4,159,705.
Upon the release of pressurized air from pressure chamber 35 the pressurized air within pressure cylinder 62 is released through pressure tube 63 back into pressure chamber 35 . The release of air from pressure cylinder 62 causes the piston 64 be spring biased by coil spring 67 back downward to its low pressure position. The downward movement of piston 64 retracts the indexing finger 69 from within a mounting plate groove 33 and positions the finger in register with the following mounting plate groove 33 . The low pressure positioning of piston 64 causes the torsion spring 68 to bias piston 58 upwards to its initial position with the top and bottom seals 59 and 60 straddling upper and lower openings 53 and 55 , as shown in FIG. 3 . This repositioning of piston 58 once again causes pressurized air within pressure tank 15 to flow through pressure tube 56 into actuator manifold 52 , thereby completing a firing cycle. The firing and indexing cycle just describe may continue in rapid sequence so long as the trigger is maintained in a position allowing the flow of pressurized air through pressure tube 56 and the pressure tank continues to contains a minimal level of pressurized air sufficient to overcome the biasing force of springs 67 and 68 , i.e. the release valve is automatically actuated by actuator 50 and the indexing of magazine 18 continues so long as the trigger is pulled open and the pressure tank contains pressurized air above a level to overcome springs 67 and 68 . Should the pressure level within pressure tank 15 reach the minimal level the operator simply actuates the manual air pump 14 so as to once again elevate the pressure within the pressure tank.
As described, the gun may be used in a fully automatic manner such that with the trigger maintained in a pulled back, actuated position the gun fires a series of projectiles without stopping between each successive shot, similar to the action of a machine gun. However, should an operator wish to fire a single projectile, one need only to pull the trigger and quickly release it so that pressurized air does not continue to flow into the actuator 50 . Operated in such a manner the gun will index the magazine and fire a projectile with each actuation of the trigger, again, so long as the pressure tank contains air pressurized above the minimal level and the trigger is quickly released.
It should be noted that pawl 32 engages teeth 31 to prevent rotation of the magazine in a direction opposite to its indexing direction, i.e. to prevent counterclockwise rotation in FIG. 3 . This prevents the firing of pressurized air into a just emptied barrel and damage to the indexing finger. It should also be noted that since the pneumatic system is closed, once the gun is initially pressurized it is maintained under at least the minimal pressure level. Thus, the gun has the capability of firing projectiles in a rapid sequence of shots one after another. Yet, the gun may also fire a sequence of single shots without having to be pumped between each successive shot.
Referring next to FIGS. 6-9, a compressed air gun 70 in another preferred form is shown. Here, the air gun 70 has a housing 71 having a support plate 72 and an L-shaped support arm 73 , a magazine 75 rotationally mounted to the housing 71 , a remote manual hand air pump 76 , and a harness 77 secured to housing 71 and configured to be supported upon the head of a person. The gun 70 has a pressure chamber 79 adapted to receive and store a supply of air at elevated pressure levels and a pressure actuatable release valve 80 mounted within the pressure chamber 79 . A control valve 81 is mounted in fluid communication with release valve 80 and is coupled in fluid communication with pump 76 by a pressure tube 78 extending therebetween. Pressure chamber 79 is pneumatically coupled to a pneumatic indexer 82 which in turn is coupled to magazine 75 for rotational movement thereof.
The head harness 77 has a generally circular base strap 83 and a inverted U-shaped, adjustable top strap 84 secured to the base strap 83 by a buckle 85 . The head harness 77 also has a clear eye sight 86 configured to be positioned over the eye of a person. The top strap 84 and base strap 83 may be made of a soft, flexible plastic which can conform to the person's head.
The magazine 75 has a central pivot rod 87 fixedly mounted to a disk-shaped mounting plate 88 and an annular array of projectile barrels or launch tubes 89 extending from the mounting plate 88 in a generally concentric circle about pivot rod 87 . Pivot rod 87 is rotationally mounted at one end to support arm 73 and rotationally mounted at its opposite end to support plate 72 . Each barrel 89 has a launch tube 90 therein aligned with an opening 91 which extends through the mounting plate 88 . The interior diameter of barrel 89 is configured to releasably hold a projectile P with the launch tube 90 configured to be received within a recess R in the rear of the projectile. The magazine is shown in FIG. 9 as having only one barrel 89 for clarity of explanation. Mounting plate 88 has series of peripheral notches 93 each of which is aligned with a barrel 89 . The notches 93 are configured to cooperate with a pawl extending from the housing 71 . Mounting plate 88 also has an annular array of L-shaped grooves 95 oriented about pivot rod 87 which are equal in number to the number of magazine barrels 89 .
The pressure chamber 79 has a recess 97 having an air exit opening 98 therein defined by an inwardly extending annular flange 99 . A spring biased sealing plate 100 is mounted within recess 97 . The sealing plate 100 has a central bore 101 configured to overlay the mounting plate openings 91 of the magazine. It should be noted that the mounting plate openings 91 are positioned so that the sealing plate bore 101 overlaps only one opening 91 at a time. A gasket 103 is mounted to the sealing plate 100 to ensure sealing engagement with the mounting plate 88 . The release valve 80 has a cylindrical manifold 105 and a cylindrical plunger 106 slidably mounted within the manifold 105 . Plunger 106 has a gasket 107 to ensure sealing engagement of the plunger 106 about opening 98 with the plunger in a sealing position shown in FIG. 9, and a O-ring type seal 109 to ensure sealing engagement of the plunger 106 against manifold flange 99 with the plunger in a released position shown in phantom lines in FIG. 9 .
The control valve 81 has an elongated cylindrical manifold 112 having a top vent opening 113 to ambience, a side opening 114 in fluid communication with release valve manifold 105 , and a cylindrical plunger 115 slidably mounted within manifold 112 . Plunger 115 has a gasket 116 to ensure sealing engagement of the plunger about vent opening 113 with the plunger in a pressurized position shown in FIGS. 7 and 9.
The indexer 82 has a pressure cylinder 119 coupled in fluid communication with pressure chamber 79 by a pressure tube 120 . A piston 121 , having an elongated piston rod 122 , is mounted within the indexer pressure cylinder 119 for reciprocal movement therein between a low pressure position shown in FIG. 8 and a high pressure position shown in FIGS. 7 and 9. A coil spring 123 is mounted about piston rod 122 so as to bias the piston 121 towards its low pressure position. A spring biased indexing finger 125 is pivotably mounted to piston rod 125 . Indexing finger 125 is configured to sequentially engage and ride within each magazine groove 95 as the piston rod is moved upward and to disengage the groove as the piston rod is moved downward. All references herein to downward and upward directions is for purposes of clarity in reference to the drawings and is not meant to indicate gravity sensitivity.
The air pump 76 includes an elongated cylinder 128 and a plunger 129 telescopically mounted for reciprocal movement within the cylinder 128 . Plunger 129 has a tubular shaft 130 with an enlarged sealing end 131 and a handle 132 opposite the Ft sealing end 131 . Sealing end 131 has an O-ring type seal 133 with an opening 134 therethrough, and a conventional check valve 135 mounted within opening 134 . Check valve 135 is oriented to allow air to pass from the interior of cylinder 128 through opening 134 into the interior of shaft 130 and to prevent air from passing through opening 134 in the opposite direction. Handle 132 has a vent 136 therethrough which allows air to pass from ambience into the interior of shaft 130 .
Pump cylinder 128 has an open end 138 through which plunger 129 extends and a closed end 139 . The pump cylinder 128 also has a port 140 in fluid communication with pressure tube 78 and a vent 141 adjacent open end 138 which is open to ambience. Port 140 is spaced from closed end 139 so as to allow seal 133 of plunger 129 to be moved past the port 140 to a position closely adjacent to the closed end 139 , as shown in FIG. 8 .
In use, a person dons the gun by securing the head harness 77 to his head with the magazine 75 to one side. The person then actuates the pump 76 by grasping the pump handle 132 and forcing the pump plunger 129 through cylinder 128 towards port 140 thereby pressurizing air within the cylinder. Thus, the plunger 129 is moved from a first position shown in phantom lines in FIG. 7 to generally a second position shown in FIG. 7 . The pressurized air passes through port 140 into pressure tube 78 where it then passes through control valve 81 . The increase in air pressure within the control valve manifold 112 forces the control valve plunger 115 to move to an upper, pressurized position sealing vent opening 113 , as shown in FIG. 9 . The pressurized air then passes about plunger 115 and through side opening 114 into the release valve manifold 105 . The increase in air pressure within the release valve manifold 105 forces the control valve plunger 106 to move to a forward, pressurized position sealing opening 98 , as shown in FIG. 9 . The pressurized air then flows between the release valve plunger 106 and the release valve manifold 105 into pressure chamber 79 .
A portion of the pressurized air within pressure chamber 79 passes through pressure tube 120 into the indexer pressure cylinder 119 . With increased pressure within pressure cylinder 119 the indexer piston 121 is forced upwards against the biasing force of coil spring 123 , i.e. the indexer piston 121 is moved from its low pressure position shown in FIG. 8 to its high pressure position shown in FIGS. 7 and 9. As shown in FIG. 9, upward movement of the piston rod 122 causes the finger 125 to ride up within a mounting plate groove 95 to cause counter-clockwise rotation of the magazine 75 as indicated by arrows in FIGS. 7 and 8.
With continued movement of the pump plunger 129 within pump cylinder 128 the seal 133 passes pump cylinder port 140 , as shown in FIG. 8 . With the plunger seal 133 in this position pressurized air within pressure tube 78 is released back into pump cylinder 128 behind seal 133 and then to ambience through vent 141 . The reentry of pressurized air into the pump cylinder 128 from pressure tube 78 causes the control valve plunger 115 to move to a downward position unsealing vent opening 113 , as shown in FIG. 8 . Thus, the decrease in air pressure within the pressure tube 78 and control valve manifold 112 triggers the actuation of control valve 81 to its open configuration. The actuation of the control valve to its open, downward position causes a release of pressurized air from within release valve manifold 105 through the control valve side opening 113 and then through vent opening 113 to ambience. This decrease in pressure causes release valve plunger 106 to move to a rearward position unsealing opening 98 , as shown in phantom lines in FIG. 9 . The position of the plunger 106 also causes and the O-ring to abut manifold 105 to seal the path between the manifold 105 and plunger 106 . With the unsealing of opening 98 pressurized air within pressure chamber 79 rapidly flows through opening 98 , through sealing plate bore 101 , through magazine mounting plate opening 91 , and into launch tube 90 in register with the sealing plate 100 where it propels the projectile P from barrel 89 . Operation of this type of release valve is described in more detail in U.S. Pat. No. 4,159,705.
Upon the release of pressurized air from pressure chamber 79 the pressurized air within indexer pressure cylinder 119 is conveyed through pressure tube 120 back into pressure chamber 79 . This release of pressurized air from indexer pressure cylinder 119 causes the indexer piston 121 to be spring biased by coil spring 123 back downward to its low pressure position. The downward movement of piston 121 pivotally retracts the indexing finger 125 from mounting plate groove 95 and positions the finger in register with the following mounting plate groove.
The pump plunger 129 may then be manually drawn back to its initial position to pressurize and fire the gun again. The drawing back of the pump plunger 129 does not create a vacuum within pump cylinder 128 since replenishment air may be drawn through vent 136 into the plunger handle 132 , through the interior of shaft 130 , and through check valve 135 into cylinder 128 . Air between the pump cylinder 128 and the plunger 129 behind seal 134 is expelled from cylinder 128 through vent 141 .
It should be noted that pawl 94 engages notches 93 to prevent rotation of the magazine 75 in a direction opposite to its indexing direction, i.e. to prevent clockwise rotation of the magazine with reference to FIGS. 7 and 8. This prevents the firing of pressurized air into a previously emptied barrel and damage to the indexing finger 125 .
As an alternative, gun 70 may also be constructed without control valve 81 . The need for the control valve is dependent upon the length and interior diameter of pressure tube 78 , i.e. the volume of air contained within the pressure tube. For a pressure tube 78 having a small interior volume the release of air therefrom causes rapid actuation of release valve 80 . Conversely, with a pressure tube 78 containing a large volume of air therein the release of air therefrom may be inadequate to actuate the release valve properly. Thus, with pressure tubes having a large volume therein a control valve 81 is coupled to the release valve 80 to ensure rapid decompression within release valve manifold 105 to actuate the release valve. The gun may also be constructed without the inner launch tube 90 within the barrel 89 . Here, the pressurized air expelled from pressure chamber 79 is directed into barrel 89 behind the projectile. This design however is not preferred as it does not concentrate the burst of pressurized air for optimal efficiency and performance. Lastly, it should be understood that the magazine and indexer of FIGS. 6-9 may also be adapted to a hand held gun of conventional design.
It should be understood that the gun of FIGS. 6-9 may also be adapted to include the two concentric circle arrangement of the opening, as shown in FIGS. 1-5, to increase the dart capacity of the magazine.
With the air gun of this construction a child may aim the gun simply by facing the intended target and manually actuating the hand pump. Because of the elongated, flexible pressure tube 78 the pump may be manipulated substantially independently of and without effecting the air of the launch tube. Thus, the gun is of an unconventional design to interest children yet is capable of being easily aimed and fired. Also, the child may fire several shots sequentially without having to reload between each successive shot.
With reference next to FIGS. 10 and 11, a compressed air gun 159 in another preferred form is shown. Here, the air gun 159 is similar in basic construction to that shown in FIGS. 1-5, except for the internal components for the sequential firing of pressurized air bursts and pneumatic indexing of the magazine, and the magazine grooves 160 are angled rather than being L-shaped. For this reason, only the new, alternative components of the air gun are shown for clarity and conciseness of explanation.
The air gun 159 has a pneumatic firing actuator 161 coupled to the pressure tank through pressure tube 56 . Actuator 161 includes an elongated manifold 162 having an inlet opening 163 in fluid communication with pressure tube 56 , an outlet opening 164 in fluid communication with a small pressure tank or pressure cell 165 , and an open end or firing opening 166 in fluid communication with an elongated recess 167 . A piston 168 is mounted for reciprocal movement within actuator manifold 162 . Piston 168 has a forward seal 169 , a rearward seal 170 and a clear button 171 extending through the air gun housing. The actuator 161 also has a flexible gasket 172 mounted within recess 167 in sealable contact with magazine 18 , and a pressure cylinder 173 in fluid communication with pressure cell 165 by a conduit 174 . A piston 175 , having an elongated piston rod 176 , is mounted within the actuator pressure cylinder 173 for reciprocal movement therein between a low pressure, pressurizing position shown in FIG. 10 and a high pressure, firing position shown in FIG. 11. A coil spring 177 mounted about piston rod 176 biases the piston 175 towards its low pressure position. Piston rod 176 is coupled to piston 168 by an over center torsion spring 179 . An indexing finger 180 , mounted to an end of the piston rod 176 , is configured to sequentially engage and ride within each magazine groove 160 for sequential rotation of the magazine.
In use, an operator actuates the pump to pressurize a supply of air by grasping the handle 22 and reciprocating the cylinder rod 21 back and forth within the cylinder 20 . With piston 168 in its rearward pressurized air is passed through pressure tube 16 into the pressure tank 15 . Manual actuation of the trigger 13 moves the trigger to a position wherein it unpinches pressure tube 56 so as to allow pressurized air within the pressure tank 15 to pass through pressure tube 56 into actuator manifold 162 through inlet opening 163 and between the forward and rearward seals 169 and 170 of piston 168 . The pressurized air then passes out of manifold 162 through outlet opening 164 and into pressure cell 165 , conduit 174 , and pressure cylinder 173 . The pressurized air within the pressure cylinder 173 causes piston 175 to move toward its high pressure position against the biasing force of coil spring 177 , i.e. the piston 175 is moved from its low pressure position shown in FIG. 10 to its high pressure position shown in FIG. 11 .
As shown in FIG. 11, forward movement of the piston 175 causes compression and rotation of torsion spring 179 and the indexing finger 180 to move forward into a magazine groove 160 , thereby causing rotation of the magazine 18 and alignment of the opening to change to the inner circle of openings 28 ″. All references herein to forward and rearward is for purposes of clarity in reference to the drawings. Upon reaching the apex of the movement of piston rod 176 the torsion spring 179 reaches a rotated position which causes decompression of the spring thereby forcing piston 168 rearward, as shown in FIG. 11 . Rearward movement of piston 168 causes the forward seal 169 to be moved to a positioned between inlet opening 163 and the outlet opening 164 . This positioning of the piston 168 isolates manifold inlet opening 163 to prevent escape of pressurized air from pressure tank 15 , i.e. the seals sandwich the inlet opening to prevent the flow of air from the pressure tank. This positioning of the forward seal 169 also allows pressurized air within the pressure cell 165 , conduit 174 and pressure cylinder 173 to flow through outlet opening 164 into the manifold and from the manifold through firing opening 166 , through sealed recess 167 and into the launch tube 27 through magazine opening 28 ′. Pressurized air within launch tube 27 propels the projectile out of the magazine barrel 26 and through gun barrel 12 .
The release of pressurized air from pressure cylinder 173 causes the piston 175 to be spring biased by coil spring 177 back rearward to its low pressure position. The rearward movement of piston 175 retracts the indexing finger 180 from within a mounting plate groove 160 and positions the finger in register with the following mounting plate groove 160 . The low pressure positioning of piston 175 causes the torsion spring 179 to bias piston 168 forwards to its initial position with the forward and rearward seals 169 and 170 sandwiching or straddling inlet and outlet openings 163 and 164 , as shown in FIG. 10 . This repositioning of piston 168 once again causes pressurized air within pressure tank 15 to flow through pressure tube 56 into actuator manifold 162 , thereby completing a firing-cycle. The firing and indexing cycle just describe may continue in rapid sequence so long as the trigger is maintained in a position allowing the flow of pressurized air through pressure tube 56 and the pressure tank continues to contains a minimal level of pressurized air sufficient to overcome the biasing force of springs 177 and 179 , i.e. the release valve is automatically actuated by actuator 161 and the indexing of magazine 18 continues so long as the trigger is pulled open and the pressure tank contains pressurized air above a level to overcome springs 177 and 179 . Should the pressure level within pressure tank 15 reach the minimal level the operator simply actuates the manual air pump 14 so as to once again elevate the pressure within the pressure tank.
As described, the gun may be used in a fully automatic manner such that with the trigger maintained in a pulled back, actuated position the gun fires a series of projectiles without stopping between each successive shot, similar to the action of a machine gun. However, should an operator wish to fire a single projectile, one need only to pull the trigger and quickly release it so that pressurized air does not continue to flow into the actuator 161 . Operated in such a manner the gun will index the magazine and fire a projectile with each actuation of the trigger, again, so long as the pressure tank contains air pressurized above the minimal level and the trigger is quickly released.
It should be understood that at times rubber seals often stick when stored for a period of time. This sticking may hamper the performance of the actuator. For this reason, the actuator is provided with clear button 171 which may be manually actuated to cause reciprocal movement of the piston in order to unstick the seals.
With reference next to FIGS. 12-15, there is shown a compressed air gun in another preferred embodiment, with like numbers referring to previously described components. Here, the air gun has a combination control valve and indexer 200 which controls the flow of compressed air from the pressure tank 15 to the magazine launch tubes 201 and indexes the magazine 202 with each firing, hereinafter referred collectively as control valve 200 .
The control valve 200 has an elongated, cylindrical, external tube or manifold 204 , a cylindrical, internal tube 205 mounted within the external tube 204 , and a plunger 206 mounted within the internal tube. The external tube 204 has an elongated slot 208 , an air inlet 209 in fluid communication with pressure tube 56 , and an air outlet 210 in fluid communication with magazine launch tubes 201 . The internal tube 205 is configured to move reciprocally within the external tube between a forward position shown in FIG. 13 and a rearward position shown in FIGS. 14-16. The internal tube 205 and external tube 204 define a first air pressure chamber 212 therebetween, while the internal tube 205 and plunger 206 define a second air pressure chamber 213 therebetween. The internal tube 205 has an air release valve 215 , an O-ring seal 216 for sealing engagement of the internal tube with the external tube, and an L-shaped member 218 extending through slot 208 . L-shaped member 218 has an end flange 219 .
Plunger 206 is mounted within the internal tube 205 for reciprocal movement between a first sealing position abutably sealing air outlet 210 as shown in FIG. 13, a second sealing position extending from the internal tube yet still sealing air outlet 210 as shown in FIGS. 14 and 15, and an unsealing position distal from and unsealing air outlet 210 as shown in FIG. 16 . The air release valve 215 has an opening 221 , a plunger 222 mounted within opening 221 , an elongated rod 223 , and a coil spring 224 mounted about elongated rod 223 . The air gun also has a spring biased trigger 227 configured to releasably engage the internal tube L-shaped member 218 .
A coil spring 229 is mounted within internal tube 205 so as to abut plunger 206 and bias the plunger in a direction towards the air outlet 210 . Another coil spring 230 is mounted between the external tube 204 and the internal tube 205 so as to bias the internal tube in a direction towards the air outlet 210 .
The magazine 202 has an annular array of Z-shaped grooves 232 sized and shaped to receive the end flange 219 of the L-shaped member 218 . Each groove 232 has a forward camming surface 233 extending to a forward portion 234 and a rearward camming surface 235 extending to a rearward portion 236 .
In use and with the trigger 227 spring biased to its position engaging the internal tube L-shaped member 218 , the internal tube 205 is initial spring biased to its forward position by compressing spring 230 , as shown in FIG. 13 . This position of the internal tube forces spring 229 to bias plunger 206 to its sealing position. With the internal tube 205 in its forward position, the L-shaped member flange 219 resides within the Z-shaped groove forward portion 234 , as shown in FIG. 21 . It should be understood that the magazine of FIGS. 21 and 22 is illustrated with only one launch tube for clarity of explanation.
As compressed air flows from the pressure tube 56 , extending from the pressure tank 15 , and into the control valve 200 through air inlet 209 , the pressure within the first air pressure chamber 212 increases. Compressed air also passes from the first air pressure chamber, between the plunger 206 and the internal tube, into the second air pressure chamber 213 . The air pressure within the first and second air pressure chambers aid in maintaining the plunger 206 in its sealing position, as the pressure upon the backside of the plunger is greater than ambient air pressure upon the front side of the plunger.
As shown in FIG. 14, with movement of the trigger 227 to its release position disengaged from the L-shaped member, the compressed air within the first air pressure chamber 212 causes the internal tube 205 to move to its rearward position. This movement of the internal tube compresses spring 230 . As the internal tube moves rearward the L-shaped member flange 219 ′ contacts the rearward camming surface 235 , as shown in phantom lines in FIG. 22 . With continued rearward movement of the internal tube, flange 219 ″ continues into the rearward portion 236 of the Z-shaped groove, as shown in FIG. 22 . The force of the flange upon the rearward camming surface causes the magazine to rotate clockwise approximately half the distance of a complete indexing cycle.
As the internal tube approaches the end of its rearward stroke the release valve spring 224 compresses to a point wherein the force of the spring overcomes the force of the air pressure within the second air pressure chamber 213 . This spring force causes the valve plunger 206 to move forward thereby unseating and allowing the compressed air within the second air pressure chamber 213 to escape rapidly therefrom through opening 221 , as shown in FIG. 15 . This rapid decompression of the second air pressure chamber 213 causes plunger 206 to snap back to its unsealing position, as shown in FIG. 16 . With the plunger in its unsealing position, the compressed air within the first pressure chamber 212 quickly passes through the air outlet 210 and into the launch tube 201 .
The release of the compressed air within the first air pressure chamber 212 causes the internal tube to move forward, through the spring biasing force of coil spring 230 . The forward movement of the internal tube causes the L-shaped member flange 219 ′″ to contact the forward camming surface 233 , as shown in phantom lines in FIG. 22, and thus force the remaining indexing rotation of the magazine as the flange 219 once again resides within the forward portion 234 , as shown initially in FIG. 21 .
It should be understood that so long as the trigger is actuated to its disengaged position and so long as there is sufficient air pressure flowing from the pressure tube, the control valve will continue to fire projectiles, as the internal tube and plunger will continue to reciprocate as long as a sufficient amount of compressed air is present to overcome the forces of the springs. Alternatively, the trigger may be pulled and immediately released so that it reengages the L-shaped member after firing a single projectile.
With reference next to FIGS. 17-20, there is shown the internal components and a portion of the magazine of a compressed air gun in another preferred embodiment, similar to that previously described in reference to FIGS. 12-16. Here again, the air gun has a combination control valve and indexer 300 which controls the flow of air from the pressure tank 15 to the magazine launch tubes 201 and indexes the magazine 202 with each firing, hereinafter referred collectively as control valve. The control valve 300 has an elongated, cylindrical, external tube or manifold 304 , an internal tube 305 mounted within the external tube 304 , and a plunger 306 mounted within the internal tube. The external tube 304 has an elongated slot 308 , an air inlet 309 in fluid communication with pressure tube 56 , and an air outlet 310 in fluid communication with magazine launch tubes 201 . The internal tube 305 is configured to move reciprocally within the external tube between a forward position, shown in FIG. 17 and a rearward position, shown in FIGS. 18-20. The internal tube 305 and external tube 304 define an air pressure chamber 312 therebetween. The internal tube 305 has an O-ring seal 316 for sealing engagement of the internal tube with the external tube, and an L-shaped member 318 extending through slot 308 . L-shaped member 318 has an end flange 219 . A coil spring 329 is mounted about the plunger 306 for biased movement of the plunger in a rearward direction.
Plunger 306 is mounted within the internal tube for reciprocal movement between a first sealing position abutably sealing air outlet 310 as shown in FIG. 17, a second sealing position extending from the internal tube yet still sealing air outlet as shown in FIGS. 18 and 19, and an unsealing position distal from and unsealing air outlet as shown in FIG. 20 . The air gun also has a spring biased trigger 327 configured to releasably engage the internal tube L-shaped member 318 .
A coil spring 330 is mounted about plunger 306 between the forward end of the internal tube and a sealing head 331 of the plunger. Coil spring 330 biases the plunger in a direction towards the air outlet. Another coil spring 328 is mounted between the external tube 304 and the internal tube so as to bias the internal tube in a direction towards the air outlet.
The magazine 202 has an annular array of Z-shaped grooves 232 sized and shaped to receive the end flange 219 of the L-shaped member 318 . Each groove 232 has a forward camming surface 233 extending to a forward portion 234 and a rearward camming surface 235 extending to a rearward portion 236 .
In use and with the trigger 327 is spring biased to its position engaging the internal tube L-shaped member, the internal tube 305 is initial spring biased to its forward position compressing spring 330 . This position of the internal tube forces spring 330 to bias plunger 306 to its sealing position. With the internal tube 305 in its forward position, the L-shaped member flange 219 resides within the Z-shaped groove forward portion 234 , as shown in FIG. 21 .
As compressed air flows from pressure tube 56 and into the control valve 300 through air inlet 309 , the pressure within air pressure chamber 312 increases. This air pressure aids in maintaining the plunger in its sealing position, as the pressure upon the backside of the plunger is greater than ambient air pressure upon the front side of the plunger.
As shown in FIG. 18, with movement of the trigger to its release position disengaging the L-shaped member, the compressed air within the air pressure chamber 312 causes the internal tube 305 to move to its rearward position. This movement of the internal tube compresses springs 328 and 329 . As the internal tube moves rearward the L-shaped member flange 219 ′ contacts the rearward camming surface 235 so as to cause the magazine to rotate clockwise approximately half the distance of a complete indexing cycle, as shown in phantom lines in FIG. 22 . The flange 219 ″ continues into the rearward portion 236 of the Z-shaped groove.
As the internal tube moves to the end of its rearward stroke the plunger spring 329 compresses to a point wherein the force of spring 329 overcomes the force of the compressed air within the air pressure chamber 312 and upon the plunger sealing head 331 . This spring force causes the plunger 306 to move rearwardly to its unsealing position, thereby allowing the compressed air within the air pressure chamber to escape through the air outlet 310 , as shown in FIG. 19 . The release of the air pressure force upon the plunger allows spring 329 to force plunger 306 quickly rearward to maximize the rapid decompression of the air pressure chamber 312 , as shown in FIG. 19 .
The release of the compressed air within the air pressure chamber 312 causes the internal tube to move forward, through the spring biasing force of coil spring 328 . The forward movement of the internal tube causes the L-shaped member flange 219 ′″ to contact the forward camming surface 233 , as shown in phantom lines in FIG. 22, and thus force the remaining indexing rotation of the magazine as the flange once again resides within the forward portion 234 , as shown initially in FIG. 21 . Again, the internal tube and plunger may continue to reciprocate as long as the trigger is disengaged and there is sufficient air pressure.
It should be understood that the second air pressure chamber 213 of FIGS. 13-16 performs the same function as spring 329 in FIGS. 17-20, as they both function to snap the plunger rearward upon initial firing.
The gun shown in FIGS. 17-20 may also be adapted to include an internal flange 340 , shown in phantom lines, extending from the external tube 305 . Flange 340 has a opening 341 therethrough through which plunger 306 extends. Spring 330 abuts flange 340 so that the spring is slightly compressed to force plunger 306 towards its sealing position. As the internal tube 305 moves rearward the spring 330 is compressed further. As air is released from the first air chamber 312 , as previously described, spring 330 decompresses so as to force plunger 306 to is sealing position.
It should also be understood that compressed air may be directed into the control valve without the use of a pressure tank 15 , as shown in reference to FIGS. 6-9. As such, the control valve may be coupled directly to a pump. Also, the triggering of the control valve, and thus the toy gun, may be accomplished through a valve or regulator mounted between the pressurized air source and the control valve, as shown in the previous embodiments.
With reference next to FIGS. 23-26, there is shown the internal components of a fluid pulsator 400 in another preferred embodiment, similar to the control valve previously described in reference to FIGS. 12-16 and 17 - 20 . The fluid pulsator may be used to control the release of compressed air, as previously described, in compressed air guns or to control the release of pressurized water in discrete bursts in water guns. When used in conjunction with an air gun the pulsator acts as a combination control valve and indexer which controls the flow of air from the pressure tank 15 to the magazine launch tubes 201 and which indexes the magazine 202 with each firing.
The pulsator 400 has an elongated, cylindrical, housing or manifold 404 , an internal tube or plunger 405 mounted within the housing 404 , and a sealing member 406 mounted about the internal tube. The housing 404 has a rear opening 408 through which extends the internal tube, a fluid inlet 409 in fluid communication with pressure tube 56 , and a fluid outlet 410 , in fluid communication with magazine launch tubes 201 of an air gun or ambience with a water gun. The internal tube 405 has a fluid inlet 420 , a fluid outlet 421 and a post 422 about which is mounted the sealing member 406 . The internal tube 405 is configured to move reciprocally within the housing between a forward position, shown in FIG. 23, and a rearward position, shown in FIGS. 24-26. The internal tube 405 and housing 404 define a rearward fluid pressure chamber 412 and a forward fluid pressure chamber 413 therebetween. The internal tube 405 has a sealing edge 416 for sealing engagement of the internal tube with the housing, and an L-shaped linkage member 418 . In an air gun the L-shaped member 418 has a previously described end flange 219 , while in a water gun the L-shaped member 418 extends to a sleeve 419 coupled to the end of the barrel for reciprocal movement relative to the barrel. The sealing member 406 has an opening 424 therethrough and a resilient sealing head 431 having a first portion 432 having a size and shape larger than fluid outlet 410 and a second portion 433 sized and shaped to be received within the fluid outlet 410 . A coil spring 429 is mounted within the sealing member 406 and about the post 422 for biased movement of the sealing member in a rearward direction as the spring is compressed, as shown in FIG. 26 .
Sealing member 406 is mounted about the internal tube post 422 for reciprocal movement between a first sealing position sealing fluid outlet 410 as shown in FIG. 23, a second sealing position extending from the internal tube yet still sealing fluid outlet as shown in FIGS. 24 and 25, and an unsealing position distal from and unsealing fluid outlet as shown in FIG. 26 . The air or water gun also has a spring biased trigger 427 configured to engage and disengage the internal tube L-shaped member 418 .
In an air gun configuration, the previously described magazine 202 has an annular array of Z-shaped grooves 232 sized and shaped to receive the end flange 219 of the L-shaped member 418 . Each groove 232 has a forward camming surface 233 extending to a forward portion 234 and a rearward camming surface 235 extending to a rearward portion 236 .
In use and with the trigger 427 spring biased to its position engaging the internal tube L-shaped member, the internal tube 405 is maintained in its forward position while fluid enters the pulsator. With the internal tube 405 in its forward position, the L-shaped member flange 219 resides within the Z-shaped groove forward portion 234 , as shown in FIG. 21 .
As pressurized fluid flows from pressure tube 56 and into the pulsator 400 through fluid inlet 409 , the pressure within the rearward fluid pressure chamber 412 increases. The pressurized fluid passes through internal tube fluid inlet 420 , through internal tube fluid outlet 421 between the internal tube 405 and sealing member 406 , through sealing member opening 424 and slowly into the forward fluid pressure chamber 413 , i.e. the fluid slowly passes from inside the internal tube and between the internal tube and sealing member to the forward fluid pressure chamber 413 , See FIG. 23 . As shown in FIG. 24, with movement of the trigger 427 to its release position disengaging the L-shaped member, the pressurized fluid within the forward fluid pressure chamber 413 and within the internal tube 405 overcomes the fluid pressure within the rearward fluid pressure chamber which causes the internal tube to move towards its rearward position. As the internal tube moves rearward its fluid outlet 421 is positioned past the end of the sealing member, thus causing the unrestricted flow of fluid therethrough and into the forward fluid pressure chamber 413 , rather than the slow flow previously associated with the fluid outlet 421 . As shown previously in FIG. 22, this movement also causes the L-shaped member flange 219 ′ of an air gun to contact the rearward camming surface 235 so as to cause the magazine to rotate clockwise approximately half the distance of a complete indexing cycle, as shown in phantom lines in FIG. 22 . The flange 219 ″ continues into the rearward portion 236 of the Z-shaped groove.
As the internal tube moves to the end of its rearward stroke the spring 429 compresses to a point wherein the force of spring overcomes the force of the pressurized fluid within the forward fluid pressure chamber 413 and upon the sealing member head 431 . This spring force causes the sealing member 406 to move rearwardly to its unsealing position, thereby allowing the pressurized fluid within the forward pressure chamber 413 to escape through the fluid outlet 410 , as shown in FIG. 26 . The release of the fluid pressure force upon the sealing member allows spring 429 to force sealing member 406 quickly rearward to maximize the rapid decompression of the rearward fluid pressure chamber 412 . The release of the pressurized fluid within the forward pressure chamber 413 causes the internal tube to move forward, through the biasing force of the fluid entering the rearward pressure chamber 412 .
In an air gun, the forward movement of the internal tube causes the L-shaped member flange 219 ′″ to contact the forward camming surface 233 , as shown in phantom lines in FIG. 22, and thus force the remaining indexing rotation of the magazine as the flange once again resides within the forward portion 234 , as shown initially in FIG. 21 . Again, the internal tube and sealing member may continue to reciprocate as long as the trigger is disengaged and there is sufficient fluid pressure. In a water gun, the movement of the L-shaped member also reciprocates sleeve 419 , as shown in FIG. 29 . This reciprocating movement of the sleeve resembles the recoil action of a machine gun.
Referring next to FIGS. 27-28, there is shown the internal components of a fluid pulsator 500 in another preferred embodiment, although similar to that previously described in reference to FIGS. 23-26. Here however, the fluid is introduced through the internal tube 505 and it is the housing 504 that moves relative to the stationary internal tube 505 , although this embodiment may be easily adapted so that the internal tube moves while the housing remains stationary. Nevertheless, the components thereof act and function similarly to those previously described. It should also be noted that a pressure release opening 503 , or series of openings, extends through the sealing member to release fluid pressure within the sealing member as the post 422 moves therein.
A distinct advantage of the present invention is the configuration of the sealing head 431 . Prior art sealing heads did not include the second portion. As such, as the sealing head would move slightly away from the fluid outlet 410 the fluid would rush between the small space between the sealing head and the housing defining the fluid outlet and into the larger space of the fluid outlet. This rushing of fluid into a larger space creates a low pressure cell in the area of the outlet which tends to pull the sealing head back into sealing engagement with the housing. Thus, the sealing head would flutter which would hamper the quick and precise release of the seal. In the present invention, the second portion 433 remains within the fluid outlet 410 as the sealing head moves rearward and separates from the housing. Thus, an additional fluid pressure is exerted upon the forward facing surface of the sealing head first portion 432 which causes the sealing member to move rearward with greater force prior to the final separation of the sealing member second portion 433 and housing. Also, the tapering of the fluid outlet causes a greater flow of fluid between the sealing head and housing with relative movement of the sealing head.
It should be understood that in the embodiments of FIGS. 23-26 and 27 - 28 the pressurized fluid may be directed into the pulsator without the use of a pressure tank 15 , as shown in reference to FIGS. 6-9. As such, the pulsator may be coupled directly to a pump. It should also be understood that internal tube fluid outlet 421 , with or without adjacent opening 424 , varies the flow of fluid passing therethrough in relation to the relative positions of the internal tube and sealing member, and as such may be referred to as variable flow valve means. However, the present invention is not limited to this embodiment of a variable flow valve and may include many other types of mechanical valves, for example that of the tapered needle type valve shown in FIG. 30, or methods of creating a flow path between the forward and rearward fluid pressure chambers, such as an imperfect seal between the housing and internal tube or a passage through the internal tube. It should be understood that as an alternative to the mechanical trigger shown herein the trigger T may also be in the form of a fluid control valve or regulator, previously described or shown in phantom lines in FIG. 27, which controls the flow of fluids passing through the fluid inlet 409 or internal tube 505 .
Referring next to FIGS. 31-33, there is shown the internal components of a fluid pulsator 600 in another preferred embodiment, although similar to that previously described in reference to FIGS. 27-28. These figures correspond to the actuation described in detail in FIGS. 23-26. Here again, and housing 604 has an internal tube opening 607 and a fluid outlet 608 , and the fluid is introduced through the internal tube or plunger 605 . The housing 604 moves relative to the stationary internal tube 605 , although this embodiment may be easily adapted so that the internal tube moves while the housing remains stationary. The internal tube 605 has a sealing head with a conventional seal adjacent thereto which divides the interior of the housing into a forward pressure chamber 631 and a rearward pressure chamber 632 . The pulsator is shown with a magazine indexing arm 609 similar to that previously shown, which is present only when the pulsator is used in conjunction with an compressed air gun having a magazine and is not used in connection with water guns.
In addition to the previously recited components, this embodiment includes an internal tube biasing spring 611 for biasing the internal tube 605 to its forward position and means for adjustably actuating the movement of the movable sealing member 606 in direct relationship to the distance traveled or position of the internal tube 605 relative to the housing. To accomplish this adjustable actuation the internal surface of sealing member 606 is provided with internal threads 612 configured to correspond with the external threads 613 of an annular spring stop 614 having an opening 615 therethrough through which post 622 movably extends. The external surface of the sealing member 606 is also provided with a outwardly extending flange 617 configured to abut laterally with an inwardly extending flange 618 extending from the internal surface of the housing 604 to prevent rotation of the sealing member 606 relative to the housing. With this construction the manual rotation of the housing 604 causes the spring stop 614 to threadably move along the longitudinal axis of the sealing member 606 thereby varying the distance between the spring stop 614 and the end stop 615 of the post 622 . FIG. 31 shows the spring stop 614 , depicted in phantom lines in an alternative position along the internal tube.
It should be understood that with the spring stop 614 positioned distally from the post end stop 616 the internal tube must move a relatively large distance relative to the housing before the spring 629 fully compresses, as shown in FIGS. 32 and 33, and the sealing member is moved from its sealing position towards its unsealing position, i.e. the sealing member is actuated, as shown in FIG. 33 . Conversely, should the spring stop 614 be positioned proximal to the post end stop 616 the internal tube 605 need only move a relatively short distance before the spring 611 is compressed and the sealing member 606 is actuated. A short distance of travel of the internal tube allows the pulsator to be actuated quicker than with a long distance of travel. Thus, one may adjust the pulse rate or cycling rate of the pulsator, and thus the fluid therefrom, by adjusting the position of the spring stop through rotation of the housing.
Again, it should be understood that in the embodiments of FIGS. 31-33 the pressurized fluid may be directed into the pulsator without the use of a pressure tank 15 , as shown in reference to FIGS. 6-9. As such, the pulsator may be coupled directly to a pump. It should also be understood that internal tube fluid outlet 621 varies the flow of fluid passing therethrough in relation to the relative positions of the internal tube and sealing member, and as such may be referred to as variable flow valve means. However, the present invention is not limited to this embodiment of a variable flow valve and may include many other types of mechanical valves, for example that of the tapered needle type valve shown in FIG. 30, or methods of creating a flow path between the forward pressure chamber 631 and rearward pressure chamber 632 , such as an imperfect seal between the housing and internal tube or a passage through the internal tube. It should be understood that this embodiment may work with either a mechanical trigger adapted to engage the housing or a fluid controlling trigger which controls the flow of fluid into the pulsator.
Lastly, it should be understood that as an alternative to the internal tube biasing spring 611 shown in the drawings the internal tube may include a fluid exit 630 in fluid communication with the rearward fluid pressure chamber. This modification replaces the biasing force provided by the internal tube biasing spring 611 with a biasing force provided by pressurized fluid within the rearward fluid pressure chamber, as previously described in reference to FIGS. 23-26.
With reference next to FIG. 34, there is schematically shown a compressed air gun 700 in yet another preferred embodiment. Here the compressed air gun 700 has a pressure chamber 701 with a release valve 702 therein in fluid communication with a launch tube 703 . The pressure chamber 701 is in fluid communication with an air pump 704 through a conduit 705 . The air pump 704 is coupled to an electric motor 707 which is electrically coupled to a battery 708 through a conductor 709 . An off/on switch 710 is also coupled to the conductor in series to the electric motor 707 . A pressure releasing trigger 712 and a pressure sensitive actuation switch 713 are also coupled to the conduit 705 . The pressure sensitive actuation switch 713 is also in fluid communication with conduit 705 so as to sense the pressure therein, which also reflects the pressure within the pressure chamber 701 .
As best illustrated in FIG. 37, the pressure sensitive actuation switch 713 has a cylindrical housing 716 , a cap 717 threadably mounted to the housing 716 , a plunger 718 movably mounted within the housing 716 and a spring 719 mounted between the plunger 718 and the cap 717 . The plunger 718 has a head portion 720 with an annular conductive bridge 721 and a stem portion 722 depending from the head portion 720 . The stem portion 722 has an annular groove 723 having an O-ring 724 mounted therein which forms a seal between the stem portion 722 and the housing 716 . Conductor 709 is coupled to two conductive ends 726 which are mounted to opposite sides of the housing 716 adjacent and contactable with conductive bridge 721 .
An operator may set the pressure level at which the actuation switch 713 is activated and de-activated. The safety switch spring 719 biases plunger 718 in a direction to cause the conductive bridge 721 to contact the ends 726 of the conductor 709 so as to close the conductive path therebetween and complete the circuit. As the actuation switch is also coupled to conduit 705 the air pressure therein acts upon the plunger stem portion 722 in a direction opposite to that of the biasing force of spring 719 . Thus, it should be understood that the threaded movement of the cap 717 upon housing 716 directly corresponds to the air pressure necessary to overcome the biasing force of the spring, i.e. the further the cap is threaded on the housing the further compressed the spring 719 becomes and thus the greater the air pressure must be to overcome the spring biasing force to move the plunger conductive bridge 721 out of contact with the conductor ends 726 . The threaded position of actuation switch cap 717 thus limits the pressure of the air within the gun and thus the pressure of the burst of air emitted.
In use, the operator initially actuates the on/off switch 710 to its on position. As the pressure within the pressure chamber 701 and conduit 705 is initially at atmospheric pressure the actuation switch conductive bridge 721 is in electrical contact with conductor ends 726 thus closing the circuit with electric motor 707 . The activation of the electric motor 707 drives air pump 704 so as to convey pressurized air through conduit 705 and into pressure chamber 701 . The increase in air pressure within the pressure chamber actuates the release valve as previously described. As the air pressure within the conduit 705 and pressure chamber increases the actuation switch plunger 718 to move against the biasing force of the spring 719 until the conductive bridge 721 is separated from the conductor ends 726 , thereby opening the circuit and de-energizing the electric motor 707 .
To fire a projectile from the air gun the operator actuates trigger 712 thereby releasing the pressurized air within the conduit 705 , which thereby actuates the release valve 702 , as previously described. This release of air pressure causes the pressure sensitive release valve plunger 718 to move with the biasing force of the spring 719 , thereby returning the conductive bridge 721 into contact with the conductor ends 726 and once again establishing a closed circuit with the electric motor 707 . The closing of the circuit re-energizes the electric motor 707 so as to actuate the air pump to automatically repressurizes the pressure chamber 701 .
It thus should be understood that the just described air gun automatically repressurizes the pressure chamber with each firing of the gun. As such, an operator does not have to actuate a manual air pump or remember to actuate a pump with each firing of the gun.
With reference next to FIG. 35, there is shown an air gun 800 in another embodiment similar to that shown in FIG. 34 . Here however a pressure tank 801 has been added in order to provide a large supply of pressurized air. Additionally, this gun 800 has been provided with a magazine 802 and indexer/pulsator 803 as previously described herein. In operation, the pressure sensitive actuation switch 804 energizes the motorized air pump 80 G when the air pressure within the pressure tank 801 or conduit falls within a minimal range of air pressures.
It should be understood that the gun may also be utilized to fire a pulse of water, and thus the gun may be referred to as a fluid gun. In order to do so the pressure tank 801 is filled with water which is then pressurized through the passage of compressed air from the air pump into the pressure tank.
With reference next to FIG. 36, there is shown an air gun 900 in another preferred embodiment. Here, the gun 900 is essentially the same as that previously described with reference to FIG. 34 except for the form of the pressure sensitive actuation switch 901 . Here the actuation switch 901 is in the form of a pressure transducer 902 coupled to the conduit between the air pump and the pressure chamber. The pressure transducer 902 is electrically coupled to a conventional control circuit 903 which control the activation of the electric motor upon the sensing of a select pressure range.
It should be understood that other types of pressure sensitive or pressure monitoring devices may be utilized to sense the pressure within the system and actuate the electric motor accordingly. Also, it should be understood that energizing the electric motor within a select range of pressure is the equivalence of de-energizing the electric motor within a range of pressures outside a select range of pressures. It should also be understood that other types of conventional mechanical release valves and triggers may be utilized as a substitute for those described herein.
While this invention has been described in detail with particular reference to the preferred embodiments thereof, it should be understood that many modifications, additions and deletions, in addition to those expressly recited, may be made thereto without departure from the spirit and scope of invention as set forth in the following claims. | A fluid gun ( 700 ) is disclosed having an electric pump ( 704 ) for conveying air to a pressure chamber ( 701 ) having a release valve ( 702 ) for controlling the release of fluid. The activation of the electric pump is controlled by a pressure sensitive actuation switch ( 713 ) which senses the pressure within the pressure chamber and activates the pump when the sensed pressure falls within a minimal range. | 5 |
BACKGROUND
[0001] Today, power is generated from a number of different sources, including renewable and non-renewable resources. Generally speaking, power output by renewable resources varies greatly depending upon weather conditions. For example, power output from solar cells is dependent upon the amount of sunlight, and power output from wind turbines is dependent upon the amount/strength of wind. Therefore, power utility entities often rely on other forms of power generators to supplement the renewable resource generators. For example, the power utility entities may utilize natural gas generators or other generators that can rapidly increase production to generate power when the power output from solar cells and/or wind turbines is insufficient to meet demand.
[0002] Moreover, power generators that utilize non-renewable resources, such as coal and/or nuclear power plants, are typically not able to adjust output rapidly in response to changes in demand (e.g., it may take a day or more to ramp up or ramp down production). Therefore, power utility entities forecast the amount of energy that will be demanded and adjust production to meet that forecast. At times when the forecast does not align with actual demand, power utility entities may be forced to take other actions. For example, when demand is greater than supply, power utility entities may utilize power generators (e.g., less efficient peaker type of generators) that can more rapidly increase production (e.g., often at a much higher cost per kWh), and when supply is greater than demand, power utility entities may decrease the cost of power to consumers (e.g., and sometimes even pay consumers) to encourage consumers to utilize more power (e.g., reducing the load on the power grid).
[0003] Thus, because electricity demands fluctuate (e.g., hourly and/or daily), it is difficult for power utility entities to match supply with demand. When supply is insufficient to meet demand, power utility entities may utilize plants that are able to ramp up production rapidly to increase supply (e.g., which are often more expensive to operate and/or are inefficient). When supply is greater than depend, power utility entities provide incentives to consumers to increase power consumption until supply is substantially aligned with demand.
SUMMARY
[0004] This Summary is provided to introduce a selection of concepts in a simplified form that are further described below in the Detailed Description. This Summary is not intended to identify key factors or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter.
[0005] Among other things, one or more systems and/or techniques for regulating the amount of power on a power grid via a datacenter(s) (e.g., a server farm) are provided. A communication channel is established between power utility entity(s) and the datacenter(s) through which information/data can be transmitted. For example, the power utility entity may provide the datacenter with information indicative of power consumption on the power grid (e.g., information indicative of power supply and demand). Based at least in part upon such information, the datacenter may be configured to adjust an amount of power consumed by the datacenter. That is, the datacenter can throttle up and/or throttle down power consumption based at least in part upon the information provided by the power utility entity. For example, when there is an excess supply on the power grid (e.g., when supply is greater than demand by a specified threshold), the datacenter may be configured to increase power consumption to bring demand closer to supply (e.g. reducing excess supply). Conversely, when there is a short supply of power, the datacenter may be configured to reduce power consumption (e.g., and/or go off the grid) until demand is more closely aligned with supply.
[0006] It will be appreciated that there are numerous ways that a datacenter can throttle up or throttle down power consumption. For example, one or more processes can be turned off, turned on, and/or transferred to another datacenter (e.g., where there is an excess demand of power on the power grid turn off processes and/or transfer processes to another data center) to adjust the amount of power being consumed by one or more servers of the datacenter. Moreover, when there is excess supply, power consumption code can be executed in a virtualized environment on one or more servers to increase consumption (e.g., execution of the code would increase the consumption of energy). It will be appreciated that these techniques and/or other techniques described throughout the disclosure are merely example techniques and are not intended to be interpreted in a limiting manner.
[0007] Regulating the amount of power on a power grid via a datacenter(s) has numerous advantages. For example, in exchange for regulating power, the datacenter may be able to negotiate energy rates that are different than (e.g., lower than) market rates and/or take advantage of periods when power utility entities pay consumers to use energy (e.g., reducing overall energy costs of the datacenter). Moreover, power supply on a power grid may be more stable (e.g., reducing the need for costly peak generators and/or reducing an excess supply of power on the grid). Also, tempering peaks in demand on the grid allows a buffer for the grid to be reduced (e.g., normal operation or utilization of the grid may be held closer to the maximum capacity for the grid, because the peaks have been tempered).
[0008] To the accomplishment of the foregoing and related ends, the following description and annexed drawings set forth certain illustrative aspects and implementations. These are indicative of but a few of the various ways in which one or more aspects may be employed. Other aspects, advantages, and novel features of the disclosure will become apparent from the following detailed description when considered in conjunction with the annexed drawings.
DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is an exemplary system for regulating power on a power grid via a datacenter.
[0010] FIG. 2 is an exemplary system illustrating example components of a datacenter configured to regulate power on a power grid.
[0011] FIG. 3 is an exemplary method for regulating power on a power grid.
[0012] FIG. 4 is an exemplary method for establishing an energy rate for a datacenter.
[0013] FIG. 5 is an illustration of an exemplary computer-readable medium wherein processor-executable instructions configured to embody one or more of the provisions set forth herein may be comprised.
[0014] FIG. 6 illustrates an exemplary computing environment wherein one or more of the provisions set forth herein may be implemented.
DETAILED DESCRIPTION
[0015] The claimed subject matter is now described with reference to the drawings, wherein like reference numerals are generally used to refer to like elements throughout. In the following description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the claimed subject matter. It may be evident, however, that the claimed subject matter may be practiced without these specific details. In other instances, structures and devices are illustrated in block diagram form in order to facilitate describing the claimed subject matter.
[0016] Traditionally, datacenters have been relatively large, but substantially constant, loads on a power grid. That is, datacenters typically consume a large amount of power (e.g., relative to most other consumers on the grid) because of the amount of energy utilized to power servers and/or to cool the servers. However, datacenters are typically still small enough that they do not substantially impact market movements (e.g., they typically do not, by themselves, cause a significant spike or drop in demand).
[0017] Among other things, one or more systems and/or techniques for regulating the amount of power on a power grid via a datacenter(s) (e.g., a server farm) are provided. A communication channel may be established between a power utility entity(ies) and the datacenter(s) through which information/data can be transmitted. For example, the power utility entity may provide the datacenter with information indicative of power consumption on the power grid (e.g., information indicative of power supply and demand). Based at least in part upon such information, the datacenter may be configured to adjust an amount of power consumed by the datacenter. It will be appreciated that the term datacenter is used herein in a broad sense to describe one or more structures that comprises servers or other devices for processing data. Such structures could be spread out over a vast geographic area (e.g., such as a campus environment, and/or across different areas serviced by the grid, etc.) and/or the servers may be comprised in merely a single structure.
[0018] Stated differently, one or more systems and/or techniques are provided for utilizing a datacenter to smooth a supply of electricity on a power grid such that the supply of electricity substantially matches the demand for electricity (e.g., within an desired/specified range). In this way, power supply may be at least partially regulated by a datacenter as opposed to a power utility entity that may have higher cost associated with regulating power supply. Moreover, because the burden of regulating power supply may be at least partially transferred to the datacenter, the datacenter may establish an energy rate(s) that is more favorable to the datacenter relative to market rates, for example.
[0019] It will be appreciated that, given the technology involved, the operations performed, etc. by datacenters, datacenters are in a unique position for regulating power relative to other power consumers (e.g., particularly large power consumers that may be able to effect changes in supply by increasing/decreasing demand). For example, a datacenter may be able to adjust power consumption from 100 kW to 100 MW in a matter of minutes based at least in part upon information regarding power consumption on the power grid, whereas other power consumers (e.g., such as automobile manufacturing plants, steel manufacturing plants, etc.) may not be able to adjust power consumption to a similar degree (e.g., and/or may be able to do so merely at a cost that makes such changes undesirable) and/or adjust power consumption as quickly as a datacenter.
[0020] FIG. 1 provides an example power regulation system 100 for regulating an amount of power on a power grid 104 via a datacenter 106 . That is, FIG. 1 illustrates a datacenter 106 configured to adjust power consumption based at least in part upon power consumption information provided to the datacenter 106 from a power utility entity 102 (e.g., responsible for managing power on the power grid 104 ). In this way, the datacenter 106 can throttle up (e.g., increase) power consumption when the power grid 104 has an excess supply of power (e.g., supply exceeds demand by a predetermined threshold) and/or throttle down (e.g., decrease) power consumption when the power grid 104 has a short supply of power (e.g., demand exceeds supply and/or supply exceeds demand by less than a predetermined threshold (e.g., a cushion)).
[0021] It will be appreciated that the example power regulation system 100 may replace and/or be used in conjunction with traditional power regulation techniques. For example, when there is an increased demand for power (e.g., above what is forecasted and therefore can be produced by low cost energy generators (e.g., such as coal and/or nuclear plants)), the datacenter 106 may be configured to reduce power consumption to drop demand. However, if the datacenter 106 is unable to reduce demand sufficiently to meet supply, one or more peak generators (e.g., power generators that can rapidly ramp up or down power output) may be utilized to provide more power to the power grid 104 .
[0022] The example power regulation system 100 comprises the power utility entity 102 and the datacenter 106 . The power utility entity 102 (e.g., which may be a power generator and/or merely an entity that monitors an amount of power on the power grid 104 ) is configured to generate information indicative of power consumption on the power grid 104 . Generally speaking, the generated information is configured to provide the datacenter 106 with enough information to determine whether to increase or decrease power consumption. For example, in one embodiment, the generated information may be indicative of real-time (e.g., present) information regarding power supplied to the power grid 104 and/or power demands by other consumers 108 and/or may be indicative of forecasting information related to future supply and/or demand on the power grid 104 . In another embodiment, the generated information may be indicative of an amount of change the power utility entity desires the datacenter 106 to make in its power consumption. For example, the generated information may comprise a request for the datacenter 106 to increase power consumption by 10 MW.
[0023] It will be appreciated that the phrase “information indicative of power consumption on a power grid” is intended to be interpreted in a broad sense to include information such as specified in the aforementioned examples and/or other types of information that could be provided to a datacenter 106 to provide guidance to the datacenter 106 on whether to increase and/or decrease power consumption (e.g., to regulate an amount of power on the power grid 104 ). Thus, the generated information may or may not comprise actual power consumption readouts (e.g., how much power is available on the power grid 104 and/or how much power is being consumed by other consumers 108 ), but rather may, in some embodiments, indicate to the datacenter 106 a desired change in power consumption by the datacenter 106 , for example.
[0024] The datacenter 106 is configured to receive the generated information from the power utility entity 102 . For example, the datacenter 106 may be configured to receive the information indicative of the present supply and present demand of power on the power grid 104 and/or forecasted future supply and demand of power on the power grid 104 . Based at least in part upon such information, the datacenter 106 may be configured to calculate how much power the datacenter 106 should consume from the power grid 104 (e.g., to bring the supply within a specified range of demand). Alternatively, the generated information may be indicative of how much power the datacenter 106 should consume, so the datacenter 106 may not have to make such a calculation.
[0025] The datacenter 106 is also configured to adjust the amount of power consumed by the datacenter 106 from the power grid 104 based at least in part upon the received information from the power utility entity 102 . Stated differently, in response to the information received from the power utility entity 102 , the datacenter 106 may throttle up and/or throttle down power consumption to increase the demand for power from the power grid 104 (e.g., when there is an excess supply of power) and/or to decrease demand for power from the power grid 104 (e.g., when there is a short supply of power).
[0026] It will be appreciated that there are numerous techniques for adjusting power consumption by a datacenter, some of which are described in more detail with respect to FIG. 2 . However, generally speaking, such an adjustment in power consumption generally utilizes the capabilities of one or more servers 110 , 112 , and/or 114 , etc. of the datacenter 106 . For example, the datacenter 106 may reduce power consumption by decreasing (e.g., to zero) the workload of one or more of the servers 110 , 112 , 114 and/or may increase power consumption by increasing the workload of one or more of the servers 110 , 112 , and 114 . Other techniques for adjusting the amount of power consumed by the datacenter 106 from the power grid 104 (e.g., which may not involve adjusting the workload of one or more of the servers 110 , 112 , and/or 114 ) include, among other things, utilizing a power generator(s) at the datacenter 106 to supplement power supplied to the datacenter 106 via the power grid 104 and/or adjusting power supplied to non-critical portions of the datacenter 106 (e.g., turning off lights and/or cooling apparatuses in areas of the datacenter 106 where such features are not required).
[0027] While the minimum and maximum amount of power that is capable of being consumed by a datacenter 106 may depend upon numerous factors (e.g., such as the size of the datacenter 106 , the functions of the datacenter 106 , and/or amount of redundancy between the datacenter 106 and other datacenters), generally speaking, the datacenter 106 can be configured adjust power consumption by about 100 MW or more in one embodiment. For example, the datacenter 106 may be able to operate at power levels in the range of 100 kW and 100 MW. Thus, the datacenter 106 may be able to influence (e.g. to a more significant degree than other power consumers 108 ) demand for power from the power grid 104 (e.g., to bring demand within a reasonable level of supply). Moreover, because the datacenter 106 is typically configured to adjust power consumption by adjusting the loads on one or more of the servers 110 , 112 , 114 (e.g., which can occur quickly), it will be appreciated that adjustments in power consumption can be performed relatively quickly (e.g., in real-time as supply and/or demand on the power grid 104 changes). For example, in a matter of minutes, the datacenter 106 may be able to adjust power consumption from 100 kW to 100 MW and/or vice-versa, for example.
[0028] FIG. 2 illustrates example components of a datacenter 200 (e.g., 106 in FIG. 1 ) that may be configured to adjust an amount of power consumed by the datacenter 200 from a power grid (e.g., 104 in FIG. 1 ). In this way, the datacenter may regulate a demand for power. For example, when there is a low supply of power on the power grid, the datacenter 200 may be configured to reduce power consumption from the power grid to decrease demand (e.g., until demand is within a specified range of supply) and/or when there is an excess supply of power on the power grid, the datacenter 200 may be configured to increase power consumption from the power grid to increase demand (e.g., bringing demand within the specified range of supply) (e.g., and using excess supply).
[0029] The example datacenter 200 comprises a power monitor component 204 configured to receive information from a power utility entity (e.g., 102 in FIG. 1 ) indicative of power consumption and/or availability on the power grid. For example, in one embodiment, the power monitor component 204 may be configured to receive information indicative of a present supply and/or a present demand on the power grid. Based at least in part upon such information, the datacenter may be configured to calculate how much power the datacenter 106 should consume from the power grid 104 (e.g., to bring the supply within a specified range of demand). In yet another embodiment, the power monitor component 204 may receive information indicative of future supply and/or forecasted, future demand for power from the power grid, and the power monitor component 204 may perform a similar calculation based at least in part upon the information regarding future power consumption. Alternatively, the power monitor component 204 may receive information indicative of how much power the datacenter 200 should consume, so the power monitor component 204 may not have to perform calculations regarding power consumption, for example.
[0030] The calculated and/or received information may be transmitted from the power monitor component 204 to a power management component 206 configured to control power consumption by the datacenter 200 (e.g. including power consumption by one or more servers 110 , 112 , 114 in FIG. 1 , for example). In one embodiment, the power management component 206 may also be configured to monitor an amount of power consumed by the datacenter and/or monitor an amount of power supplied to the datacenter from the power grid. Based at least in part upon the information transmitted to the power management component 206 from the power monitor component 204 and/or based at least in part upon current power consumption of the datacenter 200 , the power management component 206 may be configured to adjust an amount of power consumed by the datacenter 200 and/or an amount of power supplied by the power grid to the datacenter 200 .
[0031] It will be appreciated that there are numerous ways to control power consumption by a datacenter and/or to control an amount of power that the datacenter consumes from a power grid. Thus, there are numerous ways the power management component 206 may control power consumption of power supplied from the power grid. For example, in one embodiment, the power management component 206 may be configured to power up and/or power down generators (e.g., natural gas generators, diesel generators, etc.) at the datacenter 200 that are configured to supplement and/or replace power supplied by the power grid. By way of example, when the demand for power increases to within a specified threshold of supply and/or exceeds supply (e.g. as indicated in the information supplied to the power management component 206 from the power monitor component 204 ), the power management component 206 may be configured to increase (indigenous) power production by generators at the datacenter 200 (e.g., to take the datacenter 200 off the grid and/or reduce an amount of power pulled from the grid by the datacenter 200 ). Once demand drops and/or supply increases, the power management component 206 may be configured to decrease power production by the generators at the datacenter 200 to increase an amount of power consumed by the datacenter 200 from the power grid.
[0032] The power management component 206 may also be configured to adjust power consumption utilizing one or more servers (e.g., 110 , 112 , 114 in FIG. 1 ) of the datacenter 200 . By way of example, in one embodiment, the power management component 206 is configured to adjust power consumption of the datacenter 200 by adjusting a workload of one or more servers. For example, if power consumption is to be adjusted downward, the power management component 206 may request that one or more servers turn off processes that the power management component 206 deems to be of low priority (e.g., non-critical task) and/or may request that one or more processes (e.g., loads) be transferred from a server(s) in the datacenter 200 to a server(s) in another datacenter (e.g., located in a region where there is excess power on the power grid). Conversely, if power consumption is to be adjusted upward, the power management component 206 may request that one or more servers turn on additional processes (e.g., causing the one or more servers to consume additional power) and/or may request a transference of processes from one or more servers located in another datacenter to one or more servers in the datacenter 200 . Moreover where one or more servers (e.g., portions of the datacenter 200 ) merely perform non-critical tasks (e.g., routine updates, diagnostics, backups, etc.), for example, the power management component may be configured to power on and/or power off those portions of the datacenter 200 to adjust power consumption by the datacenter.
[0033] As yet another example, one or more of the servers may be configured to host a virtualized environment, and the virtualized environment may be configured to execute power consumption code. For example, when the power monitor component 204 indicates to increase power consumption, the power management component 206 may be configured to issue a request to one or more servers configured to host virtualized environments to start the virtualized environments and/or execute the power consumption code. Such code may be configured to increase processor tasks and/or spin storage devices to convert electricity into heat energy, for example. When the power monitor component 204 indicates to decrease power consumption, the power management component 206 may issue another request to turn off the virtualized environments and/or stop executing the power consumption code. It will be appreciated that the aforementioned techniques for adjusting power consumption by the datacenter are merely example techniques and are not intended to be interpreted in a limiting manner. That is, other techniques besides those described herein for adjusting power consumption by the power management component 206 are also contemplated herein.
[0034] In the illustrated embodiment, the example datacenter 200 further comprises a scheduler 202 . The scheduler 202 is configured to identify processing jobs (e.g., non-critical tasks) and to schedule one of more of processing jobs to be performed by the datacenter when the received information is indicative of an excess supply of power on the grid. In one example, using a schedule(s) developed by the scheduler 202 , the power management component 206 may be configured to adjust power consumption by the datacenter 200 . By way of example, the scheduler 202 may be configured to arrange processing jobs according to a degree of power increase. When power consumption is to be increased by 100 kW, the power management component 206 may issue a request to one or more servers to execute a first set of processes (e.g., as dictated by a first schedule generated by the scheduler 202 ), and when power consumption is to be increased by 30 MW, the power management component 206 may be configured to issue a request that one or more servers execute a second set of processes (e.g., also dictated by a second schedule generated by the scheduler 202 ). Thus, the scheduler 202 may generate one or more schedules indicative of which processing jobs may be performed at different power consumption levels/ranges, and the power management component 206 may utilize the one or more schedules when determining how to increase and/or decrease power consumption, for example.
[0035] As another example, the scheduler 202 may be configured to determine power consumption by one or more processes and/or one or more servers prior to receiving a request to increase or decrease power consumption from the power grid (e.g., creating a benchmark(s) for power consumption). For example, in one embodiment, it may be determined that the average process consumes 5 kW of power and/or that the average server (e.g., or rack of servers) consume 30 kW of power. Based upon such a determination, the power management component 206 may determine the number of processes and/or servers that could be utilized (e.g., turned on or turned off or up or down, etc.) to achieve a desired increase or reduction in power consumption. As an example, if power consumption from the power grid is to be reduced by 300 kW and the average process consumes 5 kW, the power management component 206 may determine that 60 processes are required to be turned off and may proceed with shutting down processes according to some predetermined criteria (e.g., in order from least critical to most critical). Once such processes have been shut down, the power management component 206 (e.g., and/or the power monitor component 204 ) may verify that power consumption by the datacenter from the power grid has been reduced as specified, for example. If, during the verification, it is determined that power consumption needs to be further adjusted (e.g., too many processes were turned off and/or too few processes were turned off), the power management component 206 may proceed with further adjusting the number of processes and/or servers operating accordingly. It will be appreciated that the numbers listed herein are merely intended to be examples and do not necessarily reflect actual figures that may be achieved in practical implementations. For example, in practical implementations respective processes may merely draw 1 kW or less of power.
[0036] The example datacenter 200 further comprises a datacenter communication component 208 configured to provide the power utility entity with information related to power consumption by the datacenter 200 . For example, the datacenter communication component 208 may be configured to receive information from the power management component 206 indicative of current power consumption levels and/or indicative of current throttling capacity (e.g., indicative of a maximum and/or a minimum amount of power that can be consumed by the datacenter 200 at a given time). For example, the throttling capacity of the datacenter 200 may fluctuate from time to time (e.g., non-critical task may become critical and/or load may be shifted to the datacenter from another datacenter because of scheduled maintenance at the other datacenter, etc.), and such information may be provided to the power utility entity via the datacenter communication component 208 (e.g., so that the power utility entity has knowledge regarding the extent to which the datacenter 200 can bring demand into alignment with supply). In another embodiment, the datacenter communication component 208 may be configured to provide the power utility entity with information regarding expected future demand of the datacenter 200 . For example, if the datacenter 200 has been operating for a period of time at a low power level (e.g., to reduce demand on the power grid because of high demand from other power consumers), the datacenter 200 may provide the power utility entity with a notice providing that the datacenter 200 may increase power consumption within a day to perform processes that have been on hold (e.g., such as reporting processes) while the datacenter 200 has been operating at the low power level.
[0037] It will be appreciated that by receiving power consumption information from the power utility entity (e.g., indicative of power supply and/or demand on the power grid) and/or providing to the power utility entity information regarding power consumption by the datacenter 200 , a feedback loop may be created whereby the power utility entity and the datacenter 200 may work cooperatively to regulate the amount of power on the power grid (e.g., to regulate supply and demand such that supply substantially matches demand (e.g., within a specified tolerance)). It will be appreciated that such cooperation may be mutually beneficial. For example, the datacenter 200 may benefit by negotiating rates with the power utility entity that are different than (e.g., reduced from) market rates and/or by taking advantage of instances where excess supply causes the power utility entity to provide incentives to entities that can increase power consumption (e.g. such as negative pricing, where the power utility entity pays an entity to consume power). The power utility entity may benefit because the datacenter 200 may regulate demand (e.g., to better align with supply), so that the amount of power on the power grid is substantially constant (e.g., to promote a consistent energy rate). Moreover, the power utility entity may utilize the datacenter 200 to control demand rather than and/or to supplement the use of peak generators (e.g., which may be costly to run and/or inefficient) to control supply.
[0038] Moreover, it will be appreciated that in one embodiment, the communications between the power utility entity and the datacenter 200 may be at least partially and/or fully automatic. By way of example, the power utility entity may identify a build-up in supply and/or a drop in supply and automatically notify the datacenter 200 to increase or decrease supply accordingly. Further, in one embodiment, the adjustment of power consumption from the power grid by the datacenter 200 may be performed automatically (e.g., with or without human intervention). For example, if the power utility entity forwards a request to reduce power consumption by 300 kW, the power management component 206 may determine how the datacenter 200 can reduce consumption by 300 kW and proceed to automatically perform necessary actions to achieve such reductions.
[0039] FIG. 3 illustrates an example method 300 for regulating power on a grid via a datacenter. That is, the example method 300 provides for adjusting power demand on the power grid using a datacenter (e.g., which may be configured to operate on as little power as 100 kW and/or as much power as 100 MW, for example) based at least in part upon power consumption information indicative of overall power consumption on the power grid (e.g., information regarding current (e.g., present) power supply and/or demand). In this way, an amount of power on a grid may be regulated by a datacenter (e.g., which adjusts demand) as opposed to and/or in conjunction with a power utility entity (e.g., which may adjust supply using one or more peak generators).
[0040] The example method 300 beings at 302 and information is received from the power utility entity indicative of power consumption on the power grid at 304 . For example, the received information may be representative of a current supply of power on the power grid and/or representative of a current demand of power from the power grid. In another embodiment, the received information may comprise a request for the datacenter to adjust an amount of power it consumes from the power grid. For example, the received information may comprise a request from the datacenter to increase power consumption and/or decrease power consumption by 10 MW. It will be appreciated that the received information may also and/or instead be indicative of a forecasted (e.g., predicted) future demand and/or supply from power from the power grid. In this way, the datacenter may plan accordingly with respect to power consumption (e.g., plan to increase processes and/or decrease process based at least in part upon future predictions), for example.
[0041] At 306 in the example method 300 , an amount of power consumed by the datacenter from the power grid may be adjusted based at least in part upon received information indicative of power consumption on the power grid. That is, stated differently, the datacenter may be configured to adjust an amount of power it acquires from the grid based at least in part upon the received information. In this way, the datacenter may regulate the demand for power from the power supply. By way of example, when the received information indicates that supply exceeds demand by a predetermined threshold, the datacenter may be configured to increase the amount of power consumed by the datacenter from the power grid to increase demand (e.g., bringing demand closer to supply). Conversely, when the received information indicates that demand exceeds supply and/or that demand is edging too close to supply (e.g., such that little to no reserve remains on the power grid), the datacenter may be configured to decrease the amount of power consumed by the datacenter from the power grid to decrease demand (e.g., causing demand to decrease below supply by a predetermined threshold). In this way, the power available on the power grid may substantially parallel demand (e.g., to reduce energy rate spikes caused by excess demand and/or energy rate drops caused by excess supply).
[0042] It will be appreciated that there are numerous ways to adjust the amount of power consumed by the datacenter from the power grid. For example, in one embodiment, the datacenter may comprise one or more (back-up) generators that may be throttled up to reduce the demand of the datacenter on the power grid and/or may be throttled down to increase demand of the datacenter on the power grid. Such a technique may find particular applicability in situations where power consumption to servers cannot be reduced to a level that causes the datacenter to drop power demand on the grid to a satisfactory level and/or in situations where it may be undesirable to reduce overall power consumption by the datacenter, for example. In another embodiment, the datacenter may adjust the amount of power consumed by adjusting power distribution within the datacenter. By way of example, the datacenter may comprise one or more portions that can be powered down or powered up to decrease or increase power consumption, respectively. For example, in one embodiment, the datacenter may increase power supplied to cooling units for one or more portions of the datacenter to increase power consumption (e.g., causing the one or more portions of the datacenter to drop in temperature by 1-2 degrees) and/or may decrease power supplied to cooling units for one or more portions of the datacenter to decrease power consumption (e.g., causing the one or more portions of the datacenter to increase in temperature by 1-2 degrees). Thus, the amount of power consumed by the datacenter may be adjusted by adjusting an amount of power generated by the datacenter and/or by adjusting power supplied to components that are merely indirectly related to the functions of the datacenter (e.g., processing data), such as adjusting power supplied to lighting units and/or to cooling units).
[0043] As described with respect to FIGS. 1-2 , the amount of power consumed by the datacenter from the power grid may also and/or instead be adjusted by adjusting the amount of power consumed by one or more servers of the datacenter. For example, the workload of one or more servers may be increased and/or decreased to adjust power consumption. As an example, non-critical and/or low priority tasks and/or processes may be stopped to reduce power consumption and/or may be started to increase power consumption. As yet another example, the workload of one or more servers of the datacenter (e.g., and thus workload of the datacenter) may be transferred to one or more servers of a second datacenter (e.g., in a different geographic region than the datacenter) (e.g., using workload/application prioritization techniques) to decrease power consumption of the one or more servers in the datacenter, and/or the workload of one or more servers at the second datacenter may be transferred to one or more servers in the datacenter to increase power consumption of the one or more servers in the datacenter.
[0044] In another embodiment, power consumption by one or more servers (e.g., and thus the datacenter) may be adjusted utilizing one or more virtual environments hosted on one or more servers. For example, one or more virtual environments may be configured to execute power consumption code (e.g., configured to increase processing and/or spin storage devices) when it is desirable to increase power consumption by one or more servers of the datacenter based at least in part upon the received information. In this way, code executed that is configured to cause electrical energy to be converted into heat energy (e.g., with few to no processing benefits). Conversely, when it is desirable to decrease power consumption based at least in part upon the received information, the one or more servers may be configured to stop the execution of power consumption code (e.g., and shutdown the virtual environment(s)).
[0045] In yet another embodiment, one or more processing jobs may be scheduled to be performed by the datacenter and/or servers thereof based at least in part upon the amount of power that is to be consumed. By way of example, critical task and/or processes of the datacenter may be scheduled to be performed regardless of the desired power consumption level and/or range (e.g., unless the datacenter is to be completely shutdown), a first set of non-critical tasks and/or processes may be scheduled to be performed when the desired power consumption level exceeds a first level (e.g., 300 kW), a second set of non-critical tasks and/or processes may be scheduled to be performed when the desired power consumption level exceeds a second level (e.g., 1 MW), etc. That is, stated differently, it may be determined how much power one or more processes and/or one or more servers consume (e.g., to develop benchmarks), and based upon such information, different scenarios may be developed that specify which processes and/or which servers are to be operational at different power consumption levels. Thus, one or more schedules may be devised for indicating which processes to execute (or not) when power consumption is desired to be at a given level, for example.
[0046] It will be appreciated that based at least in part upon these schedules the amount of power may be increased and/or decreased. For example, when is it desirable to increase consumption to 1 MW, the second set of non-critical tasks and/or processes (e.g., which may also include the critical tasks/processes and/or the first set of non-critical tasks/processes) may be performed, and when it is desired to decrease consumption to 400 kW, merely the first set of non-critical tasks and/or processes (e.g., which may also include the critical tasks/processes) may be performed.
[0047] At 308 in the example method 300 , information is provided to the power utility entity from the datacenter. Such information may be indicative current power consumption by the datacenter (e.g., and/or current power consumption from the power grid by the datacenter) and/or current throttling capacity of the datacenter (e.g. indicative of a minimum and/or a maximum amount of power that can be presently consumed by the datacenter), given the critical loads of the datacenter and/or the present ability to stop and/or transfer workloads to a different datacenter, for example. That is, throttling capacity may change over the course of a day, week, etc., and such information may be provided to the power utility entity to better determine whether to increase and/or decrease supply (e.g., utilizing peak generators).
[0048] In another embodiment, the provided information may be indicative of future power demands of the datacenter and/or future throttling capacity. For example, status reports related to the health of one or more servers of the datacenter may not have been generated within the past 6 days, so such status reports may be required to be generated within the next 2 days. As such, the datacenter may report to the power utility entity that the datacenter will increase power consumption from the grid in the next day (e.g., allowing the power utility entity to ramp up production of power via lower cost generators that take longer ramp up). As another example, the datacenter may have scheduled maintenance that is to begin in a couple days, and the datacenter may report a reduction in throttling capacity to the power utility entity (e.g., because one or more servers will be powered down and thus unable to increase power consumption). In this way, the power utility entity may be provided information that can be utilized by the power utility entity to better forecast necessary supply and/or to prepare itself for the responsibility of (self)adjusting supply (e.g., as opposed to the datacenter adjusting demand).
[0049] The example method 300 ends at 310 .
[0050] It will be appreciated that the example method 300 is merely intended to provide an example technique for regulating power on a power grid via a datacenter and is not intended by be construed in a limiting manner. Moreover, the order of the acts described in the example method 300 is merely intended to be an example order. For example, information may be provided to the power utility entity before and/or after information is received from the power utility entity.
[0051] It will be appreciated that because at least some of the burden of regulating power on the power grid is transferred from a power utility entity to a datacenter, an energy rate may be established for the datacenter that is different than market rates (e.g., and more favorable to the datacenter). FIG. 4 illustrates an example method 400 for establishing an energy rate(s) for the datacenter.
[0052] The example method 400 begins at 402 , and information is provided to the power utility entity to help the power utility entity regulate power on the grid at 404 . For example, in one embodiment, information indicative of throttling capacity of the data center may be provided to the power utility entity. That is, the datacenter may specify a minimum and/or a maximum amount of power that it can consume and/or that it is willing to consume to regulate the amount of power on the power grid (e.g., to maintain demand within a predetermined level of supply). It will be appreciated that other information can be provided to the power utility entity as well and/or instead of throttling capacity. For example, current power demand of the datacenter and/or forecasted, future power demand of the datacenter can be provided to the power utility entity. In this way, the power utility entity can better assess whether to increase and/or decrease supply, for example.
[0053] At 406 in the example method 400 , in exchange for the provided information, an energy rate is established for the datacenter. Such an energy rate may be a fixed sum (e.g., 12 cents per kWh) and/or may be a discount over current market rates (e.g., 15% off current market rates, which may fluctuate daily). Typically, the established energy rate is less than market rates because the datacenter is agreeing to assist the power utility entity with regulating the amount of power on the power grid, including consuming excess power that the datacenter may otherwise not consume, for example. However, the energy rate may be greater than current market rates. For example, the energy rate may be greater than current market rates in exchange for an agreement to lock in the rates for a specified time period (e.g., number of years).
[0054] At 408 , the example method 400 ends.
[0055] It will be appreciated that if the power utility entity is unable and/or unwilling to establish an energy rate that is desirable to the datacenter (e.g., using the example method 400 of FIG. 4 ), the datacenter may still obtain lower energy rates using the techniques and/or systems described herein. For example, the datacenter may increase power consumption when energy rates are favorable (e.g., when there is an excess supply of power on the power grid) and/or when there is negative pricing (e.g., a power utility entity is paying one or more power consumers to increase consumption), and may decrease power consumption when energy rates are unfavorable (e.g., when there is excess demand for power from the power grid).
[0056] Still another embodiment involves a computer-readable medium comprising processor-executable instructions configured to implement one or more of the techniques presented herein. An exemplary computer-readable medium that may be devised in these ways is illustrated in FIG. 5 , wherein the implementation 500 comprises a computer-readable medium 516 (e.g., a CD-R, DVD-R, or a platter of a hard disk drive), on which is encoded computer-readable data 514 . This computer-readable data 514 in turn comprises a set of computer instructions 512 configured to operate according to one or more of the principles set forth herein. In one such embodiment 500 , the processor-executable computer instructions 512 may be configured to perform a method 510 , such as at least some of the exemplary method 300 of FIG. 3 and/or 400 of FIG. 4 , for example. In another such embodiment, the processor-executable instructions 512 may be configured to implement a system, such as at least some of the exemplary system 100 of FIG. 1 and/or 200 of FIG. 2 , for example. Many such computer-readable media 516 may be devised by those of ordinary skill in the art that are configured to operate in accordance with the techniques presented herein.
[0057] Although the subject matter has been described in language specific to structural features and/or methodological acts, it is to be understood that the subject matter defined in the appended claims is not necessarily limited to the specific features or acts described above. Rather, the specific features and acts described above are disclosed as example forms of implementing the claims.
[0058] As used in this application, the terms “component,” “module,” “system”, “interface”, and the like are generally intended to refer to a computer-related entity, either hardware, a combination of hardware and software, software, or software in execution. For example, a component may be, but is not limited to being, a process running on a processor, a processor, an object, an executable, a thread of execution, a program, and/or a computer. By way of illustration, both an application running on a controller and the controller can be a component. One or more components may reside within a process and/or thread of execution and a component may be localized on one computer and/or distributed between two or more computers.
[0059] Furthermore, the claimed subject matter may be implemented as a method, apparatus, or article of manufacture using standard programming and/or engineering techniques to produce software, firmware, hardware, or any combination thereof to control a computer to implement the disclosed subject matter. The term “article of manufacture” as used herein is intended to encompass a computer program accessible from any computer-readable device, carrier, or media. Of course, those skilled in the art will recognize many modifications may be made to this configuration without departing from the scope or spirit of the claimed subject matter.
[0060] FIG. 6 and the following discussion provide a brief, general description of a suitable computing environment to implement embodiments of one or more of the provisions set forth herein. The operating environment of FIG. 6 is only one example of a suitable operating environment and is not intended to suggest any limitation as to the scope of use or functionality of the operating environment. Example computing devices include, but are not limited to, personal computers, server computers, hand-held or laptop devices, mobile devices (such as mobile phones, Personal Digital Assistants (PDAs), media players, and the like), multiprocessor systems, consumer electronics, mini computers, mainframe computers, distributed computing environments that include any of the above systems or devices, and the like.
[0061] Although not required, embodiments are described in the general context of “computer readable instructions” being executed by one or more computing devices. Computer readable instructions may be distributed via computer readable media (discussed below). Computer readable instructions may be implemented as program modules, such as functions, objects, Application Programming Interfaces (APIs), data structures, and the like, that perform particular tasks or implement particular abstract data types. Typically, the functionality of the computer readable instructions may be combined or distributed as desired in various environments.
[0062] FIG. 6 illustrates an example of a system 610 comprising a computing device 612 configured to implement one or more embodiments provided herein. In one configuration, computing device 612 includes at least one processing unit 616 and memory 618 . Depending on the exact configuration and type of computing device, memory 618 may be volatile (such as RAM, for example), non-volatile (such as ROM, flash memory, etc., for example), or some combination of the two. This configuration is illustrated in FIG. 6 by dashed line 614 .
[0063] In other embodiments, device 612 may include additional features and/or functionality. For example, device 612 may also include additional storage (e.g., removable and/or non-removable) including, but not limited to, magnetic storage, optical storage, and the like. Such additional storage is illustrated in FIG. 6 by storage 620 . In one embodiment, computer readable instructions to implement one or more embodiments provided herein may be in storage 620 . Storage 620 may also store other computer readable instructions to implement an operating system, an application program, and the like. Computer readable instructions may be loaded in memory 618 for execution by processing unit 616 , for example.
[0064] The term “computer readable media” as used herein includes computer storage media. Computer storage media includes volatile and nonvolatile, removable and non-removable media implemented in any method or technology for storage of information such as computer readable instructions or other data. Memory 618 and storage 620 are examples of computer storage media. Computer storage media includes, but is not limited to, RAM, ROM, EEPROM, flash memory or other memory technology, CD-ROM, Digital Versatile Disks (DVDs) or other optical storage, magnetic cassettes, magnetic tape, magnetic disk storage or other magnetic storage devices, or any other medium which can be used to store the desired information and which can be accessed by device 612 . Any such computer storage media may be part of device 612 .
[0065] Device 612 may also include communication connection(s) 626 that allows device 612 to communicate with other devices. Communication connection(s) 626 may include, but is not limited to, a modem, a Network Interface Card (NIC), an integrated network interface, a radio frequency transmitter/receiver, an infrared port, a USB connection, or other interfaces for connecting computing device 612 to other computing devices. Communication connection(s) 626 may include a wired connection or a wireless connection. Communication connection(s) 626 may transmit and/or receive communication media.
[0066] The term “computer readable media” may include communication media. Communication media typically embodies computer readable instructions or other data in a “modulated data signal” such as a carrier wave or other transport mechanism and includes any information delivery media. The term “modulated data signal” may include a signal that has one or more of its characteristics set or changed in such a manner as to encode information in the signal.
[0067] Device 612 may include input device(s) 624 such as keyboard, mouse, pen, voice input device, touch input device, infrared cameras, video input devices, and/or any other input device. Output device(s) 622 such as one or more displays, speakers, printers, and/or any other output device may also be included in device 612 . Input device(s) 624 and output device(s) 622 may be connected to device 612 via a wired connection, wireless connection, or any combination thereof. In one embodiment, an input device or an output device from another computing device may be used as input device(s) 624 or output device(s) 622 for computing device 612 .
[0068] Components of computing device 612 may be connected by various interconnects, such as a bus. Such interconnects may include a Peripheral Component Interconnect (PCI), such as PCI Express, a Universal Serial Bus (USB), firewire (IEEE 1394), an optical bus structure, and the like. In another embodiment, components of computing device 612 may be interconnected by a network. For example, memory 618 may be comprised of multiple physical memory units located in different physical locations interconnected by a network.
[0069] Those skilled in the art will realize that storage devices utilized to store computer readable instructions may be distributed across a network. For example, a computing device 630 accessible via a network 628 may store computer readable instructions to implement one or more embodiments provided herein. Computing device 612 may access computing device 630 and download a part or all of the computer readable instructions for execution. Alternatively, computing device 612 may download pieces of the computer readable instructions, as needed, or some instructions may be executed at computing device 612 and some at computing device 630 .
[0070] Various operations of embodiments are provided herein. In one embodiment, one or more of the operations described may constitute computer readable instructions stored on one or more computer readable media, which if executed by a computing device, will cause the computing device to perform the operations described. The order in which some or all of the operations are described should not be construed as to imply that these operations are necessarily order dependent. Alternative ordering will be appreciated by one skilled in the art having the benefit of this description. Further, it will be understood that not all operations are necessarily present in each embodiment provided herein.
[0071] Moreover, the word “exemplary” is used herein to mean serving as an example, instance, or illustration. Any aspect or design described herein as “exemplary” is not necessarily to be construed as advantageous over other aspects or designs. Rather, use of the word exemplary is intended to present concepts in a concrete fashion. As used in this application, the term “or” is intended to mean an inclusive “or” rather than an exclusive “or”. That is, unless specified otherwise, or clear from context, “X employs A or B” is intended to mean any of the natural inclusive permutations. That is, if X employs A; X employs B; or X employs both A and B, then “X employs A or B” is satisfied under any of the foregoing instances. In addition, the articles “a” and “an” as used in this application and the appended claims may generally be construed to mean “one or more” unless specified otherwise or clear from context to be directed to a singular form. Also, at least one of A and B or the like generally means A or B or both A and B.
[0072] Although the disclosure has been shown and described with respect to one or more implementations, equivalent alterations and modifications will occur to others skilled in the art based at least in part upon a reading and understanding of this specification and the annexed drawings. The disclosure includes all such modifications and alterations and is limited only by the scope of the following claims. In particular regard to the various functions performed by the above described components (e.g., elements, resources, etc.), the terms used to describe such components are intended to correspond, unless otherwise indicated, to any component which performs the specified function of the described component (e.g., that is functionally equivalent), even though not structurally equivalent to the disclosed structure which performs the function in the herein illustrated exemplary implementations of the disclosure. In addition, while a particular feature of the disclosure may have been disclosed with respect to only one of several implementations, such feature may be combined with one or more other features of the other implementations as may be desired and advantageous for any given or particular application. Furthermore, to the extent that the terms “includes”, “having”, “has”, “with”, or variants thereof are used in either the detailed description or the claims, such terms are intended to be inclusive in a manner similar to the term “comprising.” | One or more techniques and/or systems are provided for regulating an amount of power on a power grid using a datacenter. This allows demand to be more closely brought into alignment with supply. For example, when supply exceeds demand by a predetermined level, the datacenter may increase consumption, causing demand to increase, and when demand exceeds supply and/or comes within a predetermined threshold of supply, the datacenter may decrease consumption, causing demand to decrease. In this way, the datacenter can be utilized as a regulatory tool on the grid. It may be appreciated that given the technology used by and/or operations performed by datacenters, datacenters are uniquely situated to achieve these ends as compared to other (large) energy consumers, such as manufacturing facilities that cannot shift around and/or shut-down operations swiftly. | 8 |
[0001] This application is a continuation of U.S. patent application Ser. No. 10/924,398, filed Aug. 23, 2004, which is a continuation of U.S. patent application Ser. No. 10/446,314, filed May 28, 2003, now U.S. Pat. No. 6,782,359, which is a continuation of U.S. patent application Ser. No. 10/083,237, filed Feb. 26, 2002, now U.S. Pat. No. 6,611,799, which is a continuation of U.S. patent application Ser. No. 09/805,634, filed Mar. 14, 2001, now U.S. Pat. No. 6,385,577, which is a continuation of U.S. patent application Ser. No. 09/441,743, filed Nov. 16, 1999, now U.S. Pat. No. 6,223,152, which is a continuation of U.S. patent application Ser. No. 08/950,658, filed Oct. 15, 1997, now U.S. Pat. No. 6,006,174, which is a continuation of U.S. patent application Ser. No. 08/670,986, filed Jun. 28, 1996, which is a continuation of U.S. patent application Ser. No. 08/104,174, filed Aug. 9, 1993, which is a continuation of U.S. patent application Ser. No. 07/592,330, filed Oct. 3, 1990, now U.S. Pat. No. 5,235,670, which applications are incorporated herein by reference.
BACKGROUND
[0002] This invention relates to digital voice coders performing at relatively low voice rates but maintaining high voice quality. In particular, it relates to improved multipulse linear predictive voice coders.
[0003] The multipulse coder incorporates the linear predictive all-pole filter (LPC filter). The basic function of a multipulse coder is finding a suitable excitation pattern for the LPC all-pole filter which produces an output that closely matches the original speech waveform. The excitation signal is a series of weighted impulses. The weight values and impulse locations are found in a systematic manner. The selection of a weight and location of an excitation impulse is obtained by minimizing an error criterion between the all-pole filter output and the original speech signal. Some multipulse coders incorporate a perceptual weighting filter in the error criterion function. This filter serves to frequency weight the error which in essence allows more error in the format regions of the speech signal and less in low energy portions of the spectrum. Incorporation of pitch filters improve the performance, of multipulse speech coders. This is done by modeling the long term redundancy of the speech signal thereby allowing the excitation signal to account for the pitch related properties of the signal.
SUMMARY
[0004] The present invention is a synthetic speech encoding device that produces a synthetic speech signal which closely matches an actual speech signal. The actual speech signal is digitized, and excitation pulses are selected by minimizing the error between the actual and synthetic speech signals. The preferred pattern of excitation pulses needed to produce the synthetic speech signal is obtained by using an excitation pattern containing a multiplicity of weighted pulses at timed positions. The selection of the location and amplitude of each excitation pulse is obtained by minimizing an error criterion between the synthetic speech signal and the actual speech signal. The error criterion function incorporates a perceptual weighting filter which shapes the error spectrum.
BRIEF DESCRIPTION OF THE DRAWING(S)
[0005] FIG. 1 is a block diagram of an 8 kbps multipulse LPC speech coder.
[0006] FIG. 2 is a block diagram of a sample/hold and A/D circuit used in the system of FIG. 1 .
[0007] FIG. 3 is a block diagram of the spectral whitening circuit of FIG. 1 .
[0008] FIG. 4 is a block diagram of the perceptual speech weighting circuit of FIG. 1 .
[0009] FIG. 5 is a block diagram of the reflection coefficient quantization circuit of FIG. 1 .
[0010] FIG. 6 is a block diagram of the LPC interpolation/weighting circuit of FIG. 1 .
[0011] FIG. 7 is a flow chart diagram of the pitch analysis block of FIG. 1 .
[0012] FIG. 8 is a flow chart diagram of the multipulse analysis block of FIG. 1 .
[0013] FIG. 9 is a block diagram of the impulse response generator of FIG. 1 .
[0014] FIG. 10 is a block diagram of the perceptual synthesizer circuit of FIG. 1 .
[0015] FIG. 11 is a block diagram of the ringdown generator circuit of FIG. 1 .
[0016] FIG. 12 is a diagrammatic view of the factorial tables address storage used in the system of FIG. 1 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0017] This invention incorporates improvements to the prior art of multipulse coders, specifically, a new type LPC spectral quantization, pitch filter implementation, incorporation of pitch synthesis filter in the multipulse analysis, and excitation encoding/decoding.
[0018] Shown in FIG. 1 is a block diagram of an 8 kbps multipulse LPC speech coder, generally designated 10 .
[0019] It comprises a pre-emphasis block 12 to receive the speech signals s(n). The pre-emphasized signals are applied to an LPC analysis block 14 as well as to a spectral whitening block 16 and to a perceptually weighted speech block 18 .
[0020] The output of the block 14 is applied to a reflection coefficient quantization and LPC conversion block 20 , whose output is applied both to the bit packing block 22 and to an LPC interpolation/weighting block 24 .
[0021] The output from block 20 to block 24 is indicated at α and the outputs from block 24 are indicated at α , α 1 and at αρ, α 1 ρ.
[0022] The signal α , α 1 is applied to the spectral whitening block 16 and the signal αρ, α 1 ρ is applied to the impulse generation block 26 .
[0023] The output of spectral whitening block 16 is applied to the pitch analysis block 28 whose output is applied to quantizer block 30 . The quantized output {circumflex over (p)} from quantizer 30 is applied to the bit packer 22 and also as a second input to the impulse response generation block 26 . The output of block 26 , indicated at h(n), is applied to the multiple analysis block 32 .
[0024] The perceptual weighting block 18 receives both outputs from block 24 and its output, indicated at Sp(n), is applied to an adder 34 which also receives the output r(n) from a ringdown generator 36 . The ringdown component r(n) is a fixed signal due to the contributions of the previous frames. The output x(n) of the adder 34 is applied as a second input to the multipulse analysis block 32 . The two outputs Ê and Ĝ of the multipulse analysis block 32 are fed to the bit packing block 22 .
[0025] The signals α , α 1 , p and Ê, Ĝ are fed to the perceptual synthesizer block 38 whose output y(n), comprising the combined weighted reflection coefficients, quantized spectral coefficients and multipulse analysis signals of previous frames, is applied to the block delay N/2 40 . The output of block 40 is applied to the ringdown generator 36 .
[0026] The output of the block 22 is fed to the synthesizer/postfilter 42 .
[0027] The operation of the aforesaid system is described as follows: The original speech is digitized using sample/hold and AID circuitry 44 comprising a sample and hold block 46 and an analog to digital block 48 . ( FIG. 2 ). The sampling rate is 8 kHz. The digitized speech signal, s(n), is analyzed on a block basis, meaning that before analysis can begin, N samples of s(n) must be acquired. Once a block of speech samples s(n) is acquired, it is passed to the preemphasis filter 12 which has a z-transform function
P ( z )=1−α* z −1 (1)
[0028] It is then passed to the LPC analysis block 14 from which the signal K is fed to the reflection coefficient quantizer and LPC converter whitening block 20 , (shown in detail in FIG. 3 ). The LPC analysis block 14 produces LPC reflection coefficients which are related to the all-pole filter coefficients. The reflection coefficients are then quantized in block 20 in the manner shown in detail in FIG. 5 wherein two sets of quantizer tables are previously stored. One set has been designed using training databases based on voiced speech, while the other has been designed using unvoiced speech. The reflection coefficients are quantized twice; once using the voiced quantizer 48 and once using the unvoiced quantizer 50 . Each quantized set of reflection coefficients is converted to its respective spectral coefficients, as at 52 and 54 , which, in turn, enables the computation of the log-spectral distance between the unquantized spectrum and the quantized spectrum. The set of quantized reflection coefficients which produces the smaller log-spectral distance shown at 56 , is then retained. The retained reflection coefficient parameters are encoded for transmission and also converted to the corresponding all-pole LPC filter coefficients in block 58 .
[0029] Following the reflection quantization and LPC coefficient conversion, the LPC filter parameters are interpolated using the scheme described herein. As previously discussed, LPC analysis is performed on speech of block length N which corresponds to N/8000 seconds (sampling rate=8000 Hz). Therefore, a set of filter coefficients is generated for every N samples of speech or every N/8000 sec.
[0030] In order to enhance spectral trajectory tracking, the LPC filter parameters are interpolated on a sub-frame basis at block 24 where the sub-frame rate is twice the frame rate. The interpolation scheme is implemented (as shown in detail in FIG. 6 ) as follows: let the LPC filter coefficients for frame k−1 be α 0 and for frame k be α 1 . The filter coefficients for the first sub-frame of frame k is then
α =( α 0 + α 1 )/2 (2)
and α 1 parameters are applied to the second sub-frame. Therefore a different set of LPC filter parameters are available every 0.5*(N/8000) sec.
[0031] Pitch Analysis
[0032] Prior methods of pitch filter implementation for multipulse LPC coders have focused on closed loop pitch analysis methods (U.S. Pat. No. 4,701,954). However, such closed loop methods are computationally expensive. In the present invention the pitch analysis procedure indicated by block 28 , is performed in an open loop manner on the speech spectral residual signal. Open loop methods have reduced computational requirements. The spectral residual signal is generated using the inverse LPC filter which can be represented in the z-transform domain as A(z); A(z)=1/H(z) where H(z) is the LPC all-pole filter. This is known as spectral whitening and is represented by block 16 . This block 16 is shown in detail in FIG. 3 . The spectral whitening process removes the short-time sample correlation which in turn enhances pitch analysis.
[0033] A flow chart diagram of the pitch analysis block 28 of FIG. 1 is shown in FIG. 7 . The first step in the pitch analysis process is the collection of N samples of the spectral residual signal. This spectral residual signal is obtained from the pre-emphasized speech signal by the method illustrated in FIG. 3 . These residual samples are appended to the prior K retained residual samples to form a segment, r(n), where −K≦n≦N
[0034] The autocorrelation Q(i) is performed for τ 1 ≦i≦τ h or
Q ( i ) = n = - K N ∑ r ( n ) r ( n - i ) τ 1 ≤ i ≤ τ h ( 3 )
[0035] The limits of i are arbitrary but for speech sounds a typical range is between 20 and 147 (assuming 8 kHz sampling). The next step is to search Q(i) for the max value, M 1 , where
M 1 =max( Q ( i ))= Q ( k 1 ) (4)
[0036] The value k is stored and Q(k 1 −1), Q(k 1 ) and Q(K 1 +1) are set to a large negative value.
[0037] We next find a second value M 2 where
M 2 =max( Q ( i ))= Q ( k 2 ) (5)
[0038] The values k 1 and k 2 correspond to delay values that produce the two largest correlation values. The values k 1 and k 2 are used to check for pitch period doubling. The following algorithm is employed: If the ABS(k 2 −2*k 1 )<C, where C can be chosen to be equal to the number of taps (3 in this invention), then the delay value, D, is equal to k 2 otherwise D=k 1 . Once the frame delay value, D, is chosen the 3-tap gain terms are solved by first computing the matrix and vector values in eq. (6).
[ ∑ r ( i ) r ( n - τ - 1 ) ∑ r ( n ) r ( n - i ) ∑ r ( n ) r ( n - i + 1 ) ] = [ ∑ r ( n - i - 1 ) r ( n - i - 1 ) ∑ r ( n - i ) r ( n - i - 1 ) ∑ r ( n - i - 1 ) r ( n - i - 1 ) ∑ r ( n - i - 1 ) r ( n - i ) ∑ r ( n - i ) r ( n - i ) ∑ r ( n - i + 1 ) r ( n - i ) ∑ r ( n - i - 1 ) r ( n - i + 1 ) ∑ r ( n - i ) r ( n - i + 1 ) ∑ r ( n - i + 1 ) r ( n - i + 1 ) ] ( 6 )
[0039] The matrix is solved using the Cholesky matrix decomposition. Once the gain values are calculated, they are quantized using a 32 word vector codebook. The codebook index along with the frame delay parameter are transmitted. The {circumflex over (P)} signifies the quantized delay value and index of the gain codebook.
[0040] Excitation Analysis
[0041] Multipulse's name stems from the operation of exciting a vocal tract model with multiple impulses. A location and amplitude of an excitation pulse is chosen by minimizing the mean-squared error between the real and synthetic speech signals. This system incorporates the perceptual weighting filter 18 . A detailed flow chart of the multipulse analysis is shown in FIG. 8 . The method of determining a pulse location and amplitude is accomplished in a systematic manner. The basic algorithm can be described as follows: let h(n) be the system impulse response of the pitch analysis filter and the LPC analysis filter in cascade; the synthetic speech is the system's response to the multipulse excitation. This is indicated as the excitation convolved with the system response or
s ^ ( n ) = ∑ k = 1 n ex ( k ) h ( n - k ) ( 7 )
where ex(n) is a set of weighted impulses located at positions n 1 ,n 2 , . . . n j or
ex ( n )=β 1 δ( n−n 1 )+β 2 δ( n−n 2 )+ . . . +β j δ( n−n j ) (8)
[0042] The synthetic speech can be re-written as
s ^ ( n ) = ∑ j = 1 j β j h ( n - n j ) ( 9 )
[0043] In the present invention, the excitation pulse search is performed one pulse at a time, therefore j=1. The error between the real and synthetic speech is
e ( n )= s p ( n )−{circumflex over ( s )}( n )− r ( n ) (10)
[0044] The squared error
E = ∑ n = 1 N ⅇ 2 ( n )
or ( 11 ) E = ∑ n = 1 N ( s p ( n ) - s ^ ( n ) - r ( n ) ) 2 ( 12 )
where s p (n) is the original speech after pre-emphasis and perceptual weighting ( FIG. 4 ) and r(n) is a fixed signal component due to the previous frames' contributions and is referred to as the ringdown component.
[0045] FIGS. 10 and 11 show the manner in which this signal is generated, FIG. 10 illustrating the perceptual synthesizer 38 and FIG. 11 illustrating the ringdown generator 36 . The squared error is now written as
E = ∑ n = 1 N ( x ( n ) - β 1 h ( n - n j ) 2 ( 13 )
where x(n) is the speech signal s p (n)−r(n) as shown in FIG. 1 .
E = S - 2 BC + B 2 H
where ( 14 ) C = ∑ n = 1 N - 1 x ( n ) h ( n - n j )
and ( 15 ) S = ∑ n = 1 N - 1 x 2 ( n )
and ( 16 ) H = ∑ n = 1 N - 1 h ( n - n 1 h ( n - n 1 ) ( 17 )
[0046] The error, E, is minimized by setting the dE/dB= 0 or
dE/dB=− 2 C+ 2 HB= 0 (18)
or
B=C/H (19)
[0047] The error, E, can then be written as
E=S−C 2 /H (20)
[0048] From the above equations it is evident that two signals are required for multipulse analysis, namely h(n) and x(n). These two signals are input to the multipulse analysis block 32 .
[0049] The first step in excitation analysis is to generate the system impulse response. The system impulse response is the concatenation of the 3-tap pitch synthesis filter and the LPC weighted filter. The impulse response filter has the z-transform:
H p ( z ) = 1 1 - ∑ i = 1 3 b i z - τ - i 1 1 - ∑ τ = 1 ρ α i μ i z - i ( 20 )
[0050] The b values are the pitch gain coefficients, the α values are the spectral filter coefficients, and μ is a filter weighting coefficient. The error signal, e(n), can be written in the z-transform domain as
E ( z )= X ( z )− BH p ( z ) z −n1 (21)
where X(z) is the z-transform of x(n) previously defined.
[0051] The impulse response weight β, and impulse response time shift location n 1 are computed by minimizing the energy of the error signal, e(n). The time shift variable n 1 (1=1 for first pulse) is now varied from 1 to N. The value of n 1 is chosen such that it produces the smallest energy error E. Once n 1 is found β 1 can be calculated. Once the first location, n 1 and impulse weight, β 1 , are determined the synthetic signal is written as
ŝ ( n )=β 1 h ( n−n 1 ) (22)
[0052] When two weighted impulses are considered in the excitation sequence, the error energy can be written as
E =Σ( x ( n )−β 1 h ( n−n 1 )−β 2 h ( n−n 2 )) 2
[0053] Since the first pulse weight and location are known, the equation is rewritten as
E =Σ( x ′( n )−β 2 h ( n−n 2 )) 2 (23)
where
x ′( n )= x ( n )−β 1 h ( n−n 2 ) (24)
[0054] The procedure for determining β 2 and n 2 is identical to that of determining β 1 and n 1 . This procedure can be repeated p times. In the present instance p=5. The excitation pulse locations are encoded using an enumerative encoding scheme.
[0055] Excitation Encoding
[0056] A normal encoding scheme for 5 pulse locations would take 5*Int(log 2 N+0.5), where N is the number of possible locations. For p=5 and N=80, 35 bits are required. The approach taken here is to employ an enumerative encoding scheme. For the same conditions, the number of bits required is 25 bits. The first step is to order the pulse locations (i.e. 0L1≦L2≦L3≦L4≦L5≦N−1 where L1=min(n 1 , n 2 , n 3 , n 4 , n 5 ) etc.). The 25 bit number, B, is:
B = ( L1 1 ) + ( L2 2 ) + ( L3 3 ) + ( L4 4 ) + ( L5 5 )
[0057] Computing the 5 sets of factorials is prohibitive on a DSP device, therefore the approach taken here is to pre-compute the values and store them on a DSP ROM. This is shown in FIG. 12 . Many of the numbers require double precision (32 bits). A quick calculation yields a required storage (for N=80) of 790 words ((N−1)*2*5). This amount of storage can be reduced by first realizing
( L 1 1 )
is simply L1; therefore no storage is required. Secondly,
( L 2 2 )
contains only single precision numbers; therefore storage can be reduced to 553 words. The code is written such that the five addresses are computed from the pulse locations starting with the 5th location (Assumes pulse location range from 1 to 80). The address of the 5th pulse is 2*L5+393. The factor of 2 is due to double precision storage of L5's elements. The address of L4 is 2*L4+235, for L3, 2*L3+77, for L2, L2−1. The numbers stored at these locations are added and a 25-bit number representing the unique set of locations is produced. A block diagram of the enumerative encoding schemes is listed.
[0058] Excitation Decoding
[0059] Decoding the 25-bit word at the receiver involves repeated subtractions. For example, given B is the 25-bit word, the 5th location is found by finding the value X such that
B - ⋮ ( 79 5 ) < 0
B - ( X 5 ) < 0
B - ( X - 1 5 ) > 0
then L5=x−1. Next let
B = B - ( L 5 5 )
[0060] The fourth pulse location is found by finding a value X such that
B - ( L 5 - 1 4 ) < 0
⋮
B - ( X 4 ) < 0
B - ( X - 1 4 ) > 0
then L4=X−1. This is repeated for L3 and L2. The remaining number is L1. | The present invention is a synthetic speech encoding device that produces a synthetic speech signal which closely matches an actual speech signal. The actual speech signal is digitized, and excitation pulses are selected by minimizing the error between the actual and synthetic speech signals. The preferred pattern of excitation pulses needed to produce the synthetic speech signal is obtained by using an excitation pattern containing a multiplicity of weighted pulses at timed positions. The selection of the location and amplitude of each excitation pulse is obtained by minimizing an error criterion between the synthetic speech signal and the actual speech signal. The error criterion function incorporates a perceptual weighting filter which shapes the error spectrum. | 6 |
TECHNICAL FIELD
This invention relates to ground anchors for use in anchoring posts, poles and the like uprightly upon the ground, and to methods of performing such operations.
BACKGROUND OF THE INVENTION
Ground or earth anchors have heretofore been devised for use in anchoring structures firmly to the ground. Exemplary of such are those shown in U.S. Pat. Nos. 3,969,853, 4,280,768, 4,593,872 and 4,653,245. Some ground anchors are designed to be manually embedded into the soil while others are designed to be mechanically embedded by the use of power tools known as anchor drivers. The present invention is directed to a ground or earth anchor of the latter type for the support of posts uprightly upon the surface of the ground.
As shown in the just mentioned patents, those ground anchors that are used to support large structures have themselves had to be of relatively large, complex and rugqedized construction in order to accommodate the large forces necessary to embed the anchors deeply and to provide sufficient anchoring power once embedded. Conversely, ground anchors that have been devised for supporting smaller structures such as fence posts, guard rails, tent posts and the like have been relatively simple, lightweight and usually designed for manual installation. Heretofore, it has generally been thought that ground anchors for posts have had to be of the manual embedding type to render them economically feasible.
The present invention has for a principal object the provision of a ground anchor for use in supporting posts uprightly upon the surface of the ground which is of relatively simple and economic construction and yet which is adapted to be readily installed with the use of power tools. With its use the labor involved in digging post holes or in manually embedding an anchor may be reduced or even eliminated. Its use also eliminates the need for the use of concrete in forming an in situ anchor about the post and thus also serves to eliminate the waiting period for concrete to set in order to complete installation.
SUMMARY OF THE INVENTION
In one form of the invention a ground anchor for anchoring a post comprises an elongated prop adapted to be driven by rotary drive means and to which an end of a post to be supported may be telescopically mounted for vertical support. A spike extends from an end of the prop that bears a shoulder of a width greater than the width of the spike. A bit is mounted adjacent an end of the spike located distally from the prop. A platform is provided which is configured to be mounted about the spike in abutment with the post shoulder.
In another form of the invention a ground anchor for anchoring a post comprises a cylindrical prop to which a bottom end portion of a post may be telescopically mounted. A cylindrical spike is mounted coaxially to an end of the cylindrical prop with the spike having a diameter less than the diameter of the prop whereby a radial step is formed adjacent the junction of the prop and spike. A platform is also provided which is adapted to be mounted about the spike beneath the step. A bit is mounted to an end of the spike located distally from the step.
In yet another form of the invention a method of anchoring a post uprightly upon the ground comprises the step of driving an anchor partially into the ground of a type that has a relatively thin lower portion adapted to be embedded and a relatively thick upper portion adapted to be telescopically mounted to a bottom of the post. A stabilizing platform is placed about the anchor lower portion adjacent its junction with the anchor upper portion. The anchor is then driven further into the ground so as to cause the platform to become sandwiched snuggly and securely between a lower end of the anchor upper end portion and the surface of the ground. The post is then mounted upon the anchor and platform.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a side elevational view of a ground anchor embodying principles of the invention.
FIG. 2 is a plan view of the ground anchor illustrated in FIG. 1 shown together with a post or pole mounted thereon.
FIG. 3 is a cross-sectional view of an adapter for use with the ground anchor illustrated in FIG. 1.
FIG. 4 is a side elevational view of the ground anchor illustrated in FIG. 1 together with another adapter thereto.
FIG. 5 is a perspective view of the adapter shown in FIG. 4.
DETAILED DESCRIPTION
With reference next to FIGS. 1 and 2, there is shown a ground or earth anchor 10 which has a cylindrical, tubular support or prop 11 provided with a hole 12 in a side thereof to receive the pin of a conventional motorized anchor driver. A disc-shaped plate 13 is welded coaxially to the bottom of the tubular prop 11. A cylindrical spike 15 is in turn welded to the other side of the plate 13 so as to extend coaxially from the prop 11. The end of the spike located distally from the prop is formed with a beveled tip 16. A helical bit or auger fluke 17 is mounted to the spike adjacent the tip 16.
The ground anchor also includes a structurally independent platform 18 which, as can best be seen from FIG. 2, is in the form of a square plate. Each of the four corners of the plate are downturned to form four spade-like prongs 19. The plate is also formed with a slot 20 which extends from one of its sides to and somewhat past the plate center. This slot is sized to receive the spike 15 so that it may be placed about it.
A hollow post or pole P may be mounted uprightly upon the surface of the ground G by means of the just described anchor in the following manner. In this case the post is of a tubular configuration, such as a conventional tennis fence post. The anchor tip is first forced into the ground with the anchor oriented uprightly so as to bring the bit into contact with the surface. An anchor driver is then coupled with the prop 11 by inserting its rotatable drive arm into the upper end of the prop and extending its locking pin laterally through the hole 12 to secure it to the prop. The anchor driver is then operated which causes the anchor to rotate. With some downward pressure applied, as by the weight of the driver, the helical bit 17 forces the spike 15 down into the ground as the prop and spike are rotated. This action is continued until the spike has been driven into the ground approximately to the position shown in FIG. 1.
Next the platform 18 is placed about the spike, as shown in FIG. 1, with its prongs 19 in contact with the ground. The anchor driver is further operated which causes the spike and prop to be driven further downwardly bringing the plate 13, which forms a step or shoulder at the junction of the prop and spike, into contact with the top of the platform 18. Further operation of the anchor driver causes the ground anchor to be driven still further downward thereby causing the prongs 19 of the platform , which is not being rotated, to become embedded in the surface of the ground and to bring the remainder of the platform into flush engagement with the surface of the ground G. The anchor driver is then uncoupled and removed from the prop 11 leaving the anchor firmly embedded in the ground with its prop projecting upwardly therefrom and with the platform providing a high degree of stability positioned flushly atop the ground. The tubular fence post P is then telescoped upon the prop and brought to rest upon plate 13 with its inside positioned closely about the prop.
A ground anchor of the same size as that just described may also be used to support a larger post or pole than post P by the use of the adapter shown in FIG. 3. The adapter 25 here is comprised of a cylindrical tube or pipe 26 which has a pair of rings 27 welded to its interior adjacent its ends 28. So constructed, the adapter 25 may be slid upon the prop 11 after the ground anchor has been embedded. A larger pipe may then be telescoped over the adapter to provide a close fit for stable ground support.
The ground anchor illustrated in FIG. 1 may also be used to support square shaped rather than cylindrically shaped posts by the use of the other adapter 30 illustrated in FIGS. 4 and 5. This adapter is of U-shaped construction formed from a strip of metal that is bent into this shape to form two parallel leg portions 31 joined by a bight portion 32. The bight portion is formed with a slot 33 which is sized to receive the spike 15. In use, the adapter 30 is placed upon the platform 18 beneath the plate 13 just before the platform is finally driven into place upon the surface of the ground G, as shown in FIG. 4. With a channel having been drilled into the bottom of a wooden post P', the post is telescoped upon the prop 11 between the legs 31 of the adapter 30 thereby becoming mounted uprightly and secured upon the ground anchor and the ground.
It thus is seen that a ground anchor of very simple and economic construction is provided which may be readily embedded in the ground for use. Though the posts or poles illustrated in the drawing have been telescoped about the anchor prop, it should be understood that the telescopic arrangement may be reversed with the posts being mounted inside of the prop. Though the prop has been shown to be cylindrical here, such is not essential. Nor is the use of the plate 13 since the bottom of the prop itself may provide a step or shoulder for the platform to abut. Thus, the plate essentially serves to widen the shoulder for enhanced stability and to facilitate welding of the spike to the prop during anchor manufacture. Though steel is preferred as the material for all of the anchor components, other metals could be used instead. And though the anchor is designed to be driven with a powered driver, it could be manually driven.
Thus, it should be understood that many modifications, additions and deletions may be made to the specific embodiments illustrated, other than those just expressly suggested, without departure from the spirit and scope of the invention as set forth in the following claims. | A ground anchor has a spike with bit mounted coaxially to a prop of greater width than the spike. A structurally independent platform is provided to be placed about the spike and butted against the prop as the spike is rotatably driven into the ground. | 4 |
FIELD OF THE INVENTION
The present invention relates to the game of lawn darts and in particular to a safety lawn dart having a deformable nose section to prevent injury to the players and to bystanders.
BACKGROUND OF THE INVENTION
Lawn darts have provided outdoor entertainment to adults and children for many years. Existing lawn darts typically comprise a pointed tip, a shaft and a tail section. The tip of the traditional lawn dart is sufficiently pointed to penetrate the ground upon landing. Associated with the traditional lawn dart, however, is the ever-present threat of accidental injury to the players and to bystanders. In recent years, severe injuries have been reported resulting from the use of traditional lawn darts. The majority of these injuries have been puncture wounds to children caused by the tip of the flying lawn dart. Sufficient concern has been expressed regarding the safety of the traditional lawn dart, that legislation has been passed restricting the use of such darts.
The present invention is designed not to penetrate the ground and includes a nose section which will not penetrate human skin under normal use. The present invention is also advantageous in that it may be used indoors.
SUMMARY OF THE INVENTION
The safety lawn dart of the present invention is designed to be used in the same manner as the traditional lawn dart. The safety lawn dart is grasped by the tail section or, in another embodiment, by the distal end of the dart shaft, and is thrown towards the target. The center of gravity of the safety lawn dart is located nearer the nose section than the distal end of the dart shaft, ensuring that the nose section makes first contact with the target upon landing.
The nose section is generally bulbous in shape and deformable to avoid penetration of the target and of skin and to deaden and minimize the bounce of the dart upon impact with the target. In one embodiment, the intermediate section of the safety lawn dart is telescopic and retracts upon landing to further reduce the propensity of the dart to bounce upon landing.
The tail section of the safety dart provides aerodynamic stability during flight. The tail section may be fixably or slideably and rotatably mounted on the dart shaft. In the slideable and rotatable embodiment, the tail section is disposed forwardly and exposes the distal end of the dart shaft to be grasped by the player when throwing of the dart. During flight, the tail section shifts toward the distal end of the dart shaft to provide enhanced aerodynamic stability.
In another embodiment of the present invention, a further aerodynamic surface is peripherally mounted on the intermediate section to increase aerodynamic stability during flight. In addition, after the dart has landed, this aerodynamic surface maintains the dart shaft in an elevated position to facilitate the players' identification of the location of the dart.
DESCRIPTION OF THE DRAWINGS
The present invention will be more fully understood from the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 illustrates a first embodiment of the present invention;
FIG. 2 illustrates a second embodiment of the present invention;
FIG. 3 illustrates an end view of the tail section of the Present invention;
FIG. 4 illustrates a third embodiment of the present invention;
FIG. 5 is a front end view of the peripheral aerodynamic surface of the present invention, and
FIG. 6 illustrates the characteristics of the present invention during use.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to FIG. 1, a first embodiment of the safety dart 8 of the present invention is illustrated. In this embodiment, nose section 10 is substantially semi-spherical in shape. Nose section 10 is manufactured of a deformable material, such as latex rubber, which deforms on impact with the target, typically the ground. Nose section 10 comprises a substantially hollow member 11. The thickness of nose section wall 12 is sufficient, when the material from which nose section 10 is manufactured is taken into consideration, to permit the nose section 10 to deform on impact with the target. In addition, nose section 10 partially or fully contains bounce retarding particulate matter 14 such as sand or plastic chips. This material increases the deadening effect of the deformable nose section 10 upon impact with the target.
Connected to nose section 10 is an intermediate section 16. Intermediate section 16 has a substantially cylindrical shape although other shapes may be used without materially affecting the aerodynamic parameters of the safety dart. Extending from intermediate section 16 is an elongated shaft 18. Mounted on shaft 18 is a tail section 20 which has at least one aerodynamic surface 22. Nose section 20 may be affixed to intermediate section 16 by gluing, bonding or by other means known to those of ordinary skill in the art. Intermediate section 16, shaft 18 and tail section 20 may be integrally formed or, alternatively, may be manufactured separately and connected together by bonding, tacking or by other means known to those of ordinary skill in the art.
Referring now to FIG. 2, another embodiment of the safety dart of the present invention is illustrated. In this embodiment, intermediate section 16 comprises a first telescoping member 26 and second telescoping member 28. Second telescoping member 28 is connected to shaft 30 and is dimensioned to receive first telescoping member 26 in sliding telescopic engagement. First telescoping member 26 is connected to nose section 10. Upon impact with the target, nose section 10 deforms as described above and first telescoping member 26 retracts into second telescoping member 28, thus absorbing the shock of impact and reducing the propensity of the dart to bounce.
Tail section 32 is slidingly and rotatably mounted on shaft 30. Retaining member 34 prevents tail section 32 from becoming detached from shaft 30. Tail section 32 comprises at least one first aerodynamic surface 36 having a swept-back leading edge 38. Referring now also to FIG. 3, tail section 32 may also include at least one second aerodynamic surface 40 associated with, and at an angle to, each first aerodynamic surface 38. Second aerodynamic surface 40 urges tail section 32 to rotate about shaft 30 during flight and increases the aerodynamic stability of the safety dart.
Of course, other tail section configurations are possible and will occur to those of ordinary skill in the art. For example, tail section 32 may include 2, or 4 or more first aerodynamic surfaces 36 each having a corresponding second aerodynamic surface 40, as shown in FIG. 3.
Referring now to FIGS. 4 and 5, another embodiment of the present invention is illustrated. In this embodiment, intermediate section 16 further comprises a peripherally mounted aerodynamic surface 50. Peripheral aerodynamic surface 50 comprises a leading edge 52 and a trailing edge 54. Leading edge 52 is disposed between trailing edge 54 and nose section 56 and has a diameter smaller than the diameter of trailing edge 54. Peripheral aerodynamic surface 50 is connected to second telescoping member 28 by at least one spoke 58. When they dart is in flight, peripheral aerodynamic surface 50 contributes to the aerodynamic stability of the dart. Peripheral aerodynamic surface 50 also functions to absorb impact upon landing. After the dart has landed, and as indicated in FIG. 6, peripheral dynamic surface 50 maintains shaft 60 and tail section 62 in an elevated position, thus rendering the dart easily visible to the players even at a remote distance.
FIG. 6 illustrates the features of the embodiment of the safety dart illustrated in FIG. 4 during use. Tail section 62 is initially slid along shaft 60 towards intermediate section 16. Player 70 thereafter grasps the exposed section 71 of shaft 60 proximate retaining member 34. At this time, the force of gravity causes first telescoping member 26 to become extended from second telescoping member 28. Once in flight, tail section 74 of dart 76 slides along shaft 60 until it abuts retaining member 75. During flight, first telescoping member 26 remains extended from second telescoping member 28.
Upon impact of dart 78 with the target 80, nose section 82 is deformed and first telescoping member is forced to retract into second telescoping member 84. The combined effect of the deformation of nose section 82 and the retraction of first telescoping member into second telescoping member 28 is to cause safety dart 78 to come to rest at a position in substantially the same place at which nose section 82 first makes contact with target 80. Similarity between the game of lawn darts using the present invention and using the pointed darts of the prior art is thereby enhanced. Risk of injury to the players and bystanders from the tip of the safety dart is also virtually eliminated.
Having above indicated preferred embodiments of the present invention, it will occur to those skilled in the art that modifications and alternatives can be practiced within the spirit of the invention. It is accordingly intended to define the scope of the invention only as indicated in the following claims. | A safety lawn dart having a blunt deformable nose section. The blunt nose section is a safety feature permitting use of the lawn dart without fear of the injury associated with the use of existing lawn darts having pointed tips. A shock-absorbing telescopic intermediate section may be added to increase the deadening effect upon impact of the dart with the ground or target. A tail section is fixably or slideably and rotatably mounted on the dart shaft to promote aerodynamic stability. | 5 |
BACKGROUND OF THE INVENTION
(1) Field Of The Invention
The invention relates to a method of conveying a solid in a conveying medium ( 15 ) in which the solid is delivered to a container having an outlet ( 7 ) and the conveying medium that flows into the container generates a downwardly rotating current ( 17 ) so that the solid is delivered by the conveying medium to the outlet. More particularly the invention provides for the delivery of a solid in a conveying medium into a container having an outlet so that the downwardly rotating current provides a spiral trajectory directed sharply downward to the outlet of the container.
(2) Description of Related Art Including Information Disclosed Under 37 C.F.R. 1.97 and 1.98
It is known, for example from DE 197 55 732 C2, to transport a dispersion of granules and water through a conduit. To produce a dispersion of solid and liquid, it is known to first introduce the solid into a container filled with liquid and to mix it with the liquid using a mechanical stirrer. The mixture of solid and liquid is then drawn off from the bottom of the container. This is done using a centrifugal pump, which pumps the solid/liquid mixture from its axial inlet opening to the tangential outlet opening and into the conduit.
A disadvantage of this method is that the solid is subjected to mechanical stresses, both by the stirrer arranged in the container and by the pump, and these stresses lead to undesired attrition of the solid and/or to damage of sensitive solid particles. This method has a particularly disadvantageous effect on a solid whose specific weight is less than the specific weight of the liquid which is being used to transport the solid, because the solid of lower specific weight tends, as in a centrifuge, to accumulate at the center of the impeller of the centrifugal pump. The efficiency of the pump deteriorates as a result, because the solid has to be forced away from the center of the impeller. Moreover, the solid is subjected to particularly high mechanical stresses because the individual particles of solid which accumulate at the center of the pump rub against one another. In the container too, the solid of lower specific weight is subjected to increased stress because the mechanical stirrer forces it toward the discharge opening at the bottom counter to the lifting force.
BRIEF SUMMARY OF THE INVENTION
The object of the invention is to develop a method in which the solid is dispersed in the transport liquid and introduced into the conduit without the aid of mechanically driven parts, and which method requires minimum maintenance and in particular allows solids of lower specific weight to be conveyed hydraulically without high mechanical stresses.
Starting from the features of the method of conveying a solid in a conveying medium delivered to a container with an outlet this object is achieved, according to the invention, by the generation of a downwardly rotating current so that the solid is delivered to the outlet by the conveying medium. Advantageous and preferred developments include the method of utilizing the medium to generate the rotating current to flow tangentially as much as possible and delivering the solid through a metering device and utilizing solids of greater, lesser and equal density to the conveying medium and other objects and advantages as will become apparent to those skilled in the art.
In this method, the conveying medium, for example water, flowing into the container designed as a sender container generates a downwardly rotating current, and the solid is delivered by the conveying medium to the outlet. With the conveying medium being carried in a spiral trajectory directed sharply downward to the outlet, the solid which impinges on the conveying medium is entrained by said conveying medium and leaves the sender container together with the conveying medium and passes into a conduit. No mechanism of movement is needed in the sender container in order to produce this kind of current, and, accordingly, there is no contact causing attrition and stresses between the individual particles of the solid and moving mechanical components, for example a stirrer or an impeller of a pump.
By generating the current using a conveying medium which flows in tangentially to the greatest possible extent, it is possible to generate the current in the container without structural space being needed for this purpose in the container.
Feeding the solid into the container via a metering device allows conveying medium and solid to be exactly adapted to each other and, by this means, it is possible to obtain a ratio of liquid to solid, in the mixture of solid and liquid, which is optimum for hydraulic delivery.
In an advantageous embodiment of the subject of the invention, it is possible to convey solids whose density is less than or greater than or approximately the same as the density of the conveying medium. In this way, a very wide variety of solids can be conveyed with just one method, and the method does not have to be modified to convey a solid of different density.
By generating a current with a pumping action, the mechanical pump for maintaining the circulation of the conveying medium can be arranged at a location where it only has to convey pure conveying medium. Thus, irrespective of the solid which is to be conveyed, the pump can be optimized for conveying a specific conveying medium.
Because the conveying medium present in the sender container is driven by the conveying medium which flows anew into the sender container, the direction of rotation of the conveying medium in the sender container can be generated and maintained solely by the flow energy of the inflowing conveying medium.
The subject of the invention also proposes delivering the stream of conveying medium to an outlet along a spiral trajectory of an in particular rotationally symmetrical and in particular tapering sender container. A kind of cyclone thus develops in the container, which cyclone, in contrast to a cyclone separator, has only one outlet. In other words, the flow-generated rotation of the conveying medium in the container results in the formation of a vortex which flows off into one outlet.
In an advantageous embodiment of the subject of the invention, the sender container is designed tapering toward the outlet. The conical design of the sender container favors the formation of a flow of liquid along a narrowing spiral trajectory, because this flow of liquid is guided by the container wall.
It is advantageous if the conveying medium present as a liquid flows into the container, via a delivery nozzle, approximately parallel to the wall of the container and approximately perpendicular to a container axis. This ensures that the flow of liquid seen as a whole follows the wall of the container like an annular peripheral layer and is guided by said wall. The angle of inclination of the spiral trajectory can be influenced by the angle which the delivery nozzle forms with a plane extending perpendicular to the longitudinal axis of the container.
According to a particular embodiment of the method according to the invention, the solid, which for example can be granules of plastic, is introduced into the sender container via a star feeder. In this way, it is also possible to work using a sender container in whose interior the pressure is elevated in relation to the ambient pressure.
According to the invention, it is further provided for the solid to be delivered to the container in an area through which the conveying medium does not flow. To this end, it suffices for the container to have a simple opening through which solid is delivered.
It is particularly advantageous to deliver the solid specifically to a hollow cone which is formed by the conveying medium moving on a spiral trajectory, because the entire jacket surface of the hollow cone is available as a delivery surface for the solid and the solid is conveyed from the conical jacket surface to the outlet or to the container axis.
In a particular embodiment of the subject of the invention, the solid is delivered as a solid/liquid mixture to the conveying medium. In this way it is possible also to convey solids which are already present as a solid/liquid mixture.
In a preferred embodiment, the device according to the invention has a container which narrows toward the outlet and comprises a delivery nozzle for a liquid conveying medium, which nozzle is oriented substantially perpendicular to a main axis of the container and parallel to the container wall. With a delivery nozzle arranged in this way, it is easily possible to produce a flow of liquid running on a spiral trajectory along the container wall to the outlet.
In a further advantageous embodiment of the device, a plurality of delivery nozzles are arranged on the container wall and preferably lie in a plane perpendicular to the longitudinal axis of the container. In this way it is possible to have larger quantities of liquid flowing into the container, which quantities of liquid are guided by the container wall and combine to form a common, suctioning spiral flow.
It is also advantageous to define the profile of the current in the sender container by changing the cross section of admission. In this way, the delivery installation can be adjusted for conveying different solids.
In a modification of the invention, the level of the conveying medium in the sender container is adjusted by means of a gas pressure regulator. In this way it is possible to influence the filling level in the container and ensure that the conveying medium does not rise into the metering unit arranged above the container.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING(S)
Further details of the invention are described with reference to the drawing which shows diagrammatic views of illustrative embodiments. In the drawing:
FIG. 1 shows a diagrammatic view of an installation for hydraulic conveying,
FIG. 2 shows a diagrammatic cross section of a sender container,
FIG. 3 shows a diagrammatic cross section of a further sender container,
FIG. 4 shows a cross section, along the line IV—IV, through the sender container shown in FIG. 3 ,
FIG. 5 shows a cross section through a further sender container,
FIG. 6 shows a cross section through a sender container with an adjustable cross section of admission.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a diagrammatic view of an installation 1 for hydraulic conveying of solid 2 . The installation 1 consists principally of two reservoirs 3 which are connected to one another via a conduit 4 , one reservoir 3 being designed as the container 5 , and the other reservoir 3 being designed as a receiver container 6 . The container 5 opens into the conduit 4 via an outlet 7 . This conduit 4 opens into the receiver container 6 via an inlet 8 . The container 5 is connected to the receiver container 6 via a delivery line 9 in which motor-driven pumps 10 are arranged. An admission line 12 opening into a container lid 11 also connects the container 5 to a storage container 13 in which the solid 2 is held in readiness. The solid 2 is delivered to the container 5 via a metering device 14 . Conveying medium 15 present in the admission line 9 is conveyed with the aid of the pumps 10 in arrow direction x 1 and passed into the conveying medium 15 located in the container 5 via a nozzle 16 which is arranged tangentially with respect to the container 5 of round cross section. The introduction of the conveying medium 15 into the container 5 creates a current 17 in the latter, which current rotates about a container axis 18 to the outlet 7 , said outlet 7 being arranged in a conically tapering base 19 of the container 5 . The solid 2 which is of lower specific weight than the conveying medium 15 is shaken by the metering device 14 through a free space 20 and onto the conveying medium 15 located in the container 5 and is guided by the current 17 , as in a centrifuge, toward the container axis 18 , and drawn in arrow direction x 2 to the outlet 7 of the container 5 .
The solid 2 leaves the outlet 7 , together with the conveying medium 15 , as a solid/liquid mixture 21 which has been generated in the current 17 and passes through the conduit 4 in arrow direction X 3 . The solid/liquid mixture 21 passes through the inlet 8 into the receiver container 6 which is designed as a separator 22 . In the separator 22 , the solid/liquid mixture 21 is divided into solid 2 and conveying medium 15 . The solid 2 leaves the separator 22 by way of a pipe 23 . The conveying medium 15 passes into the delivery line 9 in which is it conveyed back to the container 5 by means of the pumps 10 and in this way moves in a conveying medium circulation 24 .
According to an alternative embodiment which is not shown, provision is made for the receiver container to be designed as a receiver/sender container, in which case the conveying medium is at least partially removed from the solid in an upper part of the container, and, in a lower part of the container, a flow of liquid is formed by inflowing conveying medium, analogously to the sender container, and the solid or the solid/liquid mixture can be pumped into a further container via this flow of liquid. Of course, the separation of the suspension and the further conveying can also take place in separate containers. Large conveying distances can thus be achieved by arranging sender and receiver containers in succession. If appropriate, intermediate reservoirs can also be provided.
FIG. 2 shows a diagrammatic cross section of a container 5 which serves as a dispersing container. A level 25 of a conveying medium 15 present in the container 5 is maintained substantially constant by a gas pressure regulator 26 . If the level 25 of the conveying medium 15 rises above a filling level H 1 , the pressure in a free space 20 of the container is then increased by means of the gas pressure regulator 26 , so that continued flow of conveying medium 15 from a delivery line 9 through a nozzle 16 into the container 5 is at least partly prevented. The free space 20 is acted upon by gas via a gas line 27 and via a control valve 28 which is assigned to the gas line 27 and is regulated by the gas pressure regulator 26 . If the level 25 of the conveying medium 15 drops below a filling level H 2 , the pressure in a free space 20 of the container 5 is then reduced by means of the gas pressure regulator 26 , so that there is less resistance to the conveying medium 15 flowing from the delivery line 9 .
FIG. 3 shows a diagrammatic cross section of a further container 5 . Arrows 29 indicate the typical profile of a current 17 generated by a conveying medium 15 passing tangentially from a delivery line 9 into the container 5 via a nozzle 16 . The conveying medium 15 flows from one container wall 30 toward a container axis 18 , at the same time moving in an arrow direction x 2 toward an outlet 7 of the container 5 . Thus, the conveying medium 15 has an axial component of velocity V A and a radial component of velocity V R . By means of the current 17 , the conveying medium 15 forms, on one surface 15 ′, a cone-shaped funnel 38 by which the solid 2 impinging on the surface 15 ′ is already guided to the container axis 18 or in the direction of the outlet 7 .
FIG. 4 shows a diagrammatic cross section of the container 5 shown in FIG. 3 , with an arrow 31 symbolizing the current 17 formed in this container 5 . The conveying medium 15 delivered via the delivery line 9 and through the nozzle 16 flows on a spiral trajectory 32 along the container wall 30 toward the outlet 7 and thus has a tangential component of velocity V T . The conveying medium 15 and the solid 2 have axial, radial and tangential components of velocity V A , V R , V T , with the velocity increasing toward the outlet 7 .
FIG. 5 shows a diagrammatic cross section of a further container 5 . In said container 5 , there are three nozzles 16 through 16 ″ which are arranged at the same height on a container wall 30 . The nozzles 16 through 16 ″ generate jets 33 through 33 ″ which run on spiral trajectories 32 through 32 ″ in the direction of a container axis 18 or spiral axis 18 ′ (indicated by an arrow end 34 ) to an outlet 7 .
FIG. 6 shows a cross section of a container 5 with a delivery line 9 which has a nozzle 16 with a variable cross section of admission A. The cross section of admission A can be adjusted by a flap 35 which can turn about a hinge 36 in arrow directions 37 . Depending on the difference in density between solid 2 and conveying medium 15 , the components of velocity V A , V R , V T can be varied by the configuration of the cross section of admission A.
The illustrative embodiments have been described on the assumption that the conveying medium used is water and that the material to be conveyed is plastic granules which are lighter than or about equally as light as water.
The invention is not limited to the illustrative embodiments shown or described. Instead, it includes developments of the invention within the scope of the patent claims. In particular, the invention also provides for solid to be conveyed which has a heavier specific weight than the conveying medium. In this case, the rotating current ensures that the solid is moving in rotation before it passes through the outlet of the container, by which means blockages are effectively counteracted.
In a further alternative embodiment which is not shown, the spiral current is formed in a pipe, preferably by guide plates, and the solid is delivered to the rotating flow of liquid by way of, for example, a conduit or a star feeder.
LIST OF REFERENCE NUMBERS
1 installation
2 solid
3 reservoir
4 conduit
5 container
6 receiver container
7 outlet
8 inlet
9 delivery line
10 pump
11 container lid
12 delivery line
13 storage reservoir
14 metering device
15 conveying medium
15 ′ surface
16 nozzle
17 current
18 container axis
19 base
20 free space
21 solid/liquid mixture
22 separator
23 pipe
24 conveying medium circuit
25 level
26 gas pressure regulator
27 gas line
28 control valve
29 arrow
30 container wall
31 arrow
32 spiral trajectory
33 jet
34 arrow end
35 flap
36 hinge
37 arrow direction
38 funnel | The invention relates to a method for conveying a solid ( 2 ) in a conveying medium ( 15 ), said solid ( 2 ) being delivered to a container ( 5 ) with outlet ( 7 ). The solid ( 2 ) is in this case dispersed in the transport liquid ( 15 ) without the aid of any mechanically driven parts and is introduced into the conduit ( 4 ). | 1 |
RIGHTS OF THE GOVERNMENT
The invention described herein may be manufactured and used by or for the Government of the United States for all governmental purposes without the payment of any royalty.
BACKGROUND OF THE INVENTION
This invention relates to a process for continuously casting metal or metalloids.
The casting of metal into coninuous sheet form by means of a rotating roller integral with the feed housing is known in the art. Brennan, U.S. Pat. No. 2,912,321, describes a sheet casting apparatus including a crucible, a rotatably supported wheel, a die cavity, and a vertical passage in communication with the die cavity and the crucible. The metal melt in the crucible is passed through the vertical passage into the die cavity and onto the wheel. The wheel is cooled, thus cooling the metal in contact with it.
Brennan, U.S. Pat. Nos. 2,838,814 and 2,931,082, describes apparatus in which the molten metal is cast onto a rotating ring wherein the ring and the cast metal pass through cooling dies for solidification of the metal.
In recent years, considerable research has been devoted to the microstructure of metals and alloys. It is known, for example, that certain post-forming heat treatments can provide improved tensile and stress crack resistance. It is desirable, however, to provide better control of the microstructures during the forming process.
Accordingly, it is an object of the present invention to provide an improved process for the continuous production of sheet material.
Other objects and advantages of the present invention will be apparent to those skilled in the art.
SUMMARY OF THE INVENTION
In accordance with the present invention there is provided a process for continuously casting a thin sheet of castable material, such as metal, which comprises feeding molten material through a metering cap and onto a rotating spreading roller, passing the thus-spread metal into and through the nip between said spreading roller and a quenching roller, taking the thus-formed sheet off the spreading roller and onto the quenching roller, maintaining the sheet in contact with the quenching roller until it is dimensionally stable, and thereafter removing the sheet from the quenching roller.
One feature of the present invention is the spreading roller integral with the molten material feed system which assures that the molten material is continuously and evenly spread to its desired sheet thickness prior to cooling.
BRIEF DESCRIPTION OF THE DRAWING
In the drawing,
FIG. 1 is a side elevation view of one form of apparatus constituting the present invention;
FIGS. 2 and 3 are portions of rollers for forming platelets and continuous wire-like strip, respectively; and
FIG. 4 is a side elevation of another form of the apparatus of the invention illustrating the fabrication of a multi-layer product.
DESCRIPTION OF THE INVENTION
Referring to the drawings, FIG. 1 is illustrative of an apparatus suitable for carrying out the purpose of this invention wherein the numeral 8 represents a spreading and thicknessing die comprising a fixed part, or roller housing 10 and a spreading roller 12, and 14 represents a quenching roller. The lower portion of housing 10 is curved to fit closely adjacent to roller 12 which is rotatably supported adjacent the lower side of housing 10 by suitable bearings 16, shaft 18 and shaft support member 20. Roller 14 is similarly rotatably supported in parallel relation to roller 12 by bearings 22, shaft 24 and shaft support member 26. The shaft support member 26 comprises adjustment means 27 for varying the nip 34 between rollers 12 and 14. Frame means 9 are provided for supporting the die 8.
The relative speeds of rotation of rollers 12 and 14 are maintained by suitable means such as, for example, gears in driving relation to rollers 12 and 14 a representative few of the gear teeth of each being shown at 28 and 30, respectively.
Either roller 12 or roller 14 is rotatably driven by a motor means, not shown, via direct, belt, chain, or other suitable drive means, such as the exemplary chain drive means indicated by reference numeral 32. The rotary motion imparted to either of these rollers is in turn imparted to the other roller through the gears 28 and 30. In a presently preferred embodiment, the circumferential speed of roller 12 is the same as that of roller 14. Thus, the gears 28 and 30 have identical pitch and the pitch circle of each gear is selected to have a diameter approximately equal to that of its associated roller.
The shafts 18 and 24 comprise integral fluid passageways so that fluids may be introduced into and withdrawn from the rollers 12 and 14, respectively, through rotary union means 36 and 38, respectively. The roller 14 is cooled to provide a cooling rate at the nip 34 of at least about 100° K./sec by passing a cooled fluid such as water, oil or a suitable gas through roller 14. The roller 12 may be cooled or heated, depending upon the requirements of the material being processed, in like fashion.
In operation, a molten material 40 to be cast is introduced through delivery passage 42 in block 10 and into the spreading passage 44 formed by the concave portion of housing 10 and the convex surface of roller 12. The rotating roller 12 picks up a finite layer of the material and carries this layer around to the nip 34 where the material contacts the cooled roller 14. The material is, in essence, picked off roller 12 at the nip 34 and thereafter maintained in contact with the roller 14 for less than one complete revolution of roller 14, until it is dimensionally stable, i.e., solidified. The solidified material 46 is taken off roller 14 and coiled or otherwise processed.
As indicated previously, the lower portion of housing 10 is curved to fit closely adjacent to the roller 12. The housing 10 and the roller 12 are preferably manufactured as a unit such that the working clearances, together with other operating parameters such as temperature, density and viscosity of the molten material 40, as well as atmosphere and the circumferential speed, of roller 12, form a metering device, by which the flow rate of the material 40 may be controlled. In general, the clearance between the roller 12 and housing 10 in the region of the spreading passage 44 can be in the approximate range of 10 to 40 mils, preferably about 10 to 20 mils.
The process and apparatus of the present invention may be employed to cast a variety of materials including metals, alloys, metalloids, glasses, thermoplastic resins, and the like, including suspensions of solid particles. Exemplary metals include titanium, copper, aluminum, iron and the like. Exemplary alloys include iron-silicon, aluminum alloys, titanium alloys, stainless steel and the like. Suitable glasses include metallic glasses, oxide glasses, silicate glasses and the like. Suitable thermoplastic resins include polyethylene, polypropylene, polyvinyl chloride, and the like. Exemplary suspensions of solid particles include silicon carbide particles suspended in molten aluminum, aluminum oxide particles suspended in aluminum, rare earth metal oxides suspended in titanium, and the like.
The process and apparatus of this invention may be employed to cast a variety of shapes including discontinuous strip, platelet, and fiber, as well as the continuous sheet discussed heretofore. Either or both of the spreading roller 12 and the quenching roller 14 may have markings etched, engraved or otherwise applied to the surface thereof, which allow the shape, thickness or other properties of the product to be varied in a desired manner. For example, FIG. 2 illustrates a portion of a quench roller 114 having a plurality of square depressions 160 machined therein. When such machined roller 114 is employed, a rotary brush 48 is employed, as shown in FIG. 1, to assure complete removal of platelets formed in the depressions 160 from the roller.
FIG. 3 illustrates a portion of a quench roller 214 having a plurality of circumferential grooves 262 machined therein, for forming continuous rounded strips.
The apparatus shown in FIG. 1 may be used in the position illustrated, employing gravity feed or pressure feed to supply the molten material 40 to the apparatus. The apparatus may also be used in an inverted position, or rotated 90 degrees in either direction, employing pressure feed to supply the material 40.
The apparatus of this invention may be employed to fabricate multi-layer materials. Referring to FIG. 4, which illustrates an apparatus according to the invention in the inverted position, comprising a roller housing 310, a spreading roller 312, and a quenching roller 314. The housing 310 has a delivery passage 342 and a spreading passage 344 for introducing a material 340 to be cast. A previously prepared strip 364 is supplied from a roll, not illustrated, and passed into the nip 366 between the rollers 312 and 314. The material 340 is introduced through passages 342 and 344 and carried by the roller 312 to the nip 366 where it is deposited onto the strip 364 and simultaneously cooled. The resulting strip 368 is a two-layer strip. As an example, the strip 364 may be a polyimide film and the material 340 may be molten copper. The resulting strip 368 is useful in the manufacture of flexible printed circuits. In general, the strip 364 may be any sheet material including those materials described previously, as well as thermosetting plastic materials.
The apparatus of this invention may be fabricated from any suitable materials. The quench roller 14, for example, may be made of an alloy of copper and beryllium. The roller housing 10 may be made of a metal, metal alloy or a ceramic material.
The process and apparatus of this invention make relatively thin sheet, platelet, strip or other form, i.e., finished material with a thickness in the approximate range of 10 to 40 mils. The imposed cooling rate of at least 100° K./sec in the quenching roller 14 can give rise to novel microstructures and properties. It may be desirable to also control the temperature of the spreading roller 12.
Various modifications may be made without departing from the spirit of the invention or the scope of the appended claims. | A process and apparatus for continuously casting a castable material to a thickness of 10 to 40 mils. A molten material is first spread onto a spreading roller to a uniform thickness and then transferred to a quenching roller whereon the material is cooled until dimensionally stable. The apparatus may be employed to continuously cast thin sheet, platelets, wire, etc. The materials castable by this process and apparatus include metals, alloys, glasses, thermoplastic materials and metalloids. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a divisional of U.S. patent application Ser. No. 11/408,474 filed on Apr. 21, 2006, which is incorporated by reference herein in its entirety.
FIELD
The present invention relates to covered stents for use in various medical procedures.
BACKGROUND
The following terms used herein are defined as follows:
The term “stent” means a frame structure containing openings through its wall, typically cylindrical in shape, intended for implantation into the body. A stent may be self-expanding and/or expanded using applied forces.
As used herein, the terms “covered stent” and “stent-graft” are used interchangeably to mean a stent with a cover on at least a portion of its length. The cover can be on the outer surface, the inner surface, on both surfaces of the stent, or the stent may be embedded within the cover itself. The cover may be porous or non-porous and permeable or non-permeable. Active or inactive agents or fillers can be attached to or incorporated into the cover.
Referring to FIG. 4 a , as used in this application, the term “wrinkle” 65 a , 65 b means a fold in a stent cover 62 that has a larger peak to valley height 64 than a thickness 66 of an adjacent stent strut 68 . In the illustrated instance where the cover is mounted within the stent, a wrinkle 65 a in a cover 62 on the outer surface of a covered stent 60 may be identified where the cover extends beyond the inner surface of the stent struts 68 . A wrinkle 65 b can also extend radially inward.
Referring to FIG. 4 b , a wrinkle 65 a in a cover on the inner surface of a covered stent 60 can extend radially outward. Such an outward-extending wrinkle may be identified where the cover 62 extends beyond the outer surface of the stent struts 68 as shown in FIG. 4 b . A wrinkle 65 b can also extend radially inward as shown in FIG. 4 b
Wrinkles can be observed with unaided vision or they can be observed and measured under magnification, such as optical microscopy. “Wrinkle-free” means a stent covering that is substantially free of “wrinkles.”
As used herein, the term “expand” has two distinct meanings. When used in the context of describing stents, it refers to the increase in diameter of those devices. When used in the context of ePTFE material, it refers to the stretching (i.e., expansion) process used to render PTFE material stronger and porous.
As used herein, the term “self-expanding” means the attribute of a device that describes that it expands outwardly, such as in a general radial direction, upon removal of a constraining means, thereby increasing in diameter without the aid of an external force. That is, self-expanding devices inherently increase in diameter once a constraining mechanism is removed. Constraining means include, but are not limited to, tubes from which the stent or covered stent device is removed, such as by pushing. Alternatively, a constraining tube or sheath may be disrupted to free the device or the constraining means can be unraveled should it be constructed of a fiber or fibers. External forces, as provided by balloon catheters for example, may be used prior to expansion to help initiate an expansion process, during expansion to facilitate expansion, and/or after stent or covered stent deployment to further expand or otherwise help fully deploy and seat the device.
As used herein, the term “fully deployed” refers to the state of a self-expanding stent after which the constraining means has been removed and the stent, at about 37° C. over the course of 30 seconds, has expanded under its own means without any restriction. A portion or portions of a self-expanding stent may be fully deployed and the remainder of the stent may be not fully deployed.
The phrase, “operating diametric range” refers to the diametric size range over which the stent or stent-graft will be used and typically refers to the inner diameter of the device. Devices are frequently implanted in vessel diameters smaller than that corresponding to the device fully deployed state. This operating range may be the labeled size(s) that appear in the product literature or on the product package or it can encompass a wider range, depending on the use of the device.
As used herein, the term “porous” describes a material that contains small or microscopic openings, or pores. Without limitation, “porous” is inclusive of materials that possess pores that are observable under microscopic examination. “Non-porous” refers to materials that are substantially free of pores. The term “permeable” describes a material through which fluids (liquid and/or gas) can pass. “Impermeable” describes materials that block the passage of fluids. It should be appreciated that a material may be non-porous yet still be permeable to certain substances.
Stents and covered stents have a long history in the treatment of trauma-related injuries and disease, especially in the treatment of vascular disease. Stents can provide a dimensionally stable conduit for blood flow. Stents prevent vessel recoil subsequent to balloon dilatation thereby maintaining maximal blood flow. Covered stents can provide the additional benefits of preventing blood leakage through the wall of the device and inhibiting, if not preventing, tissue growth through the stent into the lumen of the device. Such growth through the interstices of the stent may obviate the intended benefits of the stenting procedure.
In the treatment of carotid arteries and the neurovasculature, coverings trap plaque particles and other potential emboli against the vessel wall thereby preventing them from entering the blood stream and possibly causing a stroke. Coverings on stents are also highly desirable for the treatment of aneurismal vascular disease. The covers may further act as useful substrates for adding fillers or other bioactive agents (such as anticoagulant drugs, antibiotics, growth inhibiting agents, and the like) to enhance device performance.
The stent covers may extend along a portion or portions or along the entire length of the stent. Generally, stent covers should be biocompatible and robust. They can be subjected to cyclic stresses about a non-zero mean pressure. Consequently, it is desirable for them to be fatigue and creep resistant in order to resist the long-term effects of blood pressure. It is also desirable that stent covers be wear-resistant and abrasion-resistant. These attributes are balanced with a desire to provide as thin a cover as possible in order to achieve as small a delivery profile as possible. Covers compromise the flow cross-section of the devices, thereby narrowing the blood flow area of the device, which increases the resistance to flow. While increased flow area is desirable, durability can be critical to the long-term performance of covered stents. Design choice, therefore, may favor the stronger, hence thicker, covering. Thick covers, however, are more resistant to distension than otherwise identical thinner covers.
Some balloon-expandable stent covers are wrinkle-free over the operating range of the stents because the extreme pressures of the balloons can distend the thick, strong covers that are placed onto the stent at a less than a fully deployed stent diameter. Even the thinnest covers in the prior art such as those made of ePTFE (e.g., those taught in U.S. Pat. No. 6,923,827 to Campbell et al., and U.S. Pat. No. 5,800,522 to Campbell et al.), however, may be too unyielding to be distended by the radial forces exerted by even the most robust self-expanding stents.
Non-elastic and non-deformable self-expanding stent covers are, therefore, generally attached in a wrinkle-free state to the stent when the stent is fully deployed. When such covered stents are at any outer diameter smaller than the fully deployed outer diameter, the cover is necessarily wrinkled. These wrinkles, unfortunately, can serve as sites for flow disruption, clot initiation, infection, and other problems. The presence of wrinkles may be especially deleterious at the inlet to covered stents. The gap between the wrinkled leading edge of the cover and the host vessel wall can be a site for thrombus accumulation and proliferation. The adverse consequences of wrinkles are particularly significant in small diameter vessels which are prone to fail due to thrombosis, and even more significant in the small vessels that provide blood to the brain.
The use of thin, strong materials is known for implantable devices (e.g., those taught in U.S. Pat. No. 5,735,892 to Myers et al.). Extremely thin films of expanded PTFE (ePTFE) have been taught to cover both self-expanding and balloon expandable stents. Typically these films are oriented during the construction of the devices to impart strength in the circumferential direction of the device. Consequently, the expanding forces of the self-expanding stents may be far too low to distend these materials. In fact, such devices are generally designed to withstand high pressures. These coverings, like those of other coverings in the art, are wrinkle-free only when the devices are fully deployed.
Thin, extruded but not expanded fluoropolymer tubes have been used to cover self-expanding and balloon-expandable stents (e.g., U.S. Patent Application 2003/0082324 A1 to Sogard). These seamless extruded tube covers are applied to self-expanding stents in the fully deployed state of the stents. The stent coverings, therefore, possess wrinkles upon crushing the device to a diameter smaller than the fully deployed diameter.
Expanded PTFE material has been used to cover stents that are self-expanding up to a given diameter, then use the assistance of a balloon catheter or other expansion force to achieve the desired clinical implantation diameter (e.g., U.S. Pat. No. 6,336,937 to Vonesh et al). Such covers are wrinkled in the range of diameters up to the diameter at which the stent expands on its own. Beyond that diameter, the covers may be relatively wrinkle-free, however, the stent may no longer be freely self-expanding.
Another type of covered stent previously disclosed (e.g., U.S. Patent Application 2002/0178570 A1 to Sogard) is constructed with two polymeric liners laminated together yet not adhered to the stent. In the absence of bonding a liner to the stent, both an inner and outer liner are necessary and they need to be bonded together at the stent openings in order to construct a coherent stent-graft. This construction provides a relatively smooth liner on one side of the stent. The outer liner follows the geometry of the stent strut and is bonded to the inner liner. As such, according to the definition of a “wrinkle” as provided herein, the outer liner is wrinkled. Expanded PTFE liners of self-expanding covered stents made with shape memory alloys were taught to be laminated together at elevated temperatures, as high as 250° C. (and below 327° C.), while not exceeding a stent temperature which might reset the shape memory state of the alloy. In the absence of bonding the liners to the stent struts, gaps are formed between the liners. Such gaps may become filled with biological materials that compromise the blood flow area and, therefore, may restrict blood flow.
Without the addition of other materials, expanded PTFE materials must be heated well above 200° C. in order the heat bond them together. Given that these stent-graft devices are intended to self-expand at body temperature, the temperature at which the alloy may reset is necessarily close to body temperature. This thermal requirement obviates the possibility of heat bonding the liner to the stent at around a 250° C. temperature. Furthermore, the size of the covered stent that can be constructed in this manner is limited by the physics of heat conduction. That is, a 250° C. heat source must be at a suitable distance from the stent during the lamination process. The liners are laminated with the stent at a diameter less than deployed diameter, hence the size of the openings of the stent are smaller than if the liners were laminated at a larger stent diameter. Consequently, small diameter covered stents cannot be made in accordance with these teachings, nor can the liners be bonded to the stent.
U.S. Pat. No. 6,156,064 to Chouinard teaches use of dip coating to apply polymers to self-expanding stents. Stents and stent-grafts are dipped into polymer-solvent solutions to form a film on the stent followed by spray coating and applying a polymeric film to the tube. Stent-grafts comprising at least three layers (i.e., stent, graft, and membrane) are taught to be constructed in this manner.
Stents have also been covered with a continuous layer of elastic material. As taught in U.S. Pat. No. 5,534,287 to Lukic, a covering may be applied to a stent by radially contracting the stent, then placing it inside a tube with a coating on its inner surface. The stent is allowed to expand, thereby bringing it in contact with the coating on the tube. The surface of contact between the stent and the tube is then vulcanized or similarly bonded. No teaching is provided concerning the diameter of the tube relative to the fully deployed stent diameter. The patent specifically teaches in one embodiment the application of the coating on a stent in the expanded condition. The inventor does not teach how to eliminate or even reduce wrinkles in the stent cover. In fact, the patent teaches how to increase the thickness of the coating, a process that would only increase the occurrence of wrinkling. The patent teaches away from the use of a non-elastic material to cover the stent, and specifically teaches away from the use of a “Teflon®” (i.e., PTFE) tube.
U.S. Patent Application 2004/0024448 A1 to Chang et al teaches covered stents with elastomeric materials including PAVE-TFE. Self-expanding stent-grafts made with this material, like those made of other materials in the art, are not wrinkle-free over the operating range of the devices. These coverings of self-expanding stents are typically applied to the stent in the fully-deployed state. Consequently, wrinkles are formed when the stent-graft is crushed to any significant degree.
SUMMARY
The present invention is an improved expandable implantable stent-graft device that provides a smooth flow surface over a range of operative expanded diameters. This is accomplished by applying a unique cover material to the stent through a unique technique that allows the cover to become wrinkle-free prior to reaching fully deployed diameter. The unique cover material then allows the device to continue to expand to a fully deployed diameter while maintaining a smooth and coherent flow surface throughout this additional expansion.
In one embodiment the present invention comprises a diametrically self-expanding stent-graft device having a graft covering attached to at least a portion of the stent. The device is adapted to be constrained into a compacted diameter for insertion into a body conduit, which will produce wrinkles along its graft surface. However, when the device is unconstrained from the compacted diameter it will self-expand up to a fully deployed diameter with the graft being substantially wrinkle-free over diameters ranging from 50% to 100% of the fully deployed diameter.
Further improvements in the present invention may include providing a fluoropolymer graft component, such as an ePTFE, in the form of either a coherent continuous tube or a film tube. The graft and stent may be combined together through a variety of means, including using heat bonding or adhesive, such as FEP or PMVE-TFE.
By modifying the materials and/or the construction techniques, the range of wrinkle-free expansions can be increased to about 30%-100% or even wider ranges.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 a is a three-quarter isometric view of one embodiment of a covered stent of the present invention in the constrained state, having the cover mounted on the outside of the stent;
FIG. 1 b is a three-quarter isometric view of the embodiment of a covered stent of the present invention of FIG. 1 a in the fully deployed state;
FIG. 2 a is a transverse cross-section view of the embodiment of a covered stent of the present invention deployed to 30% of the fully deployed outer diameter of the device;
FIG. 2 b is a transverse cross-section view of the embodiment of a covered stent of the present invention deployed to 50% of the fully deployed outer diameter of the device with the smooth gradual transition of the adhesive-stent cover interface shown in detail in an enlarged sectional view;
FIG. 2 c is a transverse cross-section view of the embodiment of a covered stent of the present invention taken along line 2 c - 2 c of FIG. 1 b , deployed to 100% of the fully deployed outer diameter of the device with the smooth gradual transition of the adhesive-stent cover interface shown in detail in an enlarged sectional view;
FIG. 3 a is a photomicrograph showing the inside of a covered stent of the present invention that is constrained in a partially deployed state of about 50% of the fully deployed outer diameter of the device;
FIG. 3 b is a photomicrograph showing the inside of a covered stent of the present invention that is constrained in a partially deployed state of about 60% of the fully deployed outer diameter of the device;
FIG. 3 c is a photomicrograph showing the inside of a covered stent of the present invention that is constrained in a partially deployed state of about 70% of the fully deployed outer diameter of the device;
FIG. 3 d is a photomicrograph showing the inside of a covered stent of the present invention that is constrained in a partially deployed state of about 80% of the fully deployed outer diameter of the device;
FIG. 3 e is a photomicrograph showing the inside of a covered stent of the present invention that is constrained in a partially deployed state of about 90% of the fully deployed outer diameter of the device;
FIG. 3 f is a photomicrograph showing the inside of a covered stent of the present invention that is fully deployed;
FIG. 3 g is a photomicrograph showing the inside of a covered stent of the prior art that is constrained in a partially deployed state of about 50% of the fully deployed diameter;
FIG. 4 a is a transverse cross-section view of exemplary wrinkles in a cover on the outer surface of the stent; and
FIG. 4 b is a transverse cross-section view of exemplary wrinkles in a cover on the inner surface of the stent.
DETAILED DESCRIPTION
The present invention addresses the problem of wrinkles in the covers in stent-grafts. The covers of self-expanding stent-grafts heretofore exhibited wrinkles when deployed to diameters smaller than the diameter at which the cover was applied to the stent, which is typically the fully deployed diameter. Inasmuch as body conduits are rarely the exact diameter of the stent-graft, rarely uniformly circular in cross-section, and rarely non-tapered, sections or entire lengths of self-expanding stent-grafts frequently are not fully deployed and hence present wrinkled surfaces to flowing blood or other body fluids. Furthermore, covered stents are often intentionally implanted at less than their fully deployed diameters in order to utilize their inherent radial expansion force to better anchor the devices against the host tissue, thereby preventing device migration in response to blood flow. Such practices come at the expense of having to tolerate devices with at least partially wrinkled covers. The present invention involves the use of a unique stent cover material, one that combines two seemingly mutually exclusive properties—being both strong enough to withstand the forces exerted by constant, cyclic blood pressure and also distensible enough to expand in response to the expansion forces exerted by a self-expanding stent.
In addition, a unique manufacturing method had to be devised in order to utilize this material to construct a self-expanding stent-graft. The temperature-constrained shape-memory properties of self-expanding stents introduce significant processing challenges. Ultimately, a process was developed which entailed not only applying the cover to the stent in a cold environment, but also entailed bonding the cover to the stent at these cold temperatures.
Referring to FIGS. 1 a and 1 b , the present invention is directed to implantable device 60 having a self-expanding stent component 63 with either an inner or outer cover 62 (or both), that is wrinkle-free over an operating diametric range of the device. The cover 62 has wrinkles 65 in the constrained state as shown in FIG. 1 a . The wrinkles disappear once the device self-expands to the diameter at which the cover was applied to the stent. The cover 62 remains wrinkle-free as the device 60 self-expands even further as shown in FIG. 1 b . The invention addresses the clinical problems associated with wrinkles in self-expanding stent covers while providing the minimum amount of covering material. Wrinkles are known to disrupt blood flow and become sites for clot deposition which can ultimately lead to graft thrombosis and embolus shedding. These sequelae may create serious clinical consequences, especially in organs such as the brain. The incorporation of a single, very thin cover enables a stent-graft device with a profile dictated primarily by the stent strut dimensions, not by the mass or volume of the cover. The present invention, therefore, provides a heretofore unavailable combination of deployment diameter for a given size stent-graft and a wrinkle-free cover surface over a wide range of deployed diameters.
For use in the present invention, nitinol (nickel-titanium shape memory alloy) and stainless steel are preferred stent materials. Nitinol is preferred for its shape memory properties. The memory characteristics can be tailored for the requirements of the stenting application during the fabrication of the alloy. Furthermore, nitinol used to make the stent can be in the form of wire that can be braided or welded, for example, or it can be tubing stock from which a stent is cut. While nitinol offers a wide variety of stent design options, it should be appreciated that stainless steel and other materials may also be formed into many different shapes and constructs.
Stent covers of the present invention are preferably durable and biocompatible. They may be seamless or contain one or more seams. The stent covering of the present invention has a low Young's modulus, which enables it to be distended with the minimal force that is exerted by a self-expanding stent. Furthermore, the covering is provided with a minimal (or non-existent) elastic recoil force so that after stent expansion the covering does not cause the stent-graft to decrease in diameter over time. The cover is also preferably thin. Thinness has the multiple benefits of reducing the introduction size of the device, maximizing the blood flow cross-section, providing less resistance to radial expansion, and introducing less elastic recoil.
In a preferred embodiment, a nitinol stent is chilled and crushed to a diameter less than the fully deployed outer diameter. The chilling is desirable to help maintain the stent in the crushed state. The covering is then applied without creating wrinkles. The constrained diameter is selected according to the intended operating parameters of the device, such as about 90% of the fully deployed outer diameter or less, about 80% of the fully deployed outer diameter or less, about 70% of the fully deployed outer diameter or less, about 60% of the fully deployed outer diameter or less, and for most applications most preferably about 50% of the fully deployed outer diameter or less. While maintaining the device in the chilled state, the stent-graft is allowed to dry and then further crimped with a chilled crimping tool and transferred into a delivery catheter.
The stent cover may consist of fluorinated ethylene propylene (FEP) coating the nodes and fibrils of ePTFE film. Most preferably, a cover of ePTFE, is used to practice the invention. Whereas ePTFE is known for its high tensile strength, that strength is imparted only in the direction of expansion. If the ePTFE material is not expanded in the orthogonal direction (i.e., the transverse direction in the case of films) during the processing of the material, the ePTFE material is extremely distensible in that direction. Such materials have both very low tensile strength and very low Young's modulus in the transverse direction. The low Young's modulus property enables the material to distend under low forces. Films used to construct articles of the present invention can be easily elongated in the transverse direction by hand, thereby demonstrating their low Young's modulus values. In the most preferred embodiments, therefore, the ePTFE materials are in the form of very thin, highly porous films that are highly distensible in the transverse direction. The combination of high porosity and thinness result in a cover material that occupies minimal volume of the device. Expanded PTFE stent covers may offer additional advantages by virtue of the ability to provide and control their porosity. Various agents or fillers can be added to the surface or within the pores of the material. Such agents and fillers may include but are not limited to therapeutic drugs, antithrombotic agents, and radio opaque markers. If desired, portions of or the entire ePTFE cover may optionally be rendered non-porous or non-permeable by densifying, filling the pores, or through any other suitable means. Preferably, to provide added stability to the material, the ePTFE material is raised above its crystalline melt point, that is, the ePTFE material is “sintered.”
It is believed that thin ePTFE films possessing a thickness of less than about 0.25 mm are preferred for practicing the present invention. It is believed that even more preferred are films possessing a thickness less than about 0.1 mm. Preferred thin ePTFE films possess densities in the range of about 0.2 to about 0.6 g/cc. It is believed that more preferred thin ePTFE films have densities in the range of about 0.3 to about 0.5 g/cc. It is believed that preferred thin ePTFE films possess matrix tensile strengths in the range of about 70 to about 550 MPa and about 15 to about 50 MPa, in the longitudinal and transverse directions, respectively. It is believed that more preferred thin ePTFE films possess matrix tensile strengths in the range of about 150 to about 400 MPa and about 20 to about 40 MPa, in the longitudinal and transverse directions, respectively. The preferred film for use in practicing the present invention is a thin ePTFE film possessing a thickness of about 0.02 mm, a density of about 0.4 g/cc, longitudinal matrix strength of about 260 MPA, and a transverse matrix tensile strength of about 30 MPa.
It is believed that preferred thin ePTFE films possess Young's modulus in the range of about 100 to about 500 MPa and about 0.5 to about 20 MPa, in the longitudinal and transverse directions, respectively. It is believed that more preferred thin ePTFE films possess Young's modulus in the range of about 200 to about 400 MPa and about 1 to about 10 MPa, in the longitudinal and transverse directions, respectively. The most preferred Young's modulus values of the film in the longitudinal and transverse directions are about 300 MPa and about 2 MPa, respectively. This film is exceedingly distensible in the transverse direction.
The choice of film properties is largely dependent on the force the self-expanding stent exerts on the material during expansion. For example, stronger films may be used with stents that exert higher radial forces during self-expansion.
To take advantage of the low Young's modulus of the film, the covered stent may be constructed with the low Young's modulus direction of the film oriented in the circumferential direction of the stent. The high strength direction of the film is therefore oriented in the axial direction of the stent. Preferably, the film is applied to the stent in the shape of a tube. A film tube is constructed by rolling multiple layers of the film around the circumference of a mandrel that is covered with a release material (such as Kapton film, part number T-188-1/1, Fralock Corporation, Canoga Park, Calif.). Preferably, three or fewer ePTFE film layers are applied, more preferably a single layer is applied wherein the overlap seam is narrow and comprises only two layers of the film.
The film tube can be attached to the stent by suturing, gluing, and the like. Gluing is preferred, utilizing an adhesive or combination of adhesives by means such as spraying or dipping. It is preferred to dip coat a fully deployed stent with an adhesive, ensuring that the adhesive does not span the openings in the stent. Thermal or ambient cured adhesives can be used. When bonding the film tube to a shape memory metal stent using a thermally-activated adhesive, the adhesive should be curable at a temperature below the critical transition temperatures of the metal. Adhesives such as perfluoroethylvinylether-tetrafluoroethylene (PEVE-TFE) or perfluoropropylvinylether-tetrafluoroethylene (PPVE-TFE) are preferred. Terpolymers containing at least two of the following monomers are also preferred: PEVE, PPVE, perfluoromethylvinylether (PMVE), and TFE. Most preferably, the adhesive is perfluoromethylvinylether-tetrafluoroethylene (PMVE-TFE) material when bonding the cover to a nitinol stent.
FIG. 2 a depicts a cross-section of the covered stent of the present invention that was constructed at 50% of the fully deployed outer diameter, crimped and transferred inside a delivery catheter, and then deployed to 30% of the fully deployed outer diameter of the device. The stent cover 62 can be attached to the outer surface of the stent by bonding it to stent struts 68 as shown in FIG. 2 a , thereby providing an outer stent cover 51 to the stent 63 . The cover 62 can alternatively be bonded to the inner surface of the stent as shown in FIG. 4 b , providing an inner stent cover 41 .
The most preferred way to attach the film tube to the outer surface of the stent involves placing the film tube inside a rigid (e.g., glass) tube that has an inner diameter smaller than the fully deployed out diameter of the stent, then inserting the crimped stent inside the film tube and bonding the stent and film tube together.
The film tube covering is first inserted inside the constraining tube without creating wrinkles. The ends of the film tube may be everted over the ends of the constraining tube. Preferably the ends are everted to the extent that modest tension is applied to the film tube, enough to hold the film tube taut and thereby keep the film tube free of wrinkles. As has been noted, the inner diameter of the constraining tube, and hence the constraining diameter, should be less than the fully deployed diameter of the device, such as 90% of the fully deployed outer diameter or less, about 80% of the fully deployed outer diameter or less, about 70% of the fully deployed outer diameter or less, about 60% of the fully deployed outer diameter or less, or about 50% of the fully deployed outer diameter or less.
A nitinol stent is prepared by dip coating a thin layer of adhesive to its struts and allowing the adhesive to dry. The preferred adhesive is PMVE-TFE, such as that taught in Example 5 of US Patent Application 2004/0024448 to Chang et al. Contrary to practices in the prior art that teach bonding covers to stents at ambient or even highly elevated temperatures, the cover is applied to the stent at lower than ambient temperatures. Preferably, the stent is chilled and crimped in a cold chamber (e.g., the freezer compartment of a refrigerator). The low temperature process is desired in order to cool the stent in order to dimensionally stabilize it at a diameter less than the film tube diameter while the cover is attached. The crimped stent is next inserted inside the film tube, which is inside a rigid tube. The assembly is permitted to warm to ambient temperature. The stent expands, hence comes in intimate contact with the film tube, as it warms. The assembly is submerged in a solvent that activates the PMVE-TFE adhesive and then warmed above ambient temperature to evaporate the solvent, thus allowing the adhesive to solidify.
The device inside the rigid tube is then again chilled in a freezer to a temperature at which at the device does not self-expand if unconstrained and then the stent-graft is removed from the tube. At this point, the stent-graft is further crimped using the chilled crimping machine, and transferred inside of a delivery catheter. Instead of crimping at this stage, alternatively the porous ePTFE cover of the stent-graft device may be rendered non-permeable. One method to do so can be achieved by dipping the device into a chilled dilute solution of elastomeric material, such as PMVE-TFE, PEVE-TFE, PPVE-TFE, or silicone. A dilute solution is preferred inasmuch as the solution becomes significantly more viscous when chilled to the same temperature as the device. Once the solution dries, the stent-graft can be crimped further, as previously described, and transferred inside of a delivery catheter.
Therapeutic agents, fillers, or the like can be added to the stent cover, the adhesive used to bond the stent cover to the stent or the elastomer material used to render the cover non-permeable or any combination thereof.
Stent-grafts made in this manner exhibit wrinkle-free coverings over the device diameter range extending from the diameter at which the covering was applied up to and including the fully deployed diameter. FIG. 2 b illustrates the wrinkle-free stent cover 62 (in this case, on the outer surface of the stent) at the diameter at which it was bonded to the stent struts 68 , thereby forming the covered stent device 60 . The thin cover 62 stretches and remains wrinkle free up to and including the fully deployed diameter as shown in FIG. 2 c . FIG. 2 c depicts a cross-section of the covered stent of FIG. 1 b . In order to achieve this device performance, the covering should be applied to the stent at a diameter smaller than the fully deployed diameter. This diameter should be no larger than the smallest intended diameter of the implanted device. Crushing the device below the diameter at which the cover was applied induces wrinkles in the stent cover. For example, crushing a device of the present invention to such a degree that it is small enough to be transferred to inside a delivery catheter will induce wrinkles in the stent cover. The wrinkles are no longer present once the deployed stent-graft reaches the diameter at which the cover was applied. Attaching the covering at an intermediate stent size means less crushing is necessary to decrease the stent-graft diameter for insertion into the delivery catheter. The likelihood of perforating the cover during the crushing process is reduced when less crushing is needed.
A stent-graft with an inner cover can be fabricated with a film tube and an adhesive-coated stent as previously described. The stent can be chilled then crushed and constrained inside a constraining tube. The film tube can then be mounted onto a balloon, introduced inside the stent, pressed against the stent via inflating the underlying balloon, then bonded to the stent by immersing the assembly into the appropriate solvent for the adhesive, and then allowed to dry. The balloon is then deflated and the stent-graft plus the constraining tube are again chilled to enable removal of the constraining tube prior to further radial crushing of the stent-graft and loading the device into the delivery system.
The present invention also minimizes flow disturbances caused by blunt stent strut profiles. As seen in FIG. 2 b and FIG. 2 c the adhesive material 22 bonded to stent strut 68 forms a smooth gradual transition where it attaches to stent cover 62 . In the absence of this transition, the stent strut 68 may present a blunt profile to the flowing blood.
The wrinkle-free feature of articles of the present invention can benefit the performance of tapered stent-grafts. Tapered grafts are widely used in the treatment of aortoiliac disease. The present invention, which can include or not include a tapered stent and/or cover, can be implanted inside a tapered vessel without exhibiting wrinkles in the cover. That is, regardless of the shape of the starting materials, the device of the present invention can conform to become a tapered self-expanding stent-graft when deployed within a tapered body conduit. This allows tapered body conduits to be treated with non-tapered devices that are easier and less expensive to construct, without deploying an improperly sized stent-grafts. This also allows for a wider range of effective deployable sizes and shapes without the need to increase the number of different configurations of products.
The present invention has particular value in very demanding, small caliber stenting applications. These are applications in which a cover is needed to either protect against plaque or other debris from entering the blood stream after balloon angioplasty or to seal an aneurysm. Perhaps the most demanding applications are those involving the treatment of carotid and neural vessels where even small wrinkles in the stent cover may create a nidus for thrombosis. Given the sensitivity of the brain, the consequences of such thrombus accumulation and possible embolization can be dire. Not only does the present invention overcome the challenging problem of providing a wrinkle-free cover in a viable stent-graft, it accomplishes this with a surprisingly minimal amount of covering material. It was unanticipated that such a distensible, thin, and low mass material could satisfactorily perform as a stent covering.
The following examples are intended to illustrate how the present invention may be made and used, but not to limit it to such examples. The full scope of the present invention is defined in the appended claims.
EXAMPLES
To evaluate the examples, the following test methods were employed.
Test Methods
Assessment of Wrinkles
Stent-graft device covers were visually examined without the aid of magnification at ambient temperatures. Microscopic examination might be warranted for very small devices. The ends of devices were secured within a hollow DELRIN® acetal resin block in order fix the longitudinal axis of the device at an angle of about 45° above horizontal which enabled viewing the inner surface of the stent-grafts. The devices were positioned to allow examination of free edge of the device and stent openings nearest the ends of the device. Stent-grafts that were not fully deployed were constrained inside rigid tubes during examination. Fully deployed devices were submerged in an about 37° C. water bath prior to examination.
Alternatively, optical or scanning electron microscopy could be used to look for the presence or absence of wrinkles.
Dimensional Measurements
Stent and covered stent device outer diameters were measured with the aid of a tapered mandrel. The end of a device was slipped over the mandrel until the end fit snuggly onto the mandrel. The outer diameter of the device was then measured with a set of calipers. Optionally, a profile projector could be used to measure the outer diameter of the device while so placed on the mandrel.
The fully deployed outer diameter was measured after allowing the self-expanding device to fully deploy in a 37° C. water bath for 30 seconds, then measuring the device diameter in the water bath in the manner previously described.
For devices constrained inside constraining means having a round cross-section, the device outer diameter in the constrained state was taken to be the inner diameter of the constraining means.
In order to examine a device at some percentage of the fully deployed diameter of the device, the fully deployed diameter must first be known. A length of a device can be severed from the entire device and its fully deployed diameter can be measured. For example, a length of the device can be released from the delivery catheter and its diameter measured after being fully deployed in a 37° C. water bath.
Tensile Break Load, Matrix Tensile Strength (MTS), and Young's Modulus Determinations
Tensile break load of the film was measured using a tensile test machine (Model 5564, Instron Corporation, Norwood, Mass.) equipped with flat-faced grips and a 10 N and 100 N load cells for the transverse and longitudinal values, respectively. The gauge length was 1 inch (2.54 cm) and the cross-head speed was 1 in/min (2.54 cm/min). Each sample was weighed using a Mettler AE2000 scale (Mettler Instrument, Highstown, N.J.), then the thickness of the samples was measured using a snap gauge (Mitutoyo Absulute, Kawasaki, Japan). A total of ten samples were tested. Half were tested in the longitudinal direction, half were tested in the transverse (i.e., orthogonal to the longitudinal) direction and the average of the break load (i.e., the peak force) was calculated. The longitudinal and transverse MTS were calculated using the following equation:
MTS =(break load/cross-section area)*(density of PTFE)/bulk density of the film), wherein the density of PTFE is taken to be 2.2 g/cc.
Young's modulus was determined from tensile test data obtained using a tensile test machine (Model 5500, Instron Corporation, Norwood, Mass.). The test was performed using a sample gauge length of 1 inch (2.54 cm) and a cross-head speed of 1 in/min (2.54 cm/min). A total of ten samples were tested. Half were tested in the longitudinal direction, half were tested in the transverse (i.e., orthogonal to the longitudinal) direction.
Inventive Example 1
Tubular, self-expanding nitinol stents constructed using the pattern as described in FIG. 4 of U.S. Pat. No. 6,709,453 to Pinchasik et al., were obtained. The stents had an outer diameter of approximately 8 mm and lengths of about 44 mm. Six sections about 15 mm in length were cut from the stents. Each of the six sections was processed in the following manner. The stent was dip-coated with PMVE-TFE, a liquefied thermoplastic fluoropolymer as described in Example 5 of US Patent Application 2004/0024,448 of Chang, et. al.
A short piece of silver-plated copper wire (approximately 0.5 mm in diameter) was fashioned into a hook and used to suspend the stent. The stent was submerged in a 3% by weight solution of PMVE-TFE and FC-77 solvent (3M Fluoroinert, 3M Specialty Chemicals Division, St Paul, Minn.). The dipped stent was removed from the solution and air-dried. The hook attached to the opposite end of the stent and the dipping process was repeated. The stent was next dipped in a 2% by weight solution of the fluoropolymer and the solvent, then air-dried. Once again, the hook was attached to the opposite end of the stent and the stent was again dipped into the 2% solution. This dipping process, therefore, consisted of four total dips, which yielded a uniform and uninterrupted layer of thermoplastic fluoropolymer on the stent struts. The amount of material applied weighed approximately 0.01 grams as determined by weighing the stent before and after the dipping process.
A stent covering was made as follows. A 4.0 mm stainless steel mandrel was obtained. A 4 mm inner diameter thin-walled (wall thickness of about 0.1 mm) ePTFE tube was fitted over the mandrel. The purpose of this tube was to later assist in removing the stent cover from the mandrel. Next, a spiral wrapping of ribbon of polyimide sheeting (KAPTON®, Part Number T-188-1/1, Fralock Corporation, Canoga Park, Calif.) was applied on top of the ePTFE tube to completely cover a 75 mm length of the graft.
A thin ePTFE film with the following properties was obtained: width of about 50 mm, matrix tensile strength in the longitudinal direction of about 256 MPa, matrix tensile strength in the transverse direction of about 31 MPa, a thickness of 0.02 mm, and a density of about 0.39 g/cc. (The tensile strengths in the longitudinal and transverse directions were 45 MPa and 5 MPa, respectively.) Young's modulus values of the film in the longitudinal and transverse directions were 282 MPa and 1.9 MPa, respectively. An approximately 80 mm length of the film was applied on top of the polyimide sheeting in the axial direction of the mandrel such that the ends of film were in direct contact with the thin-walled ePTFE tube. The corners of these ends were heat bonded to the thin-wall tube with the use of a local heat source (Weller Soldering Iron, model EC200M, Cooper Tools, Apex, N.C.) set to 343° C. With the film tacked in place in this manner, one layer of the film was wrapped about the circumference of the mandrel. Wrapping of the film was performed under minimal tension in order to avoid stretching the film. Approximately a 2 mm width of overlap region was created. The film layers in this overlap region were heat bonded together with the soldering iron set to 343° C. to form a seam. For this construction, therefore, the longitudinal direction of the film, which was its high strength direction, was oriented along the length of the mandrel. The weaker, transverse, film direction was oriented in the circumferential direction of the mandrel.
A second layer of polyimide film was helically wrapped on top of the ePTFE film, completely covering it. This entire assembly was then placed in a forced air oven (Model NT-1000, Grieve Corporation, Round Lake, Ill.) set at 370° C. The assembly was removed from the oven after 7 minutes and allowed to cool. After cooling, the outer wrap of polyimide film was removed. The film tube, inner layer of polyimide film, and the thin-walled ePTFE tube, together, were carefully removed from the mandrel. The thin-walled ePTFE tube was everted, thereby removing it from the polyimide film. The polyimide film was then carefully removed from the ePTFE film tube.
The stent and film tube were next assembled into a stent-graft. The ePTFE film tube was inserted inside a 60 mm long glass tube having an inner diameter of 4 mm and a wall thickness of 1 mm such that both ends of the film tube extended beyond the ends of the glass tube. The ends of closed forceps were then used to spread the ends of the film tube by placing them inside each end of the tube and then opening them. The film tube ends were everted over the outside of the glass tube. The film was tacky enough to secure the ends to the surface of the tube, thereby holding the wrinkle-free film tube in place. The glass tube with the ePTFE film tube inside it was placed in a conventional freezer set at approximately −15° C. Tools that would later be used to create the stent-graft, namely a set of tweezers and an iris-type stent crimping device, such as taught in US 2002/0138966 A1 to Motsenbocker, were also chilled in the freezer compartment.
The chilled crimping device was used to reduce the diameter of the adhesive-coated stent uniformly along its length. The outer diameter of the stent was reduced to about 3 mm. Using chilled tweezers, the following procedure was performed inside the freezer compartment. The stent was removed from the crimper and transferred into the ePTFE film tube that was inside the chilled glass tube. The glass tube, film tube and stent were then removed from the freezer and allowed to warm to ambient temperature. The stent, by virtue of its shape memory characteristics, self-expanded as the assembly warmed. In doing so, the stent exerted radial force against the film tube, creating intimate contact between the stent and the film-tube along the length of the stent.
Next, the stent cover was bonded to the stent. This assembly, still constrained by the 4 mm inner diameter of the glass tube, was then dipped in a container of FC-77 solvent for 40 seconds in order to activate the adhesive. The assembly was then allowed to dry for approximately 30 minutes while being warmed to 40° C. through the use of a halogen lamp. The assembly was allowed to cool to ambient temperature. In this way, a stent-graft device was created.
The stent-graft device was pushed to one end of the glass tube until the end of the stent was flush with the end of the glass tube. The ePTFE covering was trimmed flush with the stent. The process was repeated to trim the opposite end of the stent-graft. With the stent-graft still inside the glass tube, the device was inspected to ensure thorough and uniform bonding between the stent cover and the stent and to verify the absence of wrinkles in the covering.
The next step entailed loading the stent-graft into a delivery system. The stent-graft device, still constrained by the glass tube, was chilled in a freezer as previously described. The device was then transferred to inside a chilled iris crimper and further radially crushed to reduce its outer diameter to the desired delivery profile (i.e., crushed outer diameter), which was about 2 mm. The device was then transferred from the crimper into its intended delivery system. Thus, the device was prevented from self-expanding to its fully deployed outer diameter during the assembly and loading processes.
The resultant stent-graft device had a delivery profile of about 2 mm and a fully deployed outer diameter of 8 mm. Photographs were taken of the device at various stages of deployment and subsequent re-crushing. The outer diameter of the device was characterized as a percentage of the fully deployed outer diameter, which was about 8 mm. The fully deployed device outer diameter was about 8 mm at both about 37° C. and at ambient temperature. It should be noted that this may not be the case for other types of nitinol alloys.
FIGS. 3 a through 3 f are photomicrographs showing the inside of the six covered stents of this example. One device was transferred from its 2 mm delivery profile constraining sheath into a hollowed DELRIN® resin block with an inner diameter corresponding to about 50% of the fully deployed outer diameter of the device. This 50% of the fully deployed outer diameter corresponds to the outer diameter at which the device was made. Photomicrographs were taken of the end of the device as previously described. A representative image is shown as FIG. 3 a . This photomicrograph indicates the absence of wrinkles in the stent covering. Another device was transferred into a hollowed DELRIN® resin block with an inner diameter corresponding to about 60% of the fully deployed outer diameter of the device. A representative image is shown as FIG. 3 b . This photomicrograph indicates the absence of wrinkles in the stent covering. A third device was transferred into a hollowed DELRIN® resin block with an inner diameter corresponding to about 70% of the fully deployed outer diameter of the device. A representative image is shown as FIG. 3 c . This photomicrograph indicates the absence of wrinkles in the stent covering. The fourth and fifth stent-grafts were transferred into hollowed DELRIN® resin blocks with inside diameters of 80% and 90% of the fully deployed outer diameter of the devices, respectively; representative photomicrographs appear in FIGS. 3 d and 3 e , respectively. The coverings were wrinkle-free in both of these states, as indicated in the photomicrographs. The sixth device was fully deployed in a 37° C. water bath and then examined under a microscope. A representative image is shown as FIG. 3 f . This photomicrograph indicates the absence of wrinkles in the stent covering.
Comparative Example 2
Film used in the construction of the six stent-graft devices of Example 1 was used to make a stent-graft in accordance with the teachings of the prior art. The cover was applied to a length of a stent of the type previously-described. In this case, the cover was attached to the stent in the fully deployed state under ambient conditions. The cover was applied in the same manner as described previously. The stent-graft device was then transferred to inside a chilled iris crimper as previously described and further radially crushed to reduce its outer diameter to the desired delivery profile (i.e., crushed outer diameter), which was about 2 mm. The device was then transferred from the crimper into its intended delivery system. Thus, the device was prevented from self-expanding to its fully deployed outer diameter during the assembly and loading processes. The resultant stent-graft device had a delivery profile of about 2 mm and a fully deployed outer diameter of 8 mm. This device was deployed within a hollow DELRIN® resin cavity, as described in Example 1. The diameter of the hole in the block corresponded to about 50% of the fully deployed diameter of the device. A representative photomicrograph of the crushed device appears as FIG. 3 g.
The advantage of making the stent-graft device of the present invention in the above-described manner is clear when comparing FIG. 3 a with FIG. 3 g . Both photomicrographs were taken at 50% of the fully deployed outer diameter. FIG. 3 a , unlike FIG. 3 g , exhibits no wrinkles. FIG. 3 a demonstrates the wrinkle-free benefit of the present invention. On the other hand, FIG. 3 g demonstrates the wrinkles that result from crushing a film tube that was made at 100% of the deployed diameter, then crushed to 50% of the deployed diameter. Note the wrinkles in the leading edge of the cover in FIG. 3 g.
While particular embodiments of the present invention have been illustrated and described herein, the present invention should not be limited to such illustrations and descriptions. It should be apparent that changes and modifications may be incorporated and embodied as part of the present invention within the scope of the following claims. | An improved stent-graft device is provided that delivers a smooth flow surface over a range of operative expanded diameters by applying a unique cover material to the stent through a technique that allows the cover to become wrinkle-free prior to reaching fully deployed diameter. The unique cover material then allows the device to continue to expand to a fully deployed diameter while maintaining a smooth and coherent flow surface throughout this additional expansion. Employed with a self-expanding device, when the device is unconstrained from a compacted diameter it will self-expand up to a fully deployed diameter with the graft being substantially wrinkle-free over diameters ranging from about 30-50% to 100% of the fully deployed diameter. | 8 |
[0001] The present application is claims priority of Japanese Patent Application Serial No. 2010-192719, filed Aug. 30, 2010, the content of which is hereby incorporated by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a code amount reducing apparatus, an encoder and a decoder in an apparatus for encoding video signals having a high frame rate particularly based on human visual property in order to perform encode control on the video signals.
[0004] 2. Description of the Related Art
[0005] As an encode system based on human spatio-temporal visual property, there is proposed a system in Patent Literature 1 described later. In the Patent Literature 1, there is disclosed a technique in which an encode parameter is decided by a cost function minimizing rule using an encode distortion weighted based on a spatio-temporal visual property.
[0006] On the other hand, in Patent Literature 2 and Non-Patent Literature 1, there is disclosed an encoded picture controlling system using an illusion principle by sharp/blurred repeated playback. The sharp/blurred repeated illusion means that when there are pictures at 60 frames per second, for example, if sharp pictures (high resolution pictures, 30 frames per second) and blurred pictures (low resolution pictures, 30 frames per second) are repeated every picture, the entire picture seems fairly sharp. Consequently, it is expected to improve a picture encode efficiency with a little deterioration of the picture quality.
Patent Literature 1: Japanese Patent Application Laid-Open No. 2008-283599 Publication Patent Literature 2: Japanese Patent Application Laid-Open No. 2009-100433 Publication Non-Patent Literature 1: “Repetition of Sharp/Blurred TV Pictures and Its Application to Frame Interpolation (TFI)-Extension of Signal Processing of Visual Perception” Journal of The Institute of Image Information and Television Engineers 63(4) (727) pp. 549-552
[0010] However, the technique described in Patent Literature 1 has a problem that the code amount cannot be drastically reduced at a high frame rate such as 60 frames per second.
[0011] As described in Patent Literature 2 and Non-Patent Literature 1, since encoding low resolution pictures every picture may lead to lowering a correlation in the temporal direction, in some cases, the encode efficiency can be lowered. The system described in Patent Literature 2 and Non-Patent Literature 1 assumes that frames are uniquely decided as either sharp or blurred frames and a uniform filter processing is applied to the blurred frames in a picture. There is known that a problem occurs in which when the uniform filter processing is performed in the picture in this way, a deterioration partially occurs due to video motion property.
SUMMARY OF THE INVENTION
[0012] It is an object of the present invention to provide a code amount reducing apparatus, an encoder and a decoder capable of highly reducing the code amount of a video signal for a high frame rate video without deteriorating the picture quality by processings only at the encode side.
[0013] In order to achieve the object, this invention is firstly characterized in that a code amount reducing apparatus in an apparatus for performing frequency conversion such as orthogonal conversion on a predictive error signal obtained by using a correlation between video signals in the temporal or spatial direction, and then encoding said predictive error signal, comprises a target frame specifying unit for specifying a frame to be processed, a unit for acquiring a coefficient string by collectively frequency-converting, for a target frame specified in said target frame specifying unit, pixel values at predetermined area or predetermined macro block of said target frame and pixel values at the same area or macro block in the frames before and after said target frame, a unit for finding a non-perceptible coefficient based on a spatio-temporal visual property model for said coefficient string and a unit for setting said non-perceptible high frequency coefficient at 0 for a frequency conversion coefficient of orthogonal conversion of said predictive error signal.
[0014] The invention is secondly characterized in that when said encode is in the intra-mode, said non-perceptible high frequency coefficient is set at 0 for said frequency conversion coefficient of orthogonal conversion of said predictive error signal, and when said encode is in the inter-mode, all said frequency conversion coefficients of orthogonal conversion of said predictive error signal are set at 0.
[0015] The invention is thirdly characterized in that the apparatus further comprises an encode mode selecting unit, wherein said encode mode selecting unit selects an encode mode having a smaller code amount from among the intra-mode in which said non-perceptible high frequency coefficient is set at 0 for said frequency conversion coefficient of orthogonal conversion of said predictive error signal and the inter-mode in which all said frequency conversion coefficients of orthogonal conversion of said predictive error signal are set at 0.
[0016] The invention is fourthly characterized in that an encoder for performing frequency conversion such as orthogonal conversion on a predictive error signal obtained by using a correlation between video signals in the temporal or spatial direction, and then encoding said predictive error signal, comprises a decoder for decoding an encoded video signal, a target frame specifying unit for specifying a frame to be processed, a unit for acquiring a coefficient string by collectively frequency-converting, for a target frame decoded in said decoding unit and specified in said target frame specifying unit, pixel values at predetermined area or predetermined macro block of said target frame and pixel values at the same area or macro block in the frames before and after said target frame, a unit for finding a non-perceptible coefficient based on a spatio-temporal visual property model for said coefficient string, a unit for setting said non-perceptible high frequency coefficient at 0 for a frequency conversion coefficient of orthogonal conversion of said predictive error signal, and a unit for reconstructing encoded data of said encoded video signal based on the result that said non-perceptible high frequency coefficient is set at 0.
[0017] The invention is fifthly characterized in that an encoder including the code amount reducing apparatus comprises a unit for encoding encode control processing information and applied frame number information acquired from said target frame specifying unit, wherein said encode control processing information and said applied frame number information encoded by said encoding unit are inserted into a bit stream containing said frequency conversion coefficient whose code amount is reduced by said code amount reducing apparatus, and are output.
[0018] The invention is sixthly characterized in that a decoder for decoding a video signal encoded by the encoder comprises a unit for separating a frequency conversion coefficient of a video signal, said encode control processing information and said applied frame number information from said bit stream, a unit for decoding said separated frequency conversion coefficient, a displaying unit for displaying a video signal acquired by said decoding, a unit for decoding said separated encode control processing information and applied frame number information, and a playback control unit for outputting a playback control signal, wherein when a control signal for slow motion playback or pause is output from said playback control unit, a processed frame specified by said target frame specifying unit from a video signal acquired by said decoding is skipped, and is not displayed on the displaying unit.
[0019] According to the first to sixth features, it is possible to provide a code amount reducing apparatus or an encoder suitable to be applied to an apparatus for encoding a video signal particularly at a high frame rate (such as 60 fps, 120 fps). The code amounts of the video signals per several frames can be largely reduced without deteriorating the picture quality by the processings only at the encode side.
[0020] According to the first feature, since the non-perceptible high frequency coefficient can be assumed as 0 based on the spatio-temporal visual property model for the frequency conversion coefficient of the orthogonal conversion of the predictive error signal, the code amount can be reduced with no or little deterioration of the substantial picture quality substantially.
[0021] According to the second feature, since all the frequency conversion coefficients of the orthogonal conversion of the predictive error signal are assumed as 0 in the inter-mode encode, a processing load is small and the code amount can be reduced with no or little deterioration of the substantial picture quality substantially.
[0022] According to the third feature, the encode mode having the smallest code amount can be selected with no or little deterioration of the substantial picture quality substantially.
[0023] Further, according to the fourth feature, the encode data can be reconstructed by the processing of assuming the high frequency coefficient which cannot be perceived based on the spatia-temporal visual property mode as 0, thereby the code amount of the encoded video signal is effectively reduced.
[0024] According to the fifth feature, the encode control processing information and the applied frame number information can be output to the decoder with ease and with no credibility damaged.
[0025] Further, according to the sixth feature, there can be configured such that deteriorated images are not displayed during slow motion playback or pause.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] FIG. 1 is a block diagram showing a schematic structure of one embodiment of the present invention;
[0027] FIG. 2 is an explanatory diagram of a 3D video signal;
[0028] FIG. 3 is an explanatory diagram showing a relationship between a spatio-temporal visual property model and encode control;
[0029] FIG. 4 is an explanatory diagram of a spatial visual property model;
[0030] FIG. 5 is an explanatory diagram of one specific example of the encode control;
[0031] FIG. 6 is a block diagram showing a structure of essential parts according to a third embodiment of the present invention;
[0032] FIG. 7 is a block diagram showing a structure of essential parts according to a fourth embodiment of the present invention;
[0033] FIG. 8 is a conceptual diagram showing an exemplary sequence format output from an encoder according to the present invention;
[0034] FIGS. 9A to 9C are explanatory diagrams showing positions in a header where encode control processing information and applied frame number information are inserted; and
[0035] FIG. 10 is a schematic block diagram of a decoder suitable for decoding a signal encoded by the encoder according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0036] The present invention will be described below in detail with reference to the drawings. FIG. 1 is a block diagram for explaining one embodiment of the present invention. An explanation will be made below by way of a H.264 encoder, but the present invention is not limited thereto and is applicable to encoders using other methods.
[0037] In FIG. 1 , it is assumed that an input video signal (I) is input to be encoded in units of frames into a code amount reducing apparatus 1 . The input video signal (I) is managed in an appropriate signal form, and frame numbers and/or pixel positions can be appropriately acquired at any stage in the system.
[0038] The input video signal (I) is first stored in a frame memory 10 in order of frame number such as F 1 , F 2 , . . . , F 7 . This is because information on frames before and after the frame to be encoded needs to be referred to in the later processings. Though a capacity of the frame memory 10 depends on the number of frames to be referred to in a 3D FFT (Fast Fourier Transform) 15 in the later stage, the memory 10 can store information for more than the number of frames to be referred to.
[0039] A frame delaying unit 11 delays the input video signal (I) for a time for storing the information required for the processing of the 3D FFT 15 in the frame memory 10 . For example, when the frame to be encoded is F 4 , the signal (I) is delayed for the time for storing the future frames F 5 to F 7 .
[0040] A sharp/blurred frame mode classifying unit 12 as target frame specifying means for specifying a frame to be processed classifies the frame F 4 to be encoded into either of sharp picture or blurred picture. It is preferable that an insertion ratio of the blurred frames into the sharp frames is such that the sharp frames and the blurred frames are repeated every frame for sharp/blurred playback, that is, at the ratio of 1:1, but the present invention is not limited thereto and may take an arbitrary ratio. The ratio of one blurred frame to two sharp frames or the ratio of one blurred frame to three sharp frames may be taken. Alternatively, the ratio may be decided according to the frame rate of the video signal. Actually, since as the frame rate is higher, the ratio of the number of blurred frames to the number of sharp frames can be increased more, there may be performed a processing of assuming 60 fps as one frame interval and, at a higher frame rate, increasing the ratio in proportion to the frame rate. The classification of sharp frame and blurred frame is made based on the frame numbers F. The sharp/blurred frame mode classifying unit 12 outputs a signal b (or binary signal 1) when the frame is classified as blurred and outputs nothing (or binary signal 0) when the frame is classified as sharp.
[0041] The sharp/blurred frame mode classifying unit 12 may also decide an interval between target frames according to a frame rate of the input signal.
[0042] When the frame is classified as blurred in the sharp/blurred frame mode classifying unit 12 , a switching unit 13 is powered on (closed) and the processings described later will be performed. On the other hand, when the frame is classified as sharp, the switching unit 13 remains off (opened). As a determination whether sharp/blurred playback is performed is done by an encode block, the subsequent processings will be performed in units of block.
[0043] A 3D video signal extracting unit 14 extracts block 3D picture information (c), i.e. a coefficient string, as shown in FIG. 2 from the frame memory 10 . In order to reflect the spatio-temporal property of the video, the encode blocks are extracted from the same positions of each frame of (N B +N F +1) frames made of the target frame F 4 , the past N B frames and the future N F frames. Assuming that the block to be processed is the block B 4 within the frame F 4 to be processed and its size is N X ×N y , the block 3D picture information (c) comprising N X ×N y ×(N B +N F +1) pixels is extracted. In the following, the block B 4 of N x ×N y pixels is called macro block.
[0044] Then, the 3D FFT 15 is applied to the block 3D picture information (c) to obtain a spatio-temporal frequency property (g). Typically, the result of the 3D FFT 15 shows the property (g) of FIGS. 3A and 3B without considering the folded part, and it can be shown as one straight line through the origin. The folded part surely occurs when the 3D FFT is performed, but its illustration is omitted from FIGS. 3A and 3B . A sign (h) in FIGS. 3A and 3B indicates a visual passband. A spatial frequency component outside the visual passband (h) of the spatia-temporal frequency property (g) is not perceptible by human eyes. The horizontal axis of FIG. 3A indicates the spatial frequency ω x and the longitudinal axis indicates the temporal frequency ω T . FIG. 3B three-dimensionally shows the relationship between ω x and ω T , where ω 0 indicates the spatial frequency in the vertical direction and ω 1 indicates the spatial frequency in the horizontal direction.
[0045] FIG. 4 shows a spatial visual property model 16 (see FIG. 1 ). Since the visual passband (h) has a human visual pass property that the passband in the spatial frequency direction is wider in a lower temporal frequency f (f 0 in FIG. 4 ) and is narrower as the temporal frequency is higher (f 0 →f 1 →f 2 in FIG. 4 ), the spatial visual property model is designed assuming that the model has a cone-like shape as shown in FIG. 4 . Since the specific frequency property depends on the resolution of a motion picture to be encoded and the sizes of display systems (monitor, projector), it is suitable that the model is separately designed. The cone of FIG. 4 indicates the visual passband (h) of FIG. 3 and means that the inside of the cone is the passband.
[0046] Turning to FIG. 1 , an intersection coordinate calculating unit 17 obtains the spatial frequency coordinate (ω 0 ′, ω 1 ′) at the intersection between the spatia-temporal frequency property (g) and the visual passband (h). In other words, as shown in FIG. 3B , the spatial frequency coordinate (ω 0 ′, ω 1 ′) at the intersection (g′) is obtained. The spatial frequency coordinate (ω 0 ′, ω 1 ′) indicates the spatial frequency at the boundary where human eyes cannot perceive.
[0047] The input video signal is input into an encoder 21 , (for example, a H.264 encoder) via the frame delaying unit 11 to be subjected to intra-encode (intra-prediction) or inter-encode (motion compensation). An encode coefficient (d) obtained by the intra-encode or inter-encode is divided into the sharp and blurred frames in a switching unit 22 which is switched by the sharp/blurred frame mode signal (b). As well known, the intra-encode and the inter-encode comprise a plurality of encode modes, respectively.
[0048] When the blurred frame mode, the encode coefficient (d) in each encode mode is transmitted to a coefficient cut processing unit 23 , while, when the sharp frame mode, the encode coefficient (d) is transmitted to a next processing unit as usual without any processing by the present invention. The coefficient cut processing unit 23 performs the processing in which the high frequency component of the encode coefficient (or conversion coefficient) of the macro block predictive error signal (called residue signal below) is cut according to the spatial frequency coordinate (ω 0 ′, ω 1 ′) found in the intersection coordinate calculating unit 17 .
[0049] In other words, in the coefficient cut processing unit 23 , the high frequency component not perceptible by human eyes is assumed as 0 according to the spatial frequency coordinate (ω 0 ′, ω 1 ′), and is removed from the components to be encoded. Consequently, the conversion coefficient having a higher frequency than the spatial frequency coordinate (ω 0 ′, ω 1 ′) does not need to be transmitted, thereby reducing the code amount.
[0050] There will be described below with reference to FIG. 5 one specific example of the processing of assuming the conversion coefficient of the macro block residue signal obtained by the intra-encode or inter-encode as 0 according to the spatial frequency coordinate (ω 0 ′, ω 1 ′). Assuming that the matrix of the orthogonal conversion coefficient of the residue signal is made in 4×4 size, M and N meeting the following equation (1) are found and the coefficients meeting m≧M and n≧N are assumed as zero for the index (m, n) of the orthogonal conversion coefficient.
[0000] ( M/ 4)π≦|ω 0 ′|<(( M+ 1)/π), ( N/ 4)π≦|ω 1 ′|<(( N+ 1)/π) (where, M, N=0, 1, 2, 3) (1)
[0051] For example, when the matrix in 4×4 size of the residue signal 30 is as shown in FIG. 5 and in the case of M=1 and N=2, a frequency component outside the frequency component at the position (1, 2) may be assumed as 0 as illustrated.
[0052] Reference numeral 51 in FIG. 1 indicates an encoder for an applied information of encode control and Reference numeral 52 indicates a muxer, and their functions will be described later.
[0053] A second embodiment of the present invention will be described below. As a result of the experiment of the present invention by the present inventors, it is found that even when the encode coefficient (d) or the residue signal is neglected (that is, not coded) for the macro block of the blurred frame subjected to the inter-encode in the encoder 21 of FIG. 1 , the picture quality is not largely influenced. Thus, it is found that it is suitable that the coefficient cut by the spatio-temporal frequency property (g) is applied only to the residue signal of the macro block subjected to the intra-encode of the blurred frame.
[0054] A third embodiment of the present invention will be described below with reference to FIG. 6 . The embodiment is such that a mode selecting unit 25 is added to the second embodiment thereby to select an encode mode having a small code amount. The same reference numerals are denoted to the blocks having the same or similar functions as those of FIG. 1 .
[0055] The input video signal (I) delayed in the frame delaying unit 11 of FIG. 1 , for example, is input into the encoder 21 of FIG. 6 . The switching unit 22 is controlled by the sharp/blurred frame mode classifying signal (b), is connected to one illustrated position for the blurred frame, and is connected to the other position for the sharp frame. The mode selecting unit 25 is input an intra-mode encode coefficient having the residue signal subjected to the code amount reduction processing in the coefficient cut processing unit 23 and an inter-mode encode coefficient for which a conversion coefficient value of the residue signal is assumed as 0 in a Not Coded unit 24 . The mode selecting unit 25 obtains the code amount of each encode coefficient in the intra-mode and the inter-mode, and selects the encode mode having the smallest code amount. On the other hand, the sharp frame encode coefficient is directly transmitted to the mode selecting unit 25 not via the coefficient cut processing unit 23 and the Not Coded unit 24 , and is subjected to the conventional mode selection processing. The mode selecting unit 25 can select the encode mode by a well-known rate distortion optimization processing, for example.
[0056] A fourth embodiment when an encoded video signal (I′) is input as the input video signal (I) will be described below with reference to FIG. 7 . The same reference numerals are denoted to the blocks having the same or similar functions as those of FIGS. 1 and 6 . The processings with numerals 15 to 17 of FIG. 1 are inserted at the dotted line between the 3D video signal extracting unit 14 and the coefficient cut processing unit 23 based on the visual property model in FIG. 7 , but an illustration thereof will be omitted for a simplified explanation.
[0057] When the encoded video signal (I′) is input, the encoded video signal (I′) is input into a decoder 31 , a MB (macro block) classifying unit 32 for odd-numbered frames and B pictures and an intra-/inter-deciding unit 33 . The decoder 31 decodes the encoded video signal (I′). The MB classifying unit 32 for odd-numbered frames and B pictures is means for specifying a frame and MB to be processed, i.e. a target frame and MB, and performs the similar processings to the sharp/blurred frame classifying unit 12 . Specifically, the MB classifying unit 32 detects the MB which is an odd-numbered frame and a B picture not referred to by other picture from the encoded video signal (I′), and powers on or closes the switching unit 13 on the detection. Thus, the 3D video signal extracting unit 14 extracts a 3D video signal made of the MB which is an odd-numbered frame and a B picture from the video signal decoded in the decoding unit 31 . The MB classifying unit 32 may also decide an interval between target frames according to a frame rate of the input signal. Thereafter, the 3D video signal passes the processings with numerals 15 to 17 of FIG. 1 , but the processings are the same as those of FIG. 1 and thus an explanation thereof will be omitted.
[0058] In the intra-/inter-deciding unit 33 , the encoded video signal (I′) is decided which of the intra-mode or the inter-mode is used for the encoding. In the case of the intra-mode, the MB which is an odd-numbered frame and a B picture is transmitted to the coefficient cut processing unit 23 which processes based on the visual property model, and the high frequency component of the residue signal is subjected to the cut processing. In the case of the inter-mode, the MB which is an odd-numbered frame and a B picture is transmitted to the Not Coded unit 24 and the conversion coefficient of the residue signal is set at 0. An encoded data reconstructing unit 34 reconstructs and outputs the encoded data of the encoded video signal (I′) based on the input result.
[0059] On the other hand, the intra- or inter-encoded video signal not corresponding to the MB which is an odd-numbered frame and a B picture is output as it is without being subjected to the coefficient cut processing or the processing by the Not Coded unit and without the reconstruction of the encoded data.
[0060] The functions of the encoder for the applied information of encode control 51 and the muxer 52 (see FIG. 1 ) will be described below in detail. The functions also are applicable to the embodiments in FIGS. 6 and 7 .
[0061] The encoder for the applied information of encode control 51 encodes (1) information on whether the sharp/blurred encode control processing is applied (which will be referred to as encode control processing information below) and (2) information on an applied frame number when the sharp/blurred encode control processing is applied. The encode control processing information and the applied frame number information can be acquired from the sharp/blurred frame mode classifying unit 12 . The encode control processing information and the applied frame number information, which are encoded in the encoder for the applied information of encode control 51 , are sent to the muxer 52 .
[0062] The muxer 52 contains the encoded encode control processing information and applied frame number information within a sequence in which image information to which the sharp/blurred encode control processing is applied is sent as a bit stream, and outputs the same. The encoded encode control processing information and applied frame number information also may be separately sent without being contained in the sequence.
[0063] Reference numeral 53 indicates an output signal of the muxer 52 . A specific example in which the encoded encode control processing information and applied frame number information are inserted into the sequence will be described with reference to FIG. 8 . FIG. 8 is a conceptual diagram of the sequence format, where the sequence is configured of a sequence header 53 a , a frame header 53 bn , and image data made of image data 53 cn (n=0, 1, 2, 3, . . . ). Herein, n indicates a frame number of an image signal. The encoded encode control processing information and applied frame number information can be inserted at position (p) of the sequence header 53 a or in the frame header 53 bn . The exemplary insertion will be described with reference to FIGS. 9A to 9C .
[0064] In FIG. 9A , the flag (f) of the encode control processing information, that is, the flag (f) indicating whether the sharp/blurred processing is applied, and a number string (r) (made of 0 or 1) indicating a sharp/blurred processed frame are contained at position (p) of the sequence header 53 a . In the number string (r), “1” indicates a sharp frame and “0” indicates a blurred frame. Reversely, “0” may indicate the sharp frame and “1” may indicate the blurred frame.
[0065] In FIG. 9B , the flag (f) of the encode control processing information, that is, the flag (f) indicating whether the sharp/blurred processing is applied, the first blurred applied frame number (s), and applied frame interval information (t) are contained at position (p) of the sequence header 53 a . In the illustrated example, since s=1 and t=2 are assumed, the first blurred applied frame is the first frame, and the blurred frame is subsequently applied per frame.
[0066] In FIG. 9C , the flag (f) indicating whether the corresponding frame is a blurred frame or a sharp frame is inserted in the frame header 53 bn . In the illustrated example, there is shown that the 0-th frame is a sharp frame (1), the first frame is a blurred frame (O), the second frame is a sharp frame (1), . . . .
[0067] One embodiment of a reproducing apparatus will be described below with reference to FIG. 10 . FIG. 10 is a schematic block diagram of the reproducing apparatus, where the reproducing apparatus has a playback control unit 61 , a displaying unit 62 and a demuxer 63 for separating multiplexed information.
[0068] The demuxer 63 is input multiplexed image information such as the output signal 53 . The demuxer 63 separates header information 64 and image data 65 from the multiplexed image information. A header data extracting unit 66 extracts the flag (f) of the encode control processing information and the applied frame number information at position (p) from the sequence header 53 a , and sends them to a decoder 67 . The decoder 67 decodes the flag (f) and the applied frame number information. An applied frame number signal (q 1 ) acquired by the decoding is sent to a first switching unit (SW 1 ). On the other hand, a frequency conversion coefficient of the image data 65 is extracted by a frequency conversion coefficient extracting unit 68 and is decoded by a decoder 69 .
[0069] Instruction signals (q 2 ) such as normal playback, slow motion playback and pause are output from a playback control unit 61 and sent to a second switching unit SW 2 . The second switching unit SW 2 selects contact (a) when the instruction signal (q 2 ) is for slow motion playback and pause, and selects contact (b) in other cases. The first switching unit SW 1 is turned off (open) when the applied frame number signal (q 1 ) is for a blurred frame, and turned on (close) when the applied frame number signal q 1 is for a sharp frame.
[0070] Thereby, when the second switching unit SW 2 is connected to contact (b) during normal playback, the decoded sharp and blurred frames are displayed on the displaying unit 62 . However, during slow motion playback or pause, since the second switching unit SW 2 is connected to contact (a) and the first switching unit SW 1 is turned off (open) or on (close) by the applied frame number signal (q 1 ) as described above, the blurred frame is skipped and is not displayed on the displaying unit 62 .
[0071] The first and second switching units SW 1 and SW 2 are merely exemplary for simplified explanation, and can be realized by a circuit, such as a logic circuit having a similar function to the switching units.
[0072] According to the embodiments, the blurred frames are not displayed on the displaying unit 62 during slow motion playback or pause, thereby preventing deteriorated images from being displayed.
[0073] The present invention has been described above using the preferred embodiments, but the present invention is not limited to the embodiments, and it is clear that various modifications may be made within the scope of the present invention. | A sharp/blurred frame mode classifying unit specifies a frame to be subjected to sharp or blurred process. A 3D video signal extracting unit extracts a predetermined area or predetermined macro block in the specified target frame, and a 3D FFT 15 frequency-converts it to acquire a coefficient string. An intersection coordinate calculating unit finds a non-perceptible high frequency coefficient based on a spatio-temporal visual property model for the coefficient string, and a coefficient cut processing unit cuts the non-perceptible high frequency coefficient for a frequency conversion coefficient of orthogonal conversion of a predictive error signal. The code amount of a video signal is largely reduced for a high frame rate video by the processings only at the encode side without deteriorating the picture quality. | 7 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an actuator powered apparatus that has application in assembly plants for clamping, welding and other assembly functions that are common in the manufacture and assembly of vehicles such as, for example, automobiles. More particularly, the invention is related to a dual action fluid powered apparatus that is equipped with two elongate arms that are spaced apart from one another. The elongate arms operate independently of one another. The elongate arms are positioned within a common housing that supports fluid drive cylinders that are attached to each elongate arm. In one embodiment, a rack gear and pinion gear arrangement is utilized to immobilize the elongate arms, thus, minimizing drift of the elongate arms because of an imbalance in forces applied to the elongate arms.
2. Description of the Prior Art
The prior art is replete with the utilization of single hydraulic and pneumatic cylinders in conjunction with mechanical devices. Many prior applications of fluid drive cylinders employ the telescoping variety when one cylinder acts within another cylinder to enhance a given force. Also, the prior art discloses a variety of devices that employ a rack and gear combination to change arcuate motion to a translatory function, or vice versa.
The present invention differs from the rack and pinion gear driven load grip device that is shown and described in U.S. Pat. No. 2,595,131, entitled "Load Grip Means for Trucks and the Like" issued Apr. 29, 1952, to Leslie G. Ehmann. FIG. 1 of the Ehmann patent depicts a pair of spaced apart cylinders 26 that are oriented parallel to one another. In cross-section, the cylinders are square in configuration and have a cylindrical bore located along the longitudinal axis of the cylinder. One of the four sides of each cylinder contains a rack gear. The rack gears of the cylinders mesh with the teeth of a pinion gear that is attached to a flange. Each one of the cylinders is powered by a piston that is connected to a piston rod. The piston and the piston rod are contained within the cylinder in the usual fashion, with only the end of the piston rod protruding from the cylinder. The ends of the piston rods are fixed, thus, when fluid pressure is applied to the piston head, the cylinder with its attached rack gear moves in a linear direction. The pinion gear is fixed against rotation by its attached flange. Consequently, when fluid pressure is applied to the piston heads, the rack gear containing cylinders walk around the teeth of the fixed pinion gear. In this manner, a torque is developed to rotate the entire plate to which the cylinders and their accompanying pistons are attached.
The present invention differs from the above described device in that the power generating fluid driven cylinders are separate from the rods or elongate arms that contain the rack gear teeth. Thus, any malfunction of the piston head, or its seals, does not affect the block assembly that houses the elongate arms. Then, too, the present invention provides elongate arms that can move independently of one another. In the previously discussed prior art device, the two arms are coupled together in a positive manner through the common pinion gear.
In U.S. Pat. No. 2,605,751, entitled "Fluid Pressure Tool Slide Control Assembly" issued Aug. 5, 1952, to Richard D. Perry et al, there is shown an apparatus for controlling the feed of a machine cutting tool. FIG. 3 of Perry et al shows a housing 11 that contains two piston chambers 19 and 20 that are in tandem. Each piston chamber 19 and 20 contains a piston head that is connected to a common piston rod 65. The smaller piston 63 is driven hydraulically with the fluid medium being oil. The oil can be metered very slowly to either side of the piston 19, providing for very slow axial movement of the piston rod. The larger piston 20 is driven pneumatically with the fluid medium being air. A cutting tool is responsive to the axial movement of the piston rod 65. The cutting tool can be moved into and out of engagement with a workpiece by utilizing air pressure on one side or the other of the piston 20. Incremental movement of the cutting tool is then achieved by metering oil to one side or the other of the piston 19. Thus, the tool is fed rapidly by the pneumatic cylinder from its rest position substantially into engagement with the workpiece and is then fed slowly at a rate determined by the setting of a throttling valve which forms a part of the hydraulic speed control.
The present invention differs from the above described cutting control for a tool in that two movable tool carrying elongate arms are in separate chambers, not in tandem as in the Perry et al reference. In one embodiment of the present invention, very precise control of the tool is achieved by means of a rack and gear arrangement.
SUMMARY OF THE PRESENT INVENTION
The present invention encompasses a dual action fluid actuated device for use in a variety of applications where a generally linear equal and opposite compressive or tensile force is applied to shape, form or hold a workpiece.
The invention includes a housing of elongate block configuration that contains two spaced apart elongate arm guides in the form of milled grooves. The elongate arm guides traverse the entire length of the housing and are open at their opposite ends. Each one of the elongate arm guides within the housing contains an elongate arm. One end of each elongate arm protrudes from the housing and is adapted for the attachment of a variety of tools that can be affixed thereto. Fluid driven cylinders are attached to the housing in line with each elongate arm. A cylinder rod extends from each fluid driven cylinder and is coupled to each elongate arm to control the linear motion thereof. An embodiment of the present invention utilizes a housing block that contains a pair of nonparallel grooves that permit the cantilevered ends of the elongate arms to converge on a small area of a workpiece. Then, too, the independent control and motion of each elongate arm increases the overall versatility of the apparatus. In another embodiment of the instant invention, the elongate arms are independently controlled for optimum movement and an additional feature is incorporated for precise control of the elongate arms. The control feature encompasses a rack gear and pinion gear concept. The elongate arms each contain a gear segment in the form of a rack gear that extends over a substantial portion of the longitudinal extent of the elongate arms. A pinion gear is mounted for rotation and translation within the housing block and is positioned intermediate the two elongate arm guides. The teeth of the pinion gear extend into each of the elongate arm guides within the housing block and mesh with the teeth of each elongate arm and rack gear. In addition, the pinion gear assembly can move longitudinally within the housing block. At any particular time, the pinion gear can undergo a state of rotation and translation. The translation of the pinion gear can be immobilized, providing a compensating lock and force equalizer to minimize the movement of the elongate arms when they are in contact with a workpiece.
A primary object of the present invention is to provide a force generating dual action apparatus with independently controlled arms that is accurate and can function with a variety of tools attached thereto.
Another object of the present invention is to provide an apparatus that uses a double rack and pinion gear to compensate for any unequal forces that may occur in the individual arms when in contact with a workpiece.
A further object of the present invention is to provide a force generating dual action apparatus that can be driven by different fluid mediums.
Another object of the present invention is to provide an apparatus that contains two elongated arms that move independently of each other yet are interconnected with one another.
Still another object of the present invention is to provide a tool carrying apparatus that contains a minimum of moving parts and seals.
A further object of the present invention is to reduce the work cycle time in that both elongate arms move tools or clamps simultaneously into and out of engagement with a workpiece.
Another object of the present invention is to eliminate the whipping or arcing movements associated with non-linear motion devices.
A further object of the present invention is to provide an apparatus having increased smoothness of performance without decreasing its overall accuracy.
Further objects and advantages of the present invention will become apparent from the following description and the appended claims, reference being made to the accompanying drawings forming a part of this specification, wherein like reference characters designate corresponding parts in the several views.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view that shows the dual action apparatus of the present invention;
FIG. 2 is a cross-sectional side view, showing the independently movable elongate arms and their position within the housing block;
FIG. 3 is a top plan view of the apparatus depicted in FIG. 2;
FIG. 4 is a cross-sectional view taken along section lines 4--4 of FIG. 2 that shows the coupling between the cylinder rod and the elongate arms;
FIG. 5 is a cross-sectional view taken along section lines 5--5 of FIG. 2 that shows the elongate arms within their respective arm guides and the cover plate that retains the arms;
FIG. 6 is a side view, partly in section, that shows an embodiment of the invention wherein the elongate arms are in nonparallel alignment with one another;
FIG. 7 is a fragmented, partly sectional side view of another embodiment of the invention that shows a rack and pinion gear coupled to the elongate arms; and
FIG. 8 is a side view that shows a cover plate with an electromagnetic lock in position against a slide bar that journals a pinion gear shaft.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings and more particularly to FIG. 1, there is illustrated in perspective a dual action apparatus indicated generally by the numeral 10 in the form of a tool adapted for a clamping function. The tool shown in FIG. 1 is adapted for a top support, such as suspension from a cable system. A side mount for a platform or pivotal mounting system is also shown.
With reference to FIG. 1, a housing block 12 of the overall apparatus 10 is shown in elongate form. The housing block 12 is of two part construction in that a milled portion 14 has attached thereto a cover plate 16 which is attached by a plurality of bolts 18. Top and bottom elongate arms 20 and 22 are positioned longitudinally within the housing block 12 and are spaced one from the other in generally parallel relationship. An end cap 24 not only prevents the ingress of contaminants, such as dirt, into the interior of the overall apparatus 10, but the end cap 24 also serves as a mounting plate for a power source, such as a pair of fluid actuated cylinders 26 and 28. The fluid actuated cylinders 26 and 28 contain respective flanges 30 and 32 that are bolted to the exterior of the end cap 24 by a series of bolts 34. The fluid actuated cylinder 26 has a plurality of fluid coupling ports 36 and 38 that permit the introduction of a fluid medium to both sides of a piston that is integral with the fluid actuated cylinder 26. In a similar manner, the fluid actuated cylinder 28 has a plurality of fluid coupling ports 40 and 42 that act as described above. The fluid actuated cylinders are also equipped with position sensors 44. Since the fluid actuated cylinders 26 and 28 must have communication with the interior of the housing block 12 apertures 46 and 48 are provided in the end cap 24, as shown in FIG. 2. A pivotal support member 50 is attached to each side of the housing block 12 by a plurality of bolts 52 to provide an alternate support system for the embodiment of the invention depicted in FIG. 1. Apertures 54 are provided in the top of the housing block 12 for mounting of the overall apparatus 10, if the particular application requires such suspension.
In FIG. 1, the top elongate arm 20 contains an attachment plate 56 attached to its free end. In a similar manner, an attachment plate 58 is attached to the free end of the bottom elongate arm 22. By way of illustration, a clamp bracket 60 is affixed to the attachment plate 56 at the end of the top elongate arm 20. A cushion pad 62 is attached to the end of the clamp bracket 60. In a similar manner, the bottom elongate arm 22 has attached at its free end a clamp bracket 64. A cushion pad 66 is attached to the clamp bracket 64 so that the cushion pad 66 is in axial alignment with the cushion pad 62. It is to be understood that other tool combinations can also be used in place of the clamping arrangement described above.
FIG. 2 is a cross-sectional side view of the overall apparatus that shows the arrangement of the elongate arms 20 and 22 and their independently connected fluid actuated cylinders 26 and 28. The milled portion 14 of the housing block 12 contains a top elongate arm guide or groove 68. The elongate arm 20 is positioned within the top elongate arm guide 68. The top elongate arm guide 68 extends from end to end of the milled portion 14 and has dimensional tolerances such that the top elongate arm 20 can slide freely therein. In a similar manner, the milled portion 14 of the housing block 12 contains a bottom elongate arm guide or groove 70 that extends over the longitudinal expanse of the milled portion 14 and is oriented generally parallel to the top elongate arm guide 68. The bottom elongate arm 22 is positioned in the bottom elongate arm guide 70. The bottom elongate arm 22 also slides freely within the confinement of the bottom elongate arm guide 70. Thus, the top and bottom elongate arm guides 68 and 70 provide independent guides for the elongate arms 20 and 22. The top and bottom elongate arms 20 and 22 are generally rectangular in cross-sectional configuration. The fluid actuated cylinders 26 and 28 are attached to the housing block 12 so that their longitudinal axes 72 and 74 coincide with the longitudinal axes of the top and bottom elongate arms 20 and 22. The fluid actuated cylinder 26 has a cylinder rod 76 that has attached thereto a fitment 78. The fitment 78 has a reduced section or neck 80 adjacent to an enlarged head 82 that is cylindrical in configuration. The actual coupling of the fitment 78 to the top elongate arm 20 will be discussed further hereinbelow. The bottom fluid actuated cylinder 28 has a cylinder rod 84, with a fitment attachment 86 attached thereto similar to the fitment 78. A neck section 88 and a head 90 are also a part of the fitment 86.
Attention is now directed toward the right-hand side of FIG. 2. The cantilevered end 92 of the top elongate arm 20 has the attachment plate 56 attached thereto by bolts 94. In a similar manner, the bottom elongate arm 22 has a cantilevered end 96 to which the attachment plate 58 is coupled by bolts 98. The cantilevered ends 92 and 96 of the respective top and bottom elongate arms 20 and 22 each have a collapsible shield 100 circumscribing their exposed ends. The shields 100 are attached to the attachment plates 56 and 58 as well as to the milled portion 14 of the housing block 12. The collapsible shields 100 are used to protect the surfaces of the top and bottom elongate arms 20 and 22 from particulate matter such as the airborne fallout from an adjacent welding operation.
In order to provide a positive stop for the top and bottom elongate arms 20 and 22, a stop block 102 is attached to the milled portion 14 by bolts (not shown). Thus, the stop block 102 serves to limit the retractable movement of both top and bottom elongate arms 20 and 22.
FIG. 3 is a top plan view of the overall apparatus 10 that is shown in FIG. 2. The position sensors 44 are shown at each end of the fluid actuated cylinder 26. The position sensors 44 are attached to the cylinder 26 by means of bolts 104. The series of apertures or tapped holes 54 are positioned in vertical alignment at each end of the housing block 12. The tapped holes 54 provide means for attaching a vertical lift mechanism, such as a cable sling or rigid arm, that would be utilized during production use of the overall apparatus 10.
FIG. 4 is a cross-sectional view taken along section lines 4--4 of FIG. 2 that shows the elongate arms 20 and 22 within their respective top and bottom elongate arm guides or grooves 68 and 70. The cover plate 16 is shown at the right-hand side of FIG. 4 where it is attached to the milled portion 14. The bottom elongate arm 22 is shown, in section, within the bottom elongate arm guide 70. Both the top and bottom elongate arms 20 and 22 are held captive within the top and bottom elongate arm guides 68 and 70 by means of the cover plate 16. However, the cover plate 16 does not interfere with the axially slidable feature of the top and bottom elongate arms 20 and 22. The end of the elongate arm 20 adjacent the fluid actuated cylinder 26 has a milled slot 106 that extends downward from a top surface 108 of the top elongate arm 20 to a position past the longitudinal axis 72. The head 82 of the fitment 78 fits into the slot 106 and is retained therein as described below with respect to the head 90. The bottom elongate arm 22 also has a milled slot 110 that extends downward from a top surface 112 of the bottom elongate arm 22 to a position past the longitudinal axis 74. The bottom of the milled slot 110 is undercut to provide a reentrant section 114. The reentrant section 114 provides a ledge for interaction with the head 90 of the fitment 86. This coupling arrangement provides for rapid connection of the fluid actuated cylinder 28 and its cylinder rod 84 to the end of the bottom elongate arm 22. As the bottom elongate arm 22 is moved to an extended position, the head 90 of the fitment 86 pushes against the end of the bottom elongate arm 22 in a positive manner. When the direction of motion of the bottom elongate arm 22 is reversed, or retracted, the enlarged head 90 of the fitment 86 engages the reentrant section 114 of the milled slot 110, thus providing a positive engagement. Thus, it becomes evident that the fitments 78 and 86 act as quick disconnect couplings.
FIG. 5 is a cross-sectional view taken along section lines 5--5 of FIG. 2 that shows the top and bottom elongate arms 20 and 22 in their respective top and bottom elongate arm guides 68 and 70. The milled portion 14 is shown with the top elongate arm guide 68 and the bottom elongate arm guide 70 milled therein. As previously pointed out, the top and bottom elongate arm guides 68 and 70 provide guides for the top and bottom elongate arms 20 and 22. A rib 116 remains within the milled portion 14 after the top and bottom elongate arm guides 68 and 70 have been milled. The rib 116 is continuous from end to end of the milled portion 14 in this particular embodiment of the present invention. The rib 116 provides extra rigidity for the overall apparatus.
FIG. 6 is a side view, partly in section, that shows an embodiment of the invention wherein the top and bottom elongate arms 20 and 22 are in nonparallel alignment with one another. The overall apparatus 10 has a housing block 118 that is of pentagonal configuration. The housing block 118 has a milled section 120 to which is attached a cover plate 122. The milled section 120 has a top groove 124 that is milled essentially parallel to a top surface 126 of the milled section 120. The top elongate arm 20 is positioned in the top groove 124 with its free or cantilevered end 128 extending from the housing block 118. An attachment plate 130 is attached by fasteners (not shown) to the cantilevered end 128 of the top elongate arm 20. A top end cap 132 is attached to a surface 134 of the milled section 120 by bolts (not shown). The top end cap 132 contains an aperture 135 therethrough for the installation of the fluid actuated cylinder 26. The fluid actuated cylinder 26 is attached to the top end cap 132 by appropriate fasteners. The cylinder rod 76 of the fluid actuated cylinder 26 is coupled to the end of the top elongate arm 20 as described above with reference to FIG. 2. The milled section 120 has a bottom groove 136 that is milled essentially parallel to a bottom surface 138 of the milled section 120. The bottom elongate arm 22 is positioned in the bottom groove 136 with its cantilevered end 140 extending from the housing block 118. An attachment plate 142 is attached to the cantilevered end 140 of the bottom elongate arm 22. A bottom end cap 144 is attached to the surface 146 of the milled section 120 by bolts (not shown). The bottom end cap 144 contains an aperture 148 therethrough for the installation of the fluid actuated cylinder 28. The fluid actuated cylinder 28 is attached to the bottom end cap 144 by fasteners (not shown). The cylinder rod 84 of the fluid actuated cylinder 28 is attached to the end of the bottom elongate arm 22 as has been previously described with respect to FIG. 2.
Attention s now directed to the right-hand area of FIG. 6. A top electrode holder 150 is attached to the attachment plate 130 by appropriate fasteners. A power source 152 is provided for the top electrode holder 150. A bottom electrode holder 154 is attached to the attachment plate 142 by suitable fasteners. A power source 156 is connected to the bottom electrode holder 154. Electrodes 158 and 160 are shown in the respective top and bottom electrode holders 150 and 154. The electrodes 158 and 160 are shown in close proximity to a weld nut 162 that is positioned in contact with a workpiece 164. The angular disposition of the top and bottom elongate arms 20 and 22 and the electrodes 158 and 160 carried thereby permit advantageous placing of the electrical energy to secure an adequate coupling of the weld nut 162 to the workpiece 164.
FIG. 7 is a fragmented, partly sectioned, side view of another embodiment of the present invention that shows a rack and pinion gear braking system coupled to the top and bottom elongate arms 20 and 22. The milled section 120 of the housing block 118 contains the top elongate arm guide 68. The top elongate arm 20 is positioned within the top elongate arm guide 68. The top elongate arm guide 68 extends from end to end of the milled section 120 and has dimensional tolerances such that the top elongate arm 20 can slide freely therein. In a similar manner, the housing block 118 contains the bottom elongate arm guide 70 that extends over the longitudinal expanse of the milled section 120 and is oriented generally parallel to the top elongate arm guide 68. The bottom elongate arm 22 is positioned in the bottom elongate arm guide 70. The bottom elongate arm 22 also slides freely within the confinement of the bottom elongate arm guide 70. Thus, the top and bottom elongate arm guides 68 and 70 provide guides for the top and bottom elongate arms 20 and 22.
The top elongate arm 20 is generally rectangular in cross-sectional configuration. One side of the top elongate arm 20 contains an array of teeth 166 in the form of a rack gear 168. In a similar manner, the bottom elongate arm 22 also contains an array of teeth 170 in the form of a rack gear 172. The rack gears 168 and 172 are opposed to one another in spaced apart relationship. An elongate cavity 174 is milled in the milled section 120. The cavity 174 extends between web blocks 176 and 178. A pinion gear 180 is positioned within the cavity 174. The pinion gear 180 is contained on a pinion shaft 182 that is journaled within slide blocks 184. The pinion gear 180 preferably rotates freely about the pinion shaft 182. The one slide block 184 slides in a milled slot 186 that is within the cover plate 122. The other slide block 184 slides within a similar milled slot (not shown) that is in the sidewall of the milled section 120. The pinion gear 180 is equipped with an arcuate array of teeth 188 that circumscribes the pinion gear 180. The teeth 188 of the pinion gear 180 are meshed with the teeth 166 and 17) of the respective top and bottom elongate arms 20 and 22. The external su-faces of the slide blocks 184 are flush with the external surface of the cover plate 122 and the external surface of the milled section 120.
The interconnection between the fluid actuated cylinders 26 and 28 and their corresponding top and bottom elongate arms 20 and 22 have been described previously.
FIG. 8 is a side view that shows the cover plate 122 with the milled slot 186 cut therethrough. The slide block 184 and the end of the pinion shaft 182 are also shown. An electromagnetic clutch 190 is attached by fasteners 192 to the slide block 184 so that, during its non-energized state, it slides freely with the slide block 184. The electromagnetic clutch is equipped with an electrical source 194 so that it can be energized to immobilize it against the sidewall of the cover plate 122. When the electromagnetic clutch is immobilized, it prevents the slide block 184, to which it is attached, from moving. Likewise, the pinion shaft 182 and the journaled pinion gear 180 are stopped from translating.
ASSEMBLY AND OPERATION
The assembly of the overall apparatus 10 of the present invention is fairly simple which is an asset when repairs are necessary. The top elongate arm 20 and the fluid actuated cylinder 26 are coupled by installing the head 82 of the fitment 78 into engagement with the milled slot 106. The top elongate arm 20 is then inserted into the top elongate arm guide 68 and the flange 30 of the fluid actuated cylinder 26 is attached to the end cap 24 by means of the bolts 25. In a similar procedure, the bottom elongate arm 22 and the fluid actuated cylinder 28 are pre-assembled and then inserted into the bottom elongate arm guide 70 of the milled portion 14. The cover plate 16 is then secured to the milled portion 14 by the bolts 18. The protective shields 100 are then telescoped over each of the cantilevered ends 92 and 96 of the top and bottom elongate arms 20 and 22. The attachment plates 56 and 58 are then anchored to the ends of the top and bottom elongate arms 20 and 22 by the bolts 94 and 98. The shields 100 are held in place by fasteners (not shown).
In the embodiment shown in FIG. 7, after the actuator arm subassemblies have been installed in the respective top and bottom guides, the pinion gear subassembly is then assembled. The pinion gear 180 is attached to the pinion shaft 182 by friction fit or by a key. The slide blocks 184 are then attached to each end of the pinion shaft. The pinion gear subassembly is then inserted into the cavity 174 and the rear slide block 184 is engaged in the milled slot 186 that is located in the milled section 120. The pinion gear 180 is then positioned so that it is in alignment with the center of the teeth 166 and 170 of the rack gears 168 and 172. The teeth 188 of the pinion gear 180 are then meshed with the teeth 166 and 170. The front slide block 184 is then placed in axial alignment with the housing block 118 and the cover plate 122 is installed so that the front slide block 184 is engaged in the milled slot 186 that is contained in the cover plate 122. The cover plate 122 is then secured to the milled section 120 by means of the bolts 18. Appropriate shields over the cantilevered ends 92 and 96 of the top and bottom elongate arms 20 and 22 are installed, if required, and the attachment plates 56 and 58 are attached by the bolts 94 and 98.
During the operation of the overall apparatus 10, with the illustrative clamp arrangement shown in FIG. 1, the top elongate arm 20 is moved to an extended position as shown in FIGS. 2 and 3. The movement of the top elongate arm 20 is achieved by the introduction of a fluid medium, such as air or oil, through the fluid coupling port 36. This, of course, creates a desirable pressure behind the piston head within the fluid actuated cylinder 26. The pressure created by the ingress of a fluid medium behind the piston within the fluid actuated cylinder 26 causes an extension of the cylinder rod 76. As the cylinder rod 76 moves to an extended position, the top elongate arm 20 also moves until it reaches its maximum extent as depicted in FIGS. 2 and 3. The top elongate arm 20 can move from the fully extended position to a retracted position 196 as shown in FIG. 2. The bottom elongate arm 22 has the same degree of linear motion as has been described above. The bottom elongate arm 22 can move from a fully retracted position to a fully extended position 198 as shown in FIG. 2.
The particular array of tools, such as clamp brackets 60 and 64, as shown in FIG. 1, permit the clamping of, for example, the interior of a structural channel section. A wide variety of additional tools can be utilized with the overall apparatus 10 since both tensile and compressive grasping can be attained through the independently controlled top and bottom elongate arms 20 and 22.
In the embodiment shown in FIG. 6, the assembly of the overall apparatus 10 is essentially the same as has been described. In the operation of the overall assembly of FIG. 6, the versatility of independently controlled elongate arms is used. Also, the nonparallel orientation of the top and bottom elongate arms 20 and 22 permits the attached tools to move into a position unattainable by a strictly parallel elongate arm arrangement. While an electrode arrangement has been shown in FIG. 6, it is to be understood that other tools can be employed equally as well.
Another embodiment of the present invention is shown in FIGS. 7 and 8. In this embodiment, the precise positioning of the top and bottom elongate arms 20 and 22 is controlled. As has been previously mentioned, each elongate arm has an independent linear motion achieved through the action of separate fluid actuators, such as 26 and 28. Because of fluctuations in the fluid medium supply to the fluid actuated cylinders 26 and 28, it is possible that one fluid actuator may overpower the other, thus causing the clamped workpiece to drift or translate. The particular embodiment of the present invention, as shown in FIGS. 7 and 8, makes it possible to minimize any drift that may be caused by a fluid medium imbalance to the independently controlled fluid actuated cylinders 26 and 28.
As shown in FIG. 7, each top and bottom elongate arm 20 and 22 has independent linear motion because of their attachment to separate fluid actuated cylinders 26 and 28. For example, when the top elongate arm 20 is moved to the right, as viewed in FIG. 7, the pinion gear 180, which is engaged with the rack gear 168, will rotate and move or translate also to the right. The pinion gear 180 can translate because its pinion shaft is journaled in slide blocks 184 which, in turn, slide along the milled slot 186 in the cover plate 122 and the corresponding milled slot in the milled section 120. Thus, the top elongate arm 20 can move linearly without any undue force being applied to the bottom elongate arm 22. In a similar manner, the bottom elongate arm 22 can move linearly without affecting the position of the top elongate arm 20. In both of the above examples, the pinion gear 180 mere-y rotates and translates to the right or to the left depending upon which direction the elongate arm is moved. Both the top and bottom elongate arms 20 and 22 can be moved simultaneously, if desired. When both of the top and bottom elongate arms 20 and 22 are moved to the right, as viewed in FIG. 7, under the influence of their respective fluid actuated cylinders 26 and 28, the pinion gear 180 translates, but does not rotate. Once again, the pinion gear 180 can translate because the journaled ends of the pinion shaft 182 are not restrained. Thus, as described above, the pinion gear 180 undergoes a combination of rotation and translation. By way of example, when the overall apparatus 10 employs a set of clamp tools that are clamped on a workpiece, there may be a slight drift of the workpiece in one direction or the other caused by an inbalance in fluid pressure that is being applied to the fluid actuated cylinders 26 and 28. To prevent the objectionable translation of the workpiece, the slide blocks 184 are immobilized by the clamping action afforded by the electromagnetic clutch 190. When the pinion gear 180 can no longer translate, any inbalance force that is being applied to one of the top and bottom elongate arms 20 and 22 will be immediately transferred in part to the other elongate arm, thus preventing drift or translation of the workpiece. While an electromagnetic clutch has been set forth by way of example, those skilled in the art will immediately recognize alternate modes for immobilizing the slide blocks 184 with respect to the milled slot 186.
While the illustrative embodiments of the present invention have been described in considerable detail for the purpose of setting forth practical operative structures whereby the invention may be practiced, it is to be understood that the particular apparatus described is intended to be illustrative only, and that the various novel characteristics of the invention may be incorporated in other structural forms without departing from the spirit and scope of the invention defined in the appended claims. | An apparatus for providing a reciprocating motion. The apparatus has a housing block that contains two movable arms in spaced apart relationship to one another. The movable arms are each controlled by independently attached fluid driven actuator cylinders that are mounted externally of the housing block. Tools for the altering of a workpiece may be attached to one or both ends of the movable arms. An embodiment utilizes a rack and pinion gear arrangement to immobilize any imbalance in forces that may exist when the movable arms are biased against a workpiece. | 1 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Reference is made to International Application No. PCT/EP2015/064282 filed Jun. 24, 2015 and French Application No. 14/57,141 filed Jul. 24, 2014, which are hereby incorporated herein by reference in their entirety.
BACKGROUND OF THE INVENTION
[0002] Field of the Invention
[0003] This invention relates to a device for controlling the quantity of air introduced into the inlet of a boosted internal combustion engine, particularly a stationary engine or one for a motor vehicle or commercial vehicle and a method of controlling the quantity of air for such an engine.
[0004] Description of the Prior Art
[0005] As is widely known, the power delivered by an internal combustion engine is dependent on the quantity of air introduced into the engine's combustion chamber which is proportional to the density of this air.
[0006] Therefore, it is customary to increase this quantity of air by compressing external air before it is let into this combustion chamber. This operation, which is called boosting, can be carried out by any means, such as a turbocharger or a mechanically driven compressor, which may be centrifugal or of the positive-displacement type.
[0007] In the case of boosting by a turbocharger, the latter comprises a single flow or double flow rotary turbine, connected by a shaft to a rotary compressor. The exhaust gases coming from the engine pass through the turbine which is then rotatingly driven. This rotation is then transmitted to the compressor which, by its very rotation, compresses the external air before it is introduced into the combustion chamber.
[0008] As is better described in French patent application 2 478 736, in order to significantly increase this quantity of compressed air in the engine combustion chamber, it is intended to increase the compression of external air by the compressor further still.
[0009] This is effected more particularly by increasing the speed of rotation of the turbine and therefore of the compressor.
[0010] For this, a portion of the compressed air coming out of the compressor is diverted to be let directly into the turbine intake to mix with the exhaust gases. This turbine is then crossed by a greater quantity of fluid (a mixture of compressed air and exhaust gas), whereby the speed of rotation of the turbine and consequently of the compressor can be increased. Therefore, with this compressor speed increase, it is possible to increase the pressure of the external air which will be compressed in this compressor and then introduced into the engine combustion chamber.
[0011] Due to this, the compressed air is of a higher density whereby the quantity of air contained by the combustion chamber can be increased.
[0012] This type of boosted engine, although satisfactory, nevertheless has some significant drawbacks.
[0013] In fact, if the flow rate of the compressed air which is let into the turbine intake is not correctly controlled, this may lead to an engine malfunction.
[0014] Therefore, by way of example, in the event of too great a quantity of compressed air being diverted to the turbine intake, the exhaust gases entering the turbine are cooled too much by this air and bring about a reduction in the overall performance of the boosting.
SUMMARY OF THE INVENTION
[0015] The present invention rectifies the aforementioned drawbacks by means of a device for controlling the quantity of air introduced into the intake of a boosted internal combustion engine with which it is possible to respond to all the engine's power requirements.
[0016] With the invention it is also possible to carry out a transfer of compressed air from the inlet to the exhaust even when the mean pressure of the compressed air in the inlet is lower than that of the gases in the exhaust. It is simply sufficient that there are phases during the engine operation cycle where the pressure in the inlet is higher than that in the exhaust.
[0017] To this end, the present invention is to a device for controlling the quantity of air introduced into the inlet of a boosted internal combustion engine. The engine comprises two exhaust gas outlets with outlet being each connected to an exhaust manifold of at least one cylinder. The invention comprises a boosting device with a turbocharger comprising a double intake turbine connected to the exhaust gas outlets as well as an external-air compressor and a duct for partial transfer of the compressed air from the compressor to the turbine intakes wherein the partial transfer duct comprises two branches connected to the turbine intakes which each carry a valve regulator controlling the circulation of the compressed air in these branches.
[0018] Advantageously, the branches can each also carry a non-return valve.
[0019] One of the branches can be connected to the other branch with a connecting line.
[0020] The connecting line can carry valve regulation.
[0021] The valve regulation can comprise proportional valves.
[0022] The transfer duct can carry heating for the compressed air circulating therein.
[0023] The heating can comprise a heat exchanger.
[0024] The heat exchanger can comprise an intake for exhaust gas coming from the turbocharger turbine and an exhaust gas outlet to the exhaust line.
[0025] The invention also relates to a method of controlling the quantity of compressed air in the inlet of a boosted internal combustion engine. The engine comprises two exhaust gas outlets with each outlet being connected to an exhaust manifold of a at least one cylinder. The invention comprises a boosting device with a turbocharger with a double intake turbine connected to the exhaust gas outlets as well as an external-air compressor and a duct for partial transfer of the compressed air from the compressor to the turbine intakes, wherein a portion of the compressed air is introduced from the compressor into the turbine's exhaust gas intake sections.
[0026] The method can divide the transfer duct into two branches and can controlling the circulation of the compressed air in each of the branches with valve regulation means.
[0027] The method can connecting one of the branches to the other branch with a connecting line.
[0028] The method can consist of heating the compressed air circulating in the transfer duct before intake into the turbine.
BRIEF DESCRIPTION OF THE DRAWINGS
[0029] The other features and benefits of the invention will appear from reading the description which is to follow, given for solely illustrative purposes and on a non-limiting basis and to which the following are attached:
[0030] FIG. 1 illustrates an internal combustion engine with a boosting device according to the invention;
[0031] FIG. 2 shows a variant of the internal combustion engine with its boosting device and
[0032] FIG. 3 illustrates a variant of the internal combustion engine with its boosting device according to FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
[0033] In FIG. 1 , the internal combustion engine 10 comprises at least two cylinders, which here are four cylinders referenced 12 1 to 12 4 from the left of the figure.
[0034] Preferably, this engine is a direct injection internal combustion engine, particularly of the Diesel type but this in no way excludes any other type of internal combustion engine.
[0035] Each cylinder comprises an inlet means 14 or inlet with at least one inlet valve 16 . Here two inlet valves each controlling an induction pipe 18 . The induction pipes 18 end at an inlet manifold 20 supplied by a supply duct 22 with inlet air, such as compressed air.
[0036] This cylinder also comprises burned gas exhaust means 24 or exhaust with at least one exhaust valve 26 . Here two valves, control an exhaust tube or lines 28 .
[0037] In the example illustrated, the engine is prepared for operating with a firing order of 1-3-4-2. In view of this firing order, the exhaust tubes or lines of the first cylinder 12 1 and second cylinder 12 4 , which form a first unit of at least one cylinder, are connected to a first exhaust manifold 30 with a first exhaust gas outlet 32 . The exhaust tubes or lines of the third and fourth cylinders 12 2 and 12 3 , which form a second unit of at least one cylinder, are connected to a second exhaust manifold 34 which comprises a second exhaust gas outlet 36 .
[0038] The two exhaust gas outlets lead to a turbocharger 38 for compressing air and more particularly to the expansion turbine 40 of this turbocharger.
[0039] As illustrated in FIG. 1 , the turbocharger is a double intake turbocharger, better known by the term “Twin Scroll” turbocharger.
[0040] This type of turbocharger comprises the expansion turbine 40 which is swept by the exhaust gases and rotatingly connected, by a shaft 42 , to a compressor 44 .
[0041] At the turbine, the exhaust gas intake is divided into two sections. A first intake section 46 is connected to the first exhaust gas outlet 32 of the first manifold 30 and a second intake section 48 is connected to the second exhaust gas outlet 36 of the second exhaust manifold 34 .
[0042] The gas discharge 50 of the turbine 40 is conventionally connected to the engine's exhaust line 52 .
[0043] The compressor 44 of the turbocharger 38 comprises an external-air inlet 54 supplied by a supply duct 56 . This compressor's compressed air outlet 58 is connected to the supply duct 22 of the inlet manifold 20 by a duct 60 .
[0044] Advantageously, it can be arranged to place a compressed air cooler 62 on the duct 60 , between the compressor and the duct 22 .
[0045] As can be seen better in FIG. 1 , with a transfer duct 64 , a portion of the compressed air coming out of the compressor 44 can be made to circulate to the turbine intakes 46 and 48 .
[0046] More precisely, this partial transfer duct starts in the duct 60 , at an intersection point 66 between the compressor and the cooler 62 and is then divided, from a bifurcation point 68 , into two branches 70 and 72 . The branch 70 leads to the turbine intake 46 via its connection to the first exhaust gas outlet 32 and the branch 72 leads to this turbine's other intake 48 via its connection to the exhaust gas outlet 36 .
[0047] Each branch carries valve regulation means of regulation 74 and 76 , such as a proportional valve, controlled by a control means 78 , which can be common to the two valve regulation means. Therefore, with this valve, the circulation of the compressed air in the branch can be controlled.
[0048] Advantageously, each branch also comprises a non-return valve 80 and 82 which prevents the circulation of the compressed air from the branch to the compressor, while preventing the two branches from coming into communication.
[0049] Therefore, with this configuration, it is possible during operation of the engine to take advantage of the zones of low exhaust pressure prevailing intermittently in the exhaust manifolds to introduce compressed air into the turbine and thus to increase the flow rate of this turbine and consequently of the compressor. With this, it is also possible to have more efficient boosting for low engine speeds.
[0050] During operation, in case of a requirement for air in a large quantity in the cylinders, the valves 74 and 76 are made to open to introduce compressed air from the compressor 44 into the turbine 40 .
[0051] The compressed air coming from the compressor 44 circulates in the duct 64 and then in the branches 70 and 72 to reach the exhaust gas intakes 46 and 48 of the turbine 40 , delivering surplus fluid to this turbine.
[0052] Therefore, the turbine is swept not only by the exhaust gases from the outlets 32 and 36 but also by compressed air which is added to these gases. Because of this, turbine rotation is increased, which causes an increase in compressor rotation and consequently an increase in the pressure of the compressed air which comes from this compressor.
[0053] Of course, the valves 74 and 76 are controlled by the control means or control 78 so as to let into the turbine the quantity of compressed air which meets the engine's boosting requirements.
[0054] The variant in FIG. 2 can be distinguished from FIG. 1 due to the placing of a connecting duct 84 between the two branches 70 and 72 . This duct is provided with a regulation valve means or regulation 86 , such as a proportional valve which, here, is also controlled by the control means or control 78 .
[0055] One of the ends of this duct is connected to the branch 70 at a point situated between the valve 74 and the exhaust gas outlet 32 and the other end is connected at a point situated between the valve 76 and the exhaust gas outlet 36 .
[0056] With this duct, it is possible to control the communication of fluid between the two branches reaching the turbine.
[0057] More precisely, with this connecting duct, it is possible to divert a portion of the compressed air circulating in one of the branches to introduce it into the other branch, mixing with the exhaust gases at the intakes of the turbine 40 .
[0058] Furthermore, with the connecting duct, it is possible to restore in one branch of the turbine the pressure differential of the exhaust gases (or pulsating exhaust) of the other branch which is angularly offset in the engine combustion cycle.
[0059] In FIG. 3 , which essentially comprises the same elements as those in FIG. 1 , the compressed air leaving the compressor 44 and circulating in the transfer duct 64 is heated before being introduced into the turbine 40 .
[0060] For this purpose, the transfer duct 64 carries a means of heater 88 for heating the compressed air, which here is a heat exchanger in the form of a heat radiator, placed between the intersection point 66 and the bifurcation point 68 of the duct. This radiator is crossed by the compressed air which circulates in this duct while being swept by the engine exhaust gases. These exhaust gases come from the turbine discharge 50 and are conveyed by a duct 90 to the radiator intake 92 . The exhaust gases sweep this radiator, transferring the heat they contain to the compressed air, subsequently to leave this radiator again through the outlet 94 , to be directed to the engine exhaust line.
[0061] Therefore, a portion of the exhaust gas energy is recovered by the compressed air which is introduced into the turbine through one or other of the intakes 46 and 48 .
[0062] Therefore, with this heated compressed air, it is possible to supply extra energy to the turbine which, as a result, will rotate at a higher speed. This high speed of rotation is then transmitted to the compressor, which will carry out higher compression of external air. | The present invention is a device for controlling a quantity of air introduced into an inlet of a boosted internal combustion engine with the engine having exhaust gas outlets each connected to an exhaust manifold of at least one cylinder. The device includes a boosting device comprising a turbocharger having a turbine with intakes connected to the exhaust gas outlets, an external-air compressor and a duct for partially transferring the compressed air from the compressor to the intakes. The partial transfer duct has branches connected to the turbine intakes which each have valve regulation for controlling circulation of compressed air in the branches. | 5 |
FIELD OF THE INVENTION
The present invention is directed to coating valve metal powder with polypropylene carbonate as a binder/lubricant and use of the coated valve metal powder in manufacturing powder metallurgy compacts such as capacitor anodes.
BACKGROUND OF THE INVENTION
During the past several decades, the use of capacitors formed using valve metal powders has grown exponentially. This increase is mainly due to a large growth in the use of solid tantalum capacitors. Solid tantalum capacitor use has increased due to their high reliability, high capacitance per unit volume, and wide variety of surface-mount configurations available.
Also contributing to the popularity of solid tantalum capacitors is the continuing decrease in cost per unit capacitance for these devices. The reduction in the cost per unit capacitance is, in part, the result of the increasing economy of scale. As ever greater numbers of the devices are manufactured ever more quickly, the fixed costs per capacitor are reduced, thereby fueling the market for these devices. Another very important factor in the continuation of cost reduction for solid tantalum capacitors is the availability of finer, higher surface area tantalum powders. The use of tantalum powders, having greater surface area per unit weight, allows the use of less tantalum powder per device, thereby facilitating a savings in the “contained tantalum” component of device cost.
Unfortunately, as tantalum capacitor powders having higher surface areas per unit weight have come into use, several disadvantages of these finer (i.e. smaller particle size) powders have become apparent. Finer powders exhibit less-than-ideal flow characteristics during the anode pressing process. The generally slower and less even flow characteristics of finer tantalum powders results in less uniform anode weights unless slower machine speeds are employed; this, in turn, makes the anode fabrication process less efficient as fewer parts are produced per unit of time.
The finest particles present in higher surface area capacitor powders tend to become airborne readily during processing on anode presses, necessitating expensive explosion-resistant high air flow rate exhaust systems to prevent injury to workers and to reduce the fire/explosion hazard from airborne dust. The dust from high surface area capacitor powders has also proven to be highly abrasive in contact with the dies, punches, sliding, and rotary bearing surfaces of anode pressing equipment. The presence of the fine dust from high surface area tantalum powders requires the use of more precise punch and die tolerances, cemented carbide tooling in place of hardened steel, and frequent bearing replacement, all of which add to the cost of capacitor anode fabrication with these powders.
The simple expedient of employing a powdered binder/lubricant material, such as ethylene diamine bis d-stearamide (sold under the tradename of “Acrawax”, by the Lonza Corporation) in mechanical mixture with the higher surface area capacitor powders imparts lubricity to these powders, minimizing anode press repairs due to wear, but results in very little improvement in flow properties or fine dust generation.
The coating of fine capacitor powders with binder/lubricant via tumbling the powders in a solution of the binder/lubricant (such as a solution of the binder, stearic acid, dissolved in one or more chlorinated solvents and/or acetone), followed by dynamic vacuum-drying of the binder-coated capacitor powder in a Patterson-Kelly V-shell type blender results in a reduction of fine powder dust generation, as well as improved pressing equipment lubrication, but does not address powder flow considerations.
An additional problem is observed with high surface area capacitor powders, such as tantalum having a surface area above about 0.3 square meter per gram, which is that traditional binder/lubricant materials become increasingly more difficult to remove completely. Tantalum powders having a surface area of 0.4-0.5 square meter per gram, mixed with 1% to 5% stearic acid or ACRAWAX (with or without the use of a solvent) and pressed into 0.1 gram anode pellets are frequently found to contain 300 to 400 ppm carbon after a thermal binder removal step in vacuum and 150 to 200+ ppm carbon following the vacuum sintering step used to produce the finished anode bodies prior to electroprocessing (anodizing, counter-electrode fabrication, and encapsulation). The level of carbon remaining in the anode bodies after vacuum-sintering is proportionally higher with progressively finer capacitor powders and larger anode size.
The presence of carbon on the valve metal surfaces within the interstices of the anodes after vacuum sintering leads to the production of anodic oxide having flaws or high electrical leakage regions. These flaws are thought to be due to the presence of spots of tantalum carbide on tantalum anode surfaces; the tantalum carbide is thought to give rise to holes or thin spots in the tantalum oxide film which conduct electricity under the application of voltage (this leakage current mechanism is discussed in Young's 1961 book, Anodic Oxide Films, in the chapters dealing with tantalum). Whatever the mechanism, the correlation between elevated levels of carbon in anodes after vacuum sintering and high finished device leakage currents has been empirically established for many years.
SUMMARY OF THE INVENTION
The present invention is directed to a high surface area valve metal powders coated with polypropylene carbonate by tumbling the valve metal powder in a solution of polypropylene carbonate in a suitable solvent, such as acetone, and then statically drying the coated powder. The polypropylene carbonate behaves as a binder/lubricant in the manufacture of powder metallurgy capacitor anodes.
The present invention is further directed to a method of preparing powder metallurgy anodes with compacted coated valve metal powder wherein the coated valve metal powder is prepared by tumbling the valve metal powder in a solution of polypropylene carbonate in a suitable solvent and statically drying the coated powder.
DETAILED DESCRIPTION OF THE INVENTION
It is known to coat valve metal powders such as tantalum powders with polypropylene carbonate and then dry the coated powder using dynamic means, e.g. tumbling in a drier. It was discovered that coating the valve metal powders, in particular tantalum powders, with polypropylene carbonate and then drying the coated powder using static means produces a coated product having better properties. Specifically, the method of drying the polypropylene carbonate-coated valve metal has an unexpected and profound effect upon the suitability of the powder for capacitor anode fabricator.
Valve metal powders coated with polypropylene carbonate using the static drying method of the present invention have higher flow rates and reduced fine dust generation than uncoated powder or powder coated and dynamically dried. This allows the use of higher valve metal capacitor body pressing rates, as well as a reduction in the rate of wear of press components, thereby reducing the cost of anode fabrication. Thus, the polypropylene carbonate-coated powder, prepared in accordance with the invention, is lubricious toward anode press components due to the lubricity of the polymer and the relative absence of “fines” in the powder.
In accordance with the invention, a high surface area valve metal powder is coated with polypropylene carbonate by tumbling the powder in a solution of polypropylene carbonate in a suitable solvent. Then, the coated is dried using static means.
The valve metal powder may be any suitable valve metal powder used in the preparation of powder metallurgy compacts. Such valve metal powders include, but are not limited to, tantalum and niobium powders. Preferably the valve metal powder is tantalum. There is not limit as to the particle size of the powders that can be used in this invention, however the method of the invention is particularly more effective than the prior art in lowering residual carbon levels using particles less than 1 micron.
The polypropylene carbonate is dissolved in a suitable solvent such as, but not limited to, 1,1,1 trichloroethane, acetone, and suitable mixtures thereof. The concentration of the polypropylene carbonate may be any suitable concentration and is typically about 0.5% to about 25%, preferably about 1% to about 10% based on the total weight of solution. The polypropylene carbonate content may also be measured based on the weight of the valve metal employed and is typically between about 0.1% to about 10%, preferably about 0.25% to about 5% based upon the weight of the valve metal.
The polypropylene carbonate may be obtained from any suitable source, such as from PAC Polymers under the name Q-PAC. Polypropylene carbonate thermally decomposes at approximately 250° C. to yield propylene carbonate, propylene oxide, and carbon dioxide, all of which are volatile in vacuum at this temperature. The 250° C. decomposition point of the polymer lies below the temperature range above which high surface area tantalum powders exhibit high reactivity with carbonaceous materials (i.e., above about 280° C. to 300° C.). Polypropylene carbonate was first synthesized by Inoue, et.al. In the late 1960's (U.S. Pat. No. 3,585,168). The technology was expanded by the Air Products Corp. (U.S. Pat. No. 4,665,136) and is described at some length in the Q-PAC binders bulletin which is put out by the Air Products Corp.
The high surface area valve metal powder is coated with polypropylene carbonate by tumbling the tantalum powder with a room temperature solution of polypropylene carbonate. Room temperature means temperatures between about 15° C. and about 30° C., preferably about 20° C.
Thereafter, the coated powder is statically dried to produce a semi-solid caked material. Statically dried means that the powder is not tumbled, agitated, shaken, or the like during drying. Instead the powder is placed on a surface and is allowed to dry simply by allowing the solvent to evaporate. Note that the surface the powder is placed on can move, e.g. a moving belt, but the particles remain static on the surface.
For example, the wet coated material is disposed on a slowly moving conveyor belt or rotating plate dryer and removed incrementally as the residual solvent is reduced to a suitably low level. This produces a more or less continuous but effectively static drying process (i.e., the valve metal powder is not agitated during the drying process). The semi-solid caked material is then sieved through a suitable screen. The screen size is between about 20 and about 50 mesh, preferably about 35 mesh. A preferred screen is stainless steel.
The temperature of the static drying is about 10° C. to about 100° C., preferably about 20° C. to about 30° C.. Preferably no heat is applied to the powder. Instead the drying is achieved by exposing the powder to ambient air.
The use of polypropylene carbonate has been found to give rise to post vacuum sintering residual carbon levels of below 150 ppm for 0.1 gram anodes fabricated from 0.4 to 0.5 square meter per gram tantalum powders. This residual carbon level is unexpectedly lower than the residual carbon level achieved when using traditional binders such as ACRAWAX C.
EXAMPLE
Approximately 10 pounds of Cabot, C-410 tantalum powder was coated with 2% polypropylene carbonate (based upon the weight of the tantalum) by tumbling the tantalum powder with the appropriate amount of a 10 wt. % solution of polypropylene carbonate in acetone. The powder was then dynamically dried (i.e., tumbled during drying) in a Patterson-Kelly V-shell blender, under vacuum to give Sample A.
Approximately 5 pounds of sample A was re-wet with acetone (approximately half as much as was used to wet the original 10 pounds of tantalum powder) with tumbling. The acetone-wet, polypropylene carbonate-coated tantalum was then placed in a pan to dry under a draft of air. The evaporation of the solvent left a semi-solid cake which was manually sieved through a 35 mesh, stainless steel screen, forming Sample B. A comparison of the properties of the two samples of tantalum powder, which contain the same amount of the same binder (polypropylene carbonate) is given in Table 1. Particle size was determined using an LA900 Horiba laser diffraction particle size analyzer.
TABLE 1
% of Particles
Hall Flow Test
<1.0 micron
Median Particle Size
Sample A
(no flow)
6.6%
30.3 microns
Sample B
1.56 gm/sec
0.9%
106.2 microns
Thus the Sample B binder-coated tantalum powder exhibited much-improved flow performance compared with the sample A powder. Although not wishing to be limited by any theory, it appears that this is due to the larger median particle size of the tantalum/binder agglomerates formed with static drying followed by screening as compared with dynamic drying.
The much reduced fines (<1.0 micron) content of the static-dried and sieved binder-coated tantalum powder was observed to give rise to significantly lower dust generation during the anode pressing process.
Subsequent batches that were simply wet once with polypropylene carbonate in acetone that were then statically dried performed in a manner similar to Sample B.
It will be apparent to those skilled in the art that various modifications and variations can be made in the compositions and methods of the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. | The application of polypropylene carbonate in solution to valve metal powders having relatively high surface area, then evaporating the solvent under static (non-agitating) conditions. The static drying of the coated valve metal powder produces a semi-solid cake which may be converted into a free-flowing powder via screening. Valve metal powders so-coated with polypropylene carbonate are particularly well-suited for the fabrication of powder metallurgy anode bodies used for the manufacture of electrolytic capacitors. | 1 |
BACKGROUND OF THE INVENTION
The invention relates to a method for operation of a safety-oriented control system with a plurality of centralized and/or decentralized stations provided with inputs and/or outputs and exchanging information with each other via a bus line, and to a safety-oriented control system for performance of the method.
A control system for interlinking of subsystems in motor vehicles is known from a specialist essay by J. U. Pehrs et al. “ Das sichere Buskonzept ” (the safe bus concept) in ELEKTRONIK, 17/1991, pp. 96-100. Here safety-relevant information such as braking, steering and engine data are transmitted to a central unit and processed there. The control system is designed as a bus system, with all the stations of the bus having a programmable control unit in the microcomputer with an integrated CAN controller. The task of the microcomputer with integrated CAN controller is to control bus line faults. By these are understood short-circuits or breaks in the bus line which impair or prevent communication of the nodes of the network.
The system described is designed exclusively for the recognition of bus faults in the event of short-circuits or breaks. It does not provide any indication of how the information such as such as braking, steering and engine data are processed within the microcomputer or how the data are exchanged between the stations of the bus with a central unit.
EP 0 732 657 A1 describes a method for fault-tolerant communication under high real-time conditions. The communication takes place in a local network, with a double bus architecture being used for fault reporting and for toleration of global bus faults. In one of the redundant bus systems all process data are transmitted in fault-free operation, and status information in the other bus system. The double-bus architecture does however involve greater assembly work and cost expenditure.
Also known from the prior art are control systems designed as bus systems. On the one hand, the bus systems are designed as so-called “master/slave systems”, with a centralized station as the “master” and decentralized stations as the “slaves”. In this case, the slaves are connected for example to signal transmitters and/or actuators whose states are transmitted via a bus line to the master. The control linkage of the input signals to corresponding output signals is performed in the centralized master, which in turn has outputs or controls decentralized outputs in order to operate a control-engineering facility.
On the other hand, “multi-master systems” are also known in which both centralized and decentralized stations are designed as masters. In this case, the control linkage of the input signals to corresponding output signals in the decentralized stations takes place with one or more masters. It is also possible to assign higher-order coordinating control functions to a centralized master station.
The bus systems described are not however safety-oriented systems. For the transmission of safety signals, only buses or bus systems that are fault-tolerating or fault-controlling can be used, e.g. of redundant design. Safety signals are those for safety purposes or duties for preventing or rapidly rectifying dangerous states for personnel or damage to plant equipment. A redundant bus system meeting the safety requirements comprises for example two identical bus systems that both evaluate the safety signals and check them for identity using a fail-safe comparator. In a bus system of this type, faults are detected by the evaluation. In the event of a fault, i.e. in the event of differences in the evaluated states, a system shutdown takes place, as a result of which machinery, production plant etc. is brought to a state which poses no risks to personnel or plant parts. The differences must be detected within a fault reaction time of—for example—20 msecs and also lead within this time to an emergency shutdown of the electrical equipment, this emergency shutdown corresponding to a safety-oriented control command.
A completely duplicated bus design requires not only a duplicated two-channel design of the bus modules for the sensors and actuators and two bus masters for system monitoring and fail-safe shutdown, but also the laying of two independent cabling systems.
The signal processing in safety circuits as a rule comprises the functions “signal transmission”, “signal linking/signal evaluation” and “processing to a control command”.
The functions “signal linking/signal evaluation” and “processing to a control command” of a safety circuit are traditionally of centralized design here. For example, the signal linking/signal evaluation and the processing to a control command for emergency-off command devices, locking devices for movable protective equipment etc. is performed centrally in one or—for larger machines, production systems or in complex facilities—several switchgear cabinets.
Here all input signals from the safety circuit are first transmitted, linked and processed to control commands regardless of the type of transmission, said control commands then having to be decentralized again in order to shut down a drive unit, for example, that powers a dangerous movement.
On that basis, the problem underlying the present invention is to develop a safety-oriented control system such that the reaction times of the control system to fault signals and input signals are shortened.
The problem is solved in accordance with the invention in that a message content in the form of logic links between inputs and outputs of the respective station is filed in at least one decentralized and/or at least one centralized station and in that a comparison is made between the message content and a data block transmitted via the bus line and having a message content and an action is activated when a predetermined pattern is obtained between the message content of the data block and the filed message content.
In processes in which a CPU such as a microcomputer is involved, the interaction of computer power and program size is crucial for the reaction speed of the overall system. If for example the state of an input of a station is inquired, the next inquiry would only be made in the next run of the program, as a result each input in the system is inquired after each cycle time of a program run. In safety-oriented systems, logic linkages are generally assigned to certain inputs and in turn act on outputs that trigger a safety shutdown. The reaction time of the system corresponds to the time from actuation of a switching element leading to a input state change, to switching of the respective output.
To achieve a minimization of the reaction time in the event of a requirement, it is necessary that the outputs within a bus system initiate an independent shutdown without the shutdown of a higher-order control system being initiated. The outputs react directly and independently to safety-relevant state changes effected at the bus by input state changes. The direct reaction of the outputs is preferably to state changes which would lead to shutdown of the releases.
SUMMARY OF THE INVENTION
For this reason, it is provided that the programmable control unit is coupled to the bus line via a coupling element such as a CAN controller, where the programmable control unit is assigned a memory element with information or message contents for activating outputs and/or inputs, and where at least one input and/or output can be activated depending on a comparison of the information filed in the memory element with the in formation transmitted to the bus.
To make this possible, the respective stations are informed before system commissioning of the bus to which message contents or information which release, i.e. which output, is to be switched off. As a result, there are in the memories of the respective output station tables containing the message contents that are to lead to shutdown of the respective releases. Of course the memories can also contain information for the switching on of outputs. The function of the higher-order control remains intact. Only an additional shutdown path/switch-on path is integrated into the system.
The method is performed by a control system characterized in that at least one of the decentralized stations has independent devices for fault-tolerating and/or fault-controlling self-monitoring to ensure normal operation for linkage and evaluation of signals located at the inputs and outputs of this station or further stations, and devices for processing of said signals and for generation of independent control commands, in that the independent device is coupled via a coupling element to the bus line, in that the independent device has a memory element for a message content in the form of logic links between inputs and outputs of the respective station and in that the independent device has a comparator for performing a comparison between the message content and a data block transmitted via the bus line.
In other words, a safety-oriented control system is achieved that comprises a plurality of decentralized input and output stations or combination input/output stations. The stations are in each case so designed that the function “signal linking/signal evaluation” and/or the function “processing to a control command” can take place decentrally. The stations can here—depending on their design—be provided as built-in switchgear cabinet devices or as field-suitable stations. In contrast with control systems according to the prior art, where signal linkage and processing to a control command takes place in centralized safety control devices accommodated in one or more switchgear cabinets, in the safety-oriented control system in accordance with the invention decentralization of the generated control commands is not necessary. To that extent, functions such as self-diagnosis, monitoring and the control functions mentioned above can be performed decentrally. A particular advantage to be mentioned here is that the transmission medium arranged between the stations is relieved of superfluous data transfer.
Centralized functions are reduced to a minimum, i.e. this function is used only for programming or parameterization of the system, for system administration (e.g. how many and which stations are connected to the system), for safety-oriented monitoring of the bus line, and for a higher-order safety function when interdependent input and output information sets are separated from one another spatially, i.e. in two different stations.
A higher-order centralized station as bus-master station can here assume pure monitoring functions, and in the event of a fault transmit shutdown signals to the decentralized master stations and/or to connected devices.
In a preferred embodiment, it is provided that the stations have a redundant design with two independent and galvanically isolated part-systems/nodes or channels. In a further preferred embodiment, it is provided that the redundant part-systems each have independent software packages with differing program structure for performance of the same computation. The redundant hardware design of the stations ensures that in the event of a danger-involving failure or disruption in one of the channels involved the other channel(s) can continue to maintain the safety function.
The hardware-based and/or software-based multi-channel feature is furthermore used to ascertain whether one of the channels involved is defective, by comparison of the desired valency or antivalency of the channels with one another. If the comparison shows a difference, a predetermined fault-controlling and/or fault-tolerating response of the system follows. In the case of a fault-controlling failure response, which is preferred in particular for the safety of machines and machine controls, shutdown is preferred in the event of a fault. With a fault-tolerating failure response, which is preferably used in aircraft, transport systems and process technology installations, non-shutdown is preferred in the event of a fault.
Furthermore, both safety-oriented fault-controlling operating methods and safety-oriented fault-tolerating methods are possible. Here “safety-oriented fault-controlling” relative to the requirements placed on the safety of machines and machine controls means that depending on a risk assessment a distinction is made between different control categories. In the case of a safety-oriented fault-tolerating mode of operation, a fault in any part of the safety-oriented control system does not also entail loss of the safety function, although the occurrence of the fault must not lead to shutdown of the system, instead the function of the other channels is sustained.
To design the “control engineering intelligence”, it is provided that at least one of the decentralized stations has at least one programmable control unit such as a microcomputer that assumes the functions of signal transmission, signal reception and evaluation as well as processing of the signals to control signals. In the case of two-channel stations, one programmable control unit is provided per channel.
The centralized and/or decentralized stations are preferably linked to one another by a bus line such as a CAN bus line, with this bus being designed as a line and extending between a bus start station (central station) and a bus end station (dezentral station), and with further dezentralized stations having a bus input and a bus output being incorporated into the bus line. It is provided here that the stations exchange information with one another, where one station provides the bus with information on the basis of a state change to the input, which is read and evaluated by at least one further station and where the stations perform independently assigned control functions depending on the information received. As a result a decentralized intelligent control system is provided in which all bus stations can locally perform self-diagnostic, monitoring and control functions in decentralized form.
In a further advantageous embodiment, the bus start station can be designed as a master station that assumes higher-order bus control functions.
Particularly advantageous is that signals are exchanged between the intelligent bus start station and the bus end station in order to detect faults of the bus line.
It is furthermore preferably provided that the bus line has a total of four conductors, two of which are used for power supply and two others for data transmission.
Particularly advantageous is also that the stations are supplied with AC voltage, with each channel of a station being assigned a separate power pack.
Each power pack here has its own transformer, so that the two channels are operated with isolated potentials.
At least one of the stations, preferably the bus start station (master station), is connected to an external isolation transformer for generating the supply AC voltage. The supply AC voltage is in the range from 20 to 50 V AC, preferably 42 V AC.
For mutual checking of the channels or nodes, the programmable control units assigned to the channels, such as microcomputers, are serially linked to one another via a galvanically isolated interface.
For communication with a higher-order control unit, at least one station has a serial interface such as an RS 232 or CAN interface. For programming of the system, at least one station has a further interface such as an RS 232 interface.
It is also provided that at least the bus start station (master station) and at least the bus end station each have units for generating preferably periodic bus messages or bus signals and devices for receiving bus messages or bus signals, with a safety-oriented control command being generated within a certain period if there are no bus messages.
In order to achieve an immediate bus shutdown in the event of a fault, the microcomputers of a station are each connected to an electromechanical switching unit such as a relay to perform a higher-order shutdown function.
BRIEF DESCRIPTION OF THE DRAWINGS
Further details, advantages and features of the invention are shown in the following description of a preferred embodiment shown in the drawings.
In the drawing,
FIG. 1 shows the design principle of a safety bus system,
FIG. 2 shows the design principle of a master station with two channels,
FIG. 3 shows a circuit design of a first channel of the master station according to FIG. 2 ,
FIG. 4 shows the design principle of an input and/or output station,
FIG. 5 shows the design principle of a bus end station,
FIG. 6 shows a circuit design of a safety circuit,
FIG. 7 shows a bus output station with external wiring,
FIG. 8 shows a current path of the bus output station with external wiring according to FIG. 7 ,
FIG. 9 shows a bus input station with external wiring,
FIG. 10 shows a current path of the bus input station with external wiring according to FIG. 9 ,
FIG. 11 shows an input and/or output station with external wiring using the example of a door monitoring station,
FIGS. 12-15 shows views of programming masks, and
FIG. 17 shows the logic structure of a shutdown table.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a safety-oriented control system 10 which in the design example shown here is designed as a line-like bus system. The bus system has a plurality of interconnected centralized and/or decentralized stations 12 , 14 , 16 , 18 , 20 provided with inputs and/or outputs. Here the first station 12 is designed as a bus start station or bus master with a bus connection 22 , and a last station 20 is designed as a bus end station with a bus input 24 . The further stations 14 , 16 , 18 have a bus input 26 , 28 , 30 respectively and a bus output 32 , 34 , 36 respectively. A single-channel bus line 38 , 40 , 42 , 44 is arranged between a bus output 22 , 32 , 34 , 36 of a bus station and a bus input 26 , 28 , 30 respectively. In this way, the bus system 10 can have a line with up to 64 stations.
The transmission medium or the single-channel bus line 38 , 40 , 42 , 44 comprises a data line 46 and an power supply line 48 . Here both the data line and the power supply line are here designed with two conductors.
For power supply, the bus master 12 is connected via a power line 50 to a transformer 52 which in turn is connected to mains voltage and provides a safe-to-touch supply AC voltage of preferably 42 V AC. Both the data line 46 and the power supply line 48 are internally incorporated through inside the stations having the bus inputs and outputs 26 , 32 ; 28 , 34 ; 30 , 36 . As a general principle, each station 12 , 14 , 16 , 18 , 20 of the bus system 10 has two part-systems or nodes A, B independent of one another and referred to in the following as channel A and channel B. With the two-channel design, a redundant system is achieved. Here each channel A, B within the station 12 - 20 has the possibility of independently accessing the bus 38 - 44 . In other words, each channel A, B works independently to the multi-master principle. As a general rule, the stations 12 - 20 have a substantially identical hardware structure.
FIG. 2 shows the design of the bus master 12 . The channels A and B each have a power pack 54 , 56 connected on the input side to the power line 50 . A first output 58 , 60 of the power pack 54 , 56 is connected to a programmable control unit 62 , 64 such as a microcomputer. The microcomputers 62 , 64 are connected via lines 66 , 68 to bus controllers 70 , 72 that are connected via further lines 74 , 76 with bus couplers 78 , 80 to the bus data line 46 . The bus couplers 78 , 80 have a separate voltage supply and are connected to a second output 82 , 84 of the power pack 54 , 56 .
Via a connecting line or link 86 between the microcomputers 62 , 64 a data exchange takes place between the channels A and B for mutual checking. This is a galvanically decoupled serial interface. Furthermore, serial interfaces 88 , 90 such as RS 232 or CAN interfaces are provided in the microcomputers 62 , 64 and are connected via a connecting line with an output plane 92 or the channel B and an output plane 94 of the channel A in order to provide a connection to an external programming unit such as a personal computer for programming of the bus system. It is also possible to provide other interfaces for coupling to other bus planes. The output planes 92 , 94 each have up to eight semiconductor outputs.
FIG. 3 shows in detail a circuit design of channel A of the master station 12 according to FIG. 2 . Here channel A has a circuit layout per se typical for the prior art. The power pack 56 comprises two transformers 96 , 98 whose primary windings 100 , 102 on the primary side are connected in series to supply voltage. The transformers 96 , 98 have a secondary winding 104 , 106 respectively which via a rectifier 108 , 110 and a voltage regulator 112 , 114 respectively provide a regulated output voltage for the microcomputer 64 or for the bus coupler 80 . The microcomputer 64 furthermore has external memory modules 116 , 118 such as RAM and ROM and a watchdog 120 . The two microcomputers 62 , 64 of the master station 12 can access the bus 38 , 40 , 42 , 44 independently of one another via the bus coupler 78 , 80 respectively. A data exchange for checking purposes is possible via the link 86 . The connection is optoelectronically decoupled.
The mains voltage of U N =230 V AC is transformed to a supply voltage of U V =42 V AC by the centralized power transformer 52 . The supply voltage U V is applied to the input of the power pack 54 , 56 and is connected to the input windings of the transformers 96 , 98 . A voltage of approx. 8 V AC is connected to the output windings 104 , 106 and is limited by the rectifier 108 , 110 and assigned voltage regulators 112 , 114 respectively to approx. 5 V. The voltage is monitored using the watchdog 120 .
The ROM module 118 is used for storage of the firmware. The ROM module 118 is designed as an EPROM and is cyclically checked with the aid of a 16 bit check sum formation (CRC check). User-specific data are stored in a flash-EPROM. The flash-EPROM is programmed via the serial interface 90 . The user data can be transferred with the aid of a switch and various saving mechanisms. The flash-EPROM is checked with the aid of the CRC check described above.
The external RAM 116 is provided additionally to a processor-internal RAM. This RAM module 116 incorporates a real time clock (RTC). An external RAM is also provided for the microcomputer 62 , albeit without RTC.
FIG. 4 shows as an example the layout of one of the stations 14 , 16 , 18 . The stations 14 , 16 , 18 have substantially the same internal structure as that of the master station 12 . A main difference is in the provision of an input and/or output plane 124 . In this way, the bus stations can be designed as bus output stations with up to eight semiconductor outputs or as bus input stations with semiconductor inputs to which one to four emergency-off switches or optionally one to eight control devices such as locking or unlocking devices are connected. The contact elements are attached to a terminal and internally—separated by optocouplers—connected to the inputs of the two microcomputer systems. For checking the lines for short-circuit, the lines are periodically subjected to signals for testing.
FIG. 5 shows a layout of the bus end station 20 . Unlike in the bus stations 14 , 16 , 18 , the bus end station has only the bus input 24 and no further bus output. The bus end station 20 can also have inputs and/or outputs 126 , 128 . The technical function of the bus end station 30 is explained later on.
FIG. 6 shows as an example a circuit design of the output plane 92 , 94 of channels A, B of bus master 12 . Here the output plane 94 of channel A comprises a plurality of NPN transistors T 1 -T 4 connected on the emitter side via resistors R 1 -R 4 to reference potential. On the collector side the transistors T 1 -T 4 are connected via two series-connected N/O contacts 130 , 132 to positive operating voltage U B .
The output plane 92 of the channel B has a plurality of PNP transistors T 5 -T 8 that are connected to one another on the emitter side and connected to negative operating voltage U B , via two series-connected N/O contacts 134 , 136 . On the collector side the transistors T 5 -T 8 are connected via resistors R 5 -R 8 to reference potential. For control of the transistors T 1 to T 4 the microcomputer 90 has outputs 138 that are connected to a base of the transistors T 1 -T 4 preferably by optocouplers. The microcomputer 62 too has corresponding outputs 140 with which the transistors T 5 -T 8 can be controlled. For monitoring of the switching functions of the transistors T 1 -T 4 on the one hand and of the transistors T 5 -T 8 on the other hand, the microcomputer 64 has inputs 142 connected to outputs E 1 -E 4 of the transistors T 5 -T 8 . The same applies for the microcomputer 62 , which has inputs 144 connected to outputs E 5 -E 8 of transistors T 1 -T 4 . All connections between the microcomputers 64 , 62 are preferably galvanically isolated via optocouplers (not shown).
Furthermore, the circuit comprises two relays 146 , 148 , where the relay 146 is connected by a first connection to an output 150 of the microcomputer 64 and by a second connection to an input 152 of the microcomputer 62 . Accordingly, the relay 148 is connected by a first connection to an output 154 of the microcomputer 62 and by a second connection to an input 156 of the microcomputer 64 .
The output 158 of the output plane 94 is connected to a winding 160 of an electromechanical switching element such as a motor contactor, which in turn is connected by a further connection to the output 162 of the output plane 92 . If due to control commands of the microcomputers 62 , 64 the transistors T 1 and T 5 are switched to conducting and if the relays 146 , 148 have picked up, the motor contactor 160 is provided with current and picks up.
To ensure dependable operation of this circuit array, the relays 146 , 148 are designed as positively-driven relays that at the moment of switch-on are electrically interlocked with one another in a time window. The relays 146 , 148 are directly controlled via a transistor by a microcomputer 62 , 64 respectively. The connection of the relay contacts 130 , 132 , 134 , 136 of the positively-driven relays 146 , 148 corresponds to a “reliable comparator”.
Of course it is also possible for further stations 14 , 16 , 18 to have outputs for control of various actuators. It is provided here that each output station 122 , 124 has eight N-switching and eight P-switching transistors.
FIG. 7 shows a corresponding bus output station 14 which is optionally connected to an external consumer 164 in single-channel design or where two consumers 166 , 168 form a redundant connection.
With the single-channel connection method, the electrical consumer 164 is connected by its first connection to an output of a transistor of channel A and by a second connection to an output of a transistor of channel B. The first connection of the consumer 164 is connected to positive operating voltage via the transistor of the channel A and the N/O contacts 130 , 132 , and a second connection of the consumer 164 is connected to negative operating voltage via the transistor of the channel A, B and further N/O contacts 134 , 136 .
With the redundant embodiment of the consumer, the first consumer 166 is connected by a first connection to positive operating voltage and by a second connection via a transistor of channel B to negative operating voltage. By contrast, the second consumer 168 is connected by one connection to negative operating voltage and by a further connection via a transistor of channel A to positive operating voltage.
To describe in principle the function of the circuits in accordance with FIGS. 6 and 7 , a current path is shown in FIG. 8 . With the single-channel operating mode, the consumer 164 is connect ed by a first connection 182 via a terminal 184 to a collector 186 of the transistor TOA. Its emitter is connected via the N/O contacts 174 , 176 to positive potential of the operating voltage.
A second connection 190 of the consumer 164 is connected via a terminal 192 to a collector 194 of the NPR transistor TOB. An emitter 196 of the transistor TOB is connected via the N/O contacts 178 , 180 to the reference potential of the operating voltage.
As already set forth in respect of FIG. 6 , a first connection 198 of the relay 170 is controlled via an optocoupler 200 by an output of the microcomputer of channel A. A further connection 202 of the relay 170 is connected via an optocoupler 204 to an output of the microcomputer of the channel B. A base 206 of the transistor TOA is connected via an optocoupler 208 to an output of the microcomputer of channel A. For checking or monitoring of the output 184 or of the function of the transistor TOA, the collector 186 is connected to an output of the microcomputer of channel B via an optocoupler 210 for read back.
The same applies for the output plane of channel B. Here the output 192 or the collector 194 is connected via an optocoupler 212 to an output of the microcomputer of channel A for readback. The transistor TOB is controlled via an optocoupler 214 and an output of the microcomputer of channel B. The relay 172 is also connected by a first connection 216 via an optocoupler 218 to a positive output of the microcomputer of channel B and by a second connection 220 and an optocoupler 222 to a negative output of the microcomputer of channel A.
After each channel A, B has performed a self-test after switch-on, the relays 10 , 172 are controlled by the microcomputers of channel A and channel B. The N/O contacts 176 - 180 switch the externally applied voltage through to the not yet actuated output transistors TOA, TOB. If a release signal is given by both microcomputers of channel A, channel B, the transistors TOA, TOB are also activated and the current path for the externally connected consumer 164 is closed.
In operation, the outputs 184 , 192 are tested by the microcomputer of channel A briefly switching off the associated output transistor TOA. The time of the short-term shutdown must be shorter than the reaction time of the connected consumer, in order to avoid any reaction to the brief current interruption. Via the readback path 210 the microcomputer of channel B receives the information on whether the output transistor TOA has really fulfilled its function. If it has not correctly fulfilled this function, the microcomputer of channel B would force its higher-order safety relay 172 to shut down.
By shutdown of the relay 172 , the relay 170 is electrically interlocked. In addition, a data exchange takes place by means of the switching behavior of the output transistors TOA, TOB via the transmission line 86 or “link” arranged between the microcomputers. These data are hence processed in parallel by two processors. The test function is then initialized by the microcomputer of channel B, where the checking function in this case is with the microcomputer of channel A.
FIG. 9 shows an external wiring of a bus input station 14 , 16 , 18 . The bus input station has a hardware layout substantially corresponding to that of the master station 12 . With the exception of the serial interface 88 , 90 and the additional ROM module 116 , the bus input station has microcomputers 62 , 64 connected to one another via the link 86 , also bus controllers 70 , 72 and power packs 54 , 56 .
On the input side, both two-channel control devices 224 and emergency-off switches or single-channel control devices 226 such as start buttons can be connected.
The function of the circuit array is to be set forth on the basis of FIG. 10 . Here the emergency-off switch 224 is connected using a first connection 226 and via an input terminal 228 on the one hand via an optocoupler 230 to an input of the microcomputer μP 1 and on the other hand via an optocoupler 232 to an input of the microcomputer μP 2 . A further connection 234 of the emergency-off switch configuration is connected via an input terminal 236 to an optocoupler 238 that in turn is connected to an output of the microcomputer μP 2 . The optocoupler 238 has a transistor output that is connected via a further transistor output 240 of an optocoupler 242 to operating voltage. The transistor output 240 is controllable via an output of the microcomputer μP 1 .
The function of read-in is set forth in FIG. 10 . The inputs 230 , 232 are reading inputs of the respective microcomputer μP 1 , μP 2 . The outputs 242 , 238 are writing outputs of the respective microcomputer μP 1 , μP 2 . For the optocouplers 230 , 232 to be activated, the outputs of the microcomputers μP 1 and μP 2 must be set to actuate the optocouplers 242 , 238 , so that positive potential is applied at the output 236 . If the microcomputer μP 1 interrupts the current flow with the help of its output, the inputs of the microcomputers μP 1 and μP 2 must change their status. This also applies when microcomputer μP 2 interrupts the current flow for testing.
In addition, a data exchange takes place via the link 86 to ascertain whether the respective input has fulfilled its function. If the control device 224 is actuated during testing, this information is made available to the first channel by a second channel of the switch 224 and the test is confined to the homogeneous state of the channels. This function is only active during testing. With the principle of input testing, a cross-wise test comparison is to be created for the input information.
Furthermore signal paths are shown in FIG. 9 that represent a short-circuit test of the inputs. All inputs are here reset briefly one after the other for <1 ms, with the respective input having to retain its status within this period of resetting for an output.
FIG. 11 shows a combination of bus output station and bus input station. The testing methods correspond to those of the respective individual stations explained with reference to FIGS. 6 to 10 . In the design example shown here, a locking device with lock feature 244 is connected to the bus station 14 , 16 , 18 and has both active elements such as coils 246 and passive switching elements such as door/magnet contacts 248 , 249 . The active elements 246 are controlled via transistor stages, with the passive elements 248 , 250 being inquired and monitored by optocouplers. In addition, it is possible using a transformer (not shown) integrated in this station to provide an AC voltage for actuation of the electrical consumer such as door magnet 146 . Here too the specific advantage of supplying the individual stations with AC voltage becomes clear: on the one hand electrical consumers with DC voltage can be used by insertion of a simple rectifier with downstream smoothing or regulation, and on the other hand the voltage supply to AC voltage consumers is assured in simple fashion.
In particular it should be pointed out that the hardware is designed to avoid faults wherever possible. For this reason, two independent channels or function units A and B were integrated into each of stations 12 - 20 for performance of specified functions. The channels A and B are equally, i.e. homogeneously, redundant. The signals used or generated by both channels are continuously compared with one another for the purposes of fault recognition (comparison of relevant input and/or output signals). In this connection, the higher-order relay plane (fail-safe comparisons) explained in FIG. 6 , the internal mutual comparison via the link 86 , and an external comparison of the input data by the user should be pointed out in particular.
The RAM module 116 is tested with the aid of a software test, whereas testing of the ROM module 118 is limited to the signature formation of both modules and their comparison.
By the use of partially diversitary microcomputers (microcomputers having the same command set, but internally differing hardware structures), systematic hardware faults can be detected in some cases. Regardless of this, the microcomputers of both channels of a station continuously perform self-test functions in the background.
In accordance with the invention, communication between the bus start station or bus master 12 and the bus end station 20 is subject to time-related information. An absence of a message within a defined time window, e.g. 15 ms, leads to a total shutdown of the system. Alternatively, it is possible to exchange time-related information not only between the master and the bus end station 20 , but also between a plurality of intelligent bus stations 14 , 16 , 18 . This time-critical information exchange is restricted not only to the bus master 12 and the bus end station 20 .
This measures ensures that an interruption of a bus line 38 - 44 can be detected within about 15 ms. The message content is subject to a change over time (counting-up method). With this measure, it is prevented that another station within the bus system can simulate the message of the master or bus end station.
An interruption within a station can only affect one channel in accordance with the usual fault consideration methods and with the PCB layout. As a result, the second fault occurrence time is taken as the basis for this fault type. This consideration results in the necessity that all channels in each station (except the master 12 and the bus end station 20 ) would have to report within one hour for example, depending on the safety requirements. In this way, the strain on the bus can be reduced to a dimension meeting the requirements as regards availability.
In the following, the user software on which the bus system 10 is based is to be explained. A user is given the possibility of adapting the control system to his circumstances. With the aid of a menu-controlled software, the user can assign inputs and/or outputs to the stations 12 - 20 . This configuration software can be installed on any IBM-compatible system which has for example the MS-DOS operating system. The assignment of input and output planes is performed in a matrix-like form.
In accordance with the invention, function blocks are displayed to the user without the latter having access to the logic functions of these blocks. Function blocks concern for example the parameterization of commercially available protective devices, e.g. door tumblers, emergency-off command devices and similar, but also—for specific protective functions—the programming of logic functions such as AND, OR, NOT. The logic functions are not filed in the programming unit such as a PC, instead only the name of the function block, e.g. door tumbler, its number, options, input terminal numbers, output terminal numbers and comments are filed in the programming unit. The actual logic components realized in a relay module thanks to the internal wiring are filed as a macro in the memory module 118 such as an EPROM. The memory module is for example an integral part of the bus master 12 .
The user can transmit data from the programming unit via the serial interface 90 to the bus master 12 , for example. To provide the user with the possibility of incorporating his own non-safety-relevant actuators/sensors into the system, macros are additionally provided with simple logic functions such as “AND”, “OR” and “NOT” that may only affect a firmly predetermined output area. With these functions, the user can use an input area, assign logic functions to the latter and make it affect predetermined outputs. Since the logic functions of these macros are filed only in the bus master 12 , and the input variable block has been restricted to one address area and only predefined outputs may be used, the user cannot exert any influence on the safety-related program part of this data block.
FIGS. 12-16 show as examples programming masks using which the system is programmable. With the aid of a mask M 1 , it is stipulated at which point the respective stations 12 - 20 should be located inside the bus system 10 . In the design example shown, a maximum expansion capacity is 64 bus stations. It is provided here that the bus master 12 and the bus end station 20 are already permanently set.
FIG. 13 shows a mask M 2 for the emergency-off module. The mask M 2 has a field “designation” into which a freely selectable name can be entered. Furthermore, a field “channel 1 ”/“channel 2 ” is provided, into which a terminal designation of the attached contact is entered. Also, a “Start” field is provided that describes the terminal of a start button. The “Additional conditions” field for example represents a feedback loop. In the field “Release” the required output is set when all conditions have been fulfilled. A further delayed-drop-out release signal is provided in a field “Delayed”. The time-lag is settable here. The start condition can be effective automatically with a falling flank or with a rising flank. Within the scope of other applications, an automatic start could also be provided depending on the safety-related framework conditions.
FIG. 14 shows a mask M 3 for a locking device module that has substantially the same design as the mask M 2 according to FIG. 13 .
FIG. 15 shows a mask M 4 that represents a logic module. With the help of this mask M 4 , inputs or markers can be linked. Here the logic links “AND”, “OR” or “NAND” are available. All logic functions can be programmed by the combination of various logic expressions.
FIG. 16 shows a mask M 5 of a contact multiplication module. In an “Input” field an output of a emergency-off module can be inserted, for example, so that one input can act on several outputs. Furthermore the fields “Channel 1 to 8” are provided in which only free outputs can be entered that respond equivalently to the “master input”.
Overall, a user-friendly interface for user programming is created. The software is checked with the aid of automatic checking programs for their compliance with self-produced guidelines. Since in accordance with the invention software modules are filed as macros in the bus master 12 , they are easy to check and wherever necessary alter for expansion purposes, since instead of total sequence programs interlinked with one another, self-contained and relatively small and clearly verifiable blocks (=macros) form the total program. By the use of a software module for each task such as door tumbler, spring-force locking, magnetic-force locking or emergency-off, these functions can be programmed at the lowest microcomputer or processor level, which increases the transparency and fault-freedom of these program parts in comparison with compiled program codes.
After a user has programmed the required links at the programming unit such as PC, the user program is transmitted via the serial interface 88 to the channel A of the bus master 12 . Here the following data are transmitted.
module type (emergency-off, door locking, . . . ) address inputs address outputs and time-lags.
Channel A of the bus master 12 transmits the data parts in inverted form via the link 86 to channel B, which inverts the data back completely and transmits them directly via the serial interface 88 of channel A back to the programming unit. The non-inverted and read-back user program and the inverted and transmitted user program are now in the programming unit. These data are compared in the programming unit.
The channels of the bus master compare user program data received via the link 86 . In the respective channel these data are assigned to the appropriate macros and copied into the flash-EPROM 218 . Once all data have been transmitted, the user must compare them with the original parameters by loading back the stated parameters. By confirmation of this action, the user can start his program as a test run/commissioning. In addition, the programming unit and the respective channels A and B form a CRC using the received/transmitted data. The programming unit concludes by transmitting its CRC, which is compared by channels A and B.
In the following, implemented monitoring functions are explained. Implemented saving methods or monitoring functions on the bus plane, on the protocol plane and on the processor plane are provided.
Implemented saving methods on the bus plane have been provided by using three out of eight possible data bytes and transferring into these a current counter reading, a current inverted counter reading and a saving byte. Each channel in the master has the information about the counter readings of each module. Each station has its own counter, whose level is filed in the master. The counters of a station (channel A, channel B) are independent.
Accordingly, the information on the counter reading of each station is available four times in the bus master (channel A station planes A, B; channel B station planes A, B). The saving byte contains the information on the status of the inputs/outputs and is stored in the channels of the master with the respective counter readings. The counter readings change with every transmission of a message/status report. The saving byte can remain constant if no change in the output/input statuses occurs. If the counter reading does not change, an internal fault is assumed and the bus system is shut down. The transmission of status messages within the stated time windows is monitored in accordance with the following table I:
TABLE I
Status transmitted of
Monitored by
Time window/ms
master
bus end
15 ms
all stations
15 ms
bus end
master
15 ms
all stations
15 ms
stations
master
100 ms
The time windows are the result of the following fault case considerations:
1st Assumption—That One of the Bus Lines 38 , 40 , 42 , 44 is Broken.
Since the bus line is only single-channel, a break in this line would initially not be noticed from the viewpoint of the bus master 12 . Since the bus end station 20 as the last station in this chain was necessarily unable to report, its status messages would no longer be present in the bus master 12 . The reaction time of the overall system to initial faults must correspond at least to the fault recognition time of traditional safety systems. If relay modules are taken as the basis for these safety considerations, and the break in the supply voltage is recognized as an equivalent fault, this module would ideally drop out in approx. 20 ms.
2nd Assumption—That There is a Fault in Channel A of Station 16
The defect of a channel inside a station that suppresses a transmission of status messages. Since all stations are designed redundant, a failure of one channel within this station would not lead to the loss of the overall function of the station. To achieve a safety failure of the station, at least one further fault within the same station would have to be assumed. As a result the detection time of the first fault is restricted to the time which must be assumed in which the second fault will not yet occur in corresponding probability considerations. The second fault occurrence time was set at <1 hr.
3rd Assumption—That the Bus End Station Has a Defect
In the case of a defect in the bus end station 20 , the same considerations apply as with reference to fault description 1 , i.e. break of the bus line.
Node B on master B: Message type 100 Plane 1 040 Unit no. 16 010 750 h for identifier 00101010000+counter+inv. counter+status
Unlike with the status messages, the event-oriented messages are provided with a high priority (zero dominant) and are preferred in the arbitration.
Finally, implemented monitoring functions on the processor plane in the form of RAM tests are provided.
To achieve a rapid shutdown of outputs in a bus system with safety functions, it is provided in accordance with the device that the programmable control unit 62 , 64 is coupled to the bus via a coupling element, with the programmable control units 62 , 64 being assigned a memory element in which information or message contents are filed for the activation of outputs and/or inputs, and where at least one input and/or output can be activated depending on a comparison of the information filed in the memory element with the signals or information transmitted to the bus.
It is provided in accordance with the method that one bus station transmits a message to the bus line, depending on a signal applied to the input and/or the output, with this message being read by at least one other bus station and compared with message contents assigned for the respective bus station, and an action such as shutdown of a release signal being performed by the bus station when there is agreement between the message and the assigned message content.
To permit this, the respective outputs are informed by the bus about which release signal is to be switched to which message contents before commissioning of the system. As a result, there are tables in the memories of the respective output station which contain the message contents that are to lead to shutdown of the respective release signals. The function of the higher-order control is preserved. Only an additional shutdown path is integrated into the system.
The shutdown and/or switch-on tables filed in memory elements in the individual stations are generated automatically in a programming unit. Here those inputs are assigned to each safety-relevant output to which the latter should react. If for example an output depends on a emergency-off switch and a contact of a safety door, this output is assigned an AND function that depends directly on the respective inputs.
FIG. 17 shows the logic structure of a shutdown table. In the design example shown, an output A 1 depends on a signal M 1 of an emergency-off module 252 and on an output signal M 2 of a door module 254 . The signals M 1 , M 2 are supplied to an AND element 256 in order to generate a release signal for the output.
The emergency-off module 252 has inputs 258 , 260 , 270 , 272 for input signals E 1 , E 2 , “Feedback loop” and “Start”. The door module 254 has inputs 274 , 276 , 278 , 280 , 282 , 284 for input signals E 3 , E 4 , “Locking”, “Unlocking”, “Feedback loop” and “Start”. The described shutdown table initiates a direct shutdown of the output A 1 when the input information E 1 or E 2 or E 3 or E 4 is not met.
If an input station transmits that an input has been opened, this information is read by all output stations and compared with the station's own shutdown table. The shutdown table only has an effect on the shutdown of a release signal. The setting of a release signal can be initiated only by the control unit or by the bus master.
After a user has confirmed the individual modules, the programming unit such as a PC automatically generates a shutdown table and attaches it to the transmission protocol.
The shutdown table is initially filed in the memory of the control. Then the respective shutdown tables are transmitted via the bus to the respective stations. The stations transmit after receipt of the respective shutdown table an echo of the data received, which is checked by the control or by the bus master.
If both channels of a station receive the shutdown table, they perform an internal comparison. The shutdown tables in both channels must be identical, as otherwise no system release signal is given.
If a faulty shutdown table is generated in the programming unit, so that the wrong input information is assigned to an output, this fault is detected as follows:
An output station which is to reset an output on the basis of a request is made to perform the following actions with four independent sets of information:
1. shutdown table channel A 2. shutdown table channel B 3. shutdown by master channel A 4. shutdown by master channel B
These sets of information are dependent on one another in terms of timing.
The shutdown by the shutdown tables must always be faster than the shutdown by the control or bus master. The shutdown sequences must be complied with so that a reset is possible after a shutdown. The channels in the respective output station monitor each other for the correctness of the shutdown sequences.
The user-specific data is stored in the flash-EPROM. The flash-EPROM is programmed via the serial interface 88 . The user data can be transferred with the aid of a switch and/or different saving mechanisms.
The flash-EPROM is checked using the CRC check mentioned above. The check sum for the CRC check was generated by the user PC and compared with the check sum independently generated by the master station. Only when both of these tally is this check sum stored in the flash-EPROM.
A self-test is also provided for, with a register test, a flag test, an LA test and a command set test also being provided for. A test program is provided for the tests.
The watchdog monitors the self-test functions and is operated with more than one trigger point. It is designed so that not only late triggering but also early triggering is detected.
When the control system is put into service, it starts automatically with an initialization phase. The bus master station 12 asks all connected stations 14 to 20 to transmit their status. If all internal test methods such as REM, ROM, I/O, CPU have been completed, the output planes are released. The use of volatile working memories and of voltage monitoring ICs means that the overall system is back in its original state after every start. | A safety-oriented control system with a plurality of decentralized stations is disclosed. The safety-oriented control system is provided with inputs and outputs and at least one centralized station exchanging information with each other via a bus line, wherein at least one of the decentralized stations has independent devices for fault-tolerating and/or fault-controlling self-monitoring to ensure normal operation for linkage and evaluation of signals located at the inputs and outputs of this station or further stations, and devices for processing of the signals and for generation of independent control commands. | 7 |
CROSS REFERENCE TO RELATED APPLICATION
This application is a divisional of U.S. application Ser. No. 14/504,745 filed 2 Oct. 2014, and which is incorporated herein by reference in its entirety.
TECHNICAL FIELD
The present invention pertains to the field of gardening implements. More particularly, the present invention pertains to a detachable or an integrated blowing assembly and other mechanical means for use with motorized mowing machines, for displacing honeybees and other animals from vegetation immediately prior to mowing, so as to save the animals from being killed by the mowing machine.
BACKGROUND OF THE INVENTION
Honeybees worldwide are threatened by a mysterious problem known as Colony Collapse Disorder, or CCD, where the colony loses significant numbers of adult bees and thus cannot sustain itself. This disorder affects the European Honeybee, a valuable pollinator and honey producer here in the US and in Europe. The cause of CCD is unknown at this time, and beekeepers, scientists, and citizens alike are interested in saving as many bees as possible. For instance, the Aug. 19, 2013 issue of Time Magazine features a front page story on the plight of the honeybee, the Sep. 23, 2013 issue of the Pittsburgh Tribune Review featured a story on the European response to CCD, and the Oct. 2, 2013 issue of the Wall Street Journal features a front page article by Joel Millman entitled “A Scientist Teaches Drones and Queens the Birds and Bees” discussing ways in which scientists are trying to reinvigorate honeybee populations by crossbreeding and introducing more diverse genetic material into native honeybee populations. These articles, and many more, discuss an “all the above” approach to the problem of CCD and saving as many bees as possible.
Honeybees love clover, a common plant found in fields and lawns. The bees are so determined to collect pollen from clover and other flowers ordinarily found in lawns and fields that they will not move out of the way, even with the maw of a noisy lawn mower bearing down on them. In some cases, the lawn mower operator can shoo the bee away from the front of the mower, but in many cases, the bee will tenaciously grasp the flower to avoid being dislodged by even moderately strong winds or agitation by sticks, and worse, the operator often cannot even see the bee, who might be on the underside of the flower or otherwise hidden. Hundreds of bees are killed during a single mowing of a typical American lawn, and about 75% of the bees killed by mowing are the ones busy pollinating flowers in the mowed vegetation. Furthermore, placing anything in front of an operational lawn mower creates a danger to the operator, as any attachment to the front of the lawn mowing machine may inhibit the operation of the mower itself and distractions in general are dangerous.
What is needed is a method and assembly to displace bees from fields and lawns that does not harm the bees, is easy to use, and can be safely retrofitted to a number of different lawn mowing machine styles.
DISCLOSURE OF THE INVENTION
Accordingly, a first aspect of the invention provides an improved funnel attachment for a bee displacement assembly, the funnel attachment having walls defining a passageway with a neck opening and opposed mouth opening, and a midpoint positioned between the neck and the mouth, wherein the passageway is further defined by a pair of opposed sidewalls, a ceiling and a floor, the ceiling and the floor arranged in a spaced apart relationship defining a first diameter, wherein at the midpoint, the first diameter tapers to the mouth such that the first diameter at the neck is greater than the first diameter at the mouth.
Also, in accord with the first aspect of the invention, the funnel attachment is further provided with the sidewalls arranged in a spaced apart relationship defining a second diameter, wherein at the midpoint, the sidewalls flare away from each other and terminate at the mouth, such that the second diameter at the mouth is greater than the second diameter at the neck.
A second aspect of the invention provides for a displacement assembly used with a motorized mowing machine, the displacement assembly including a blower assembly having a blower and having the funnel attachment affixed to the blower assembly. The blower assembly is positioned on the front of the motorized mowing machine.
Also, in accord with the second aspect of the invention, the blower is powered by its own motor or by a pulley-belt system coupled to a fan and to a motor of the motorized mowing machine.
Also, in accord with the second aspect of the invention, the displacement assembly is selectively operated by power means and a control assembly.
A third aspect of the invention provides for a displacement assembly kit comprising the blower, the funnel attachment, power means, and adaptors allowing the displacement assembly to be affixed to the motorized mowing machine.
Still in accord with the third aspect of the invention, wire harnesses are provided to couple the power means to the blower for simple installation.
A fourth aspect of the invention provides for a rake having a plurality of tines, the rake positioned on the mowing machine so as to agitate vegetation directly in front of a cutting deck of the mowing machine.
A fifth aspect of the invention provides for a method of displacing animals while mowing vegetation, according to the steps of positioning the displacement assembly so that the vegetation agitation portion of the displacement assembly disturbs an area of vegetation directly in front of the mowing machine cutting deck during operation of the mowing machine. The method provides for use of the rake apparatus as well as the blower assembly, used either separately or together, to agitate vegetation.
BRIEF DESCRIPTION OF THE DRAWINGS
The features and advantages of the invention will become apparent from a consideration of the subsequent detailed description presented in connection with accompanying drawings, in which:
FIG. 1 is a perspective view of the bee displacement assembly according to the invention adapted for use with a typical so-called push mowing machine, the bee displacement assembly oriented in an operational position.
FIG. 2 is a detailed front elevational view of a power assembly of the bee displacement assembly of FIG. 1 .
FIG. 3 is a perspective view of the bee displacement assembly adapted for use with a typical so-called residential-style riding mowing machine, with the invention oriented in the operational position.
FIG. 4 is a front elevational view of the bee displacement assembly shown in FIG. 3 , where the displacement assembly is oriented in a non-operation position.
FIG. 5 is a perspective view of a clamp used to affix the bee displacement assembly according to the invention to the riding mowing machine shown in FIGS. 3 and 4 .
FIG. 6 is a front elevational view the bee displacement assembly according to the invention, as shown in the operational position on a so-called professional-style riding mowing machine.
FIG. 7 is a side elevational, cross sectional view of a funnel attachment portion of the invention.
FIG. 8 is a top, cross sectional view of the funnel attachment in FIG. 7 .
FIG. 9 is a front elevational view of a first embodiment of a bee displacement rake assembly according to the invention, as it would appear affixed to the riding mowing machine.
FIG. 10 is a perspective view of a second embodiment of the bee displacement rake assembly, as it would appear affixed to the riding mowing machine.
FIG. 11 is a side elevational view of a second embodiment of the bee displacement assembly according to the invention, in which a motor of the mowing machine turns a fan housed within a secondary deck structure.
FIG. 12 is a cross sectional, side elevational view of the second embodiment of the bee displacement assembly from FIG. 11 , showing how the second embodiment is installed in the mowing machine via an exploded view of the mowing machine's motor, pulley system and cutting deck.
FIG. 13 is a front elevational view of the second embodiment of the bee displacement assembly in FIG. 11 .
FIG. 14 is a diagrammatic representation of a method of using the bee displacement assembly.
DRAWINGS LIST OF REFERENCE NUMERALS
The following is a list of reference labels used in the drawings to label components of different embodiments of the invention, and the names of the indicated components.
20 blower assembly 22 funnel attachment 22 a neck of funnel 22 b midpoint 22 c mouth of funnel 22 d wall 23 A first diameter (height) measured at neck 23 C first diameter (height) measured at mouth 23 B length of wall 23 E second diameter (width) measured at neck 23 H second diameter (width) measured at mouth 23 G length of wall 23 D mouth extension 29 blower box 26 blower 30 power assembly 30 a power bracket 30 b battery or power supply 30 c power supply on/off controls 30 d battery charger 30 e first wire harness 30 f second wire harness 30 g fastener 40 angled bracket 40 a lower position of angled bracket 40 b upper position of angled bracket 42 bumper bracket 42 a first fastener 42 b blower clamp 42 c second fastener 42 d third fastener 42 e bumper clamp 42 f fastener 46 a rake bracket for push mower 46 rake bracket for riding mower 48 bracket for professional mower 50 rake assembly 50 a head 50 b tines 60 method for displacing bees 60 aa determine if mowing machine has a bee displacement assembly already affixed 60 a affix bee assembly to mowing machine 60 b determine if bee displacement assembly is in an operational position 60 c actuate bee displacement assembly 60 d position bee displacement assembly into operational position 70 second blower assembly 70 a shaft 70 b clutch 70 c drive pulley 70 d belt 70 e pulley 70 f motor of mowing machine 70 g pulley-belt system 72 fan housing or secondary deck 72 a hole 74 fan 90 a push-style mowing machine 90 b residential-style riding mowing machine 90 c deck of mowing machine 90 d professional-style riding mowing machine 92 bumper or front bar 94 handle portion of mowing machine
DETAILED DESCRIPTION
A bee displacement assembly according to the invention is shown in FIGS. 1-13 , and a method of using the bee displacement assembly is shown in FIG. 14 .
Turning now to the Figures, a first embodiment of the bee displacement assembly is provided as a blower assembly 20 coupled to a power assembly 30 adapted for use with grass, brush or other vegetation-cutting machines. For use with a push-style mowing machine 90 a , the blower assembly 20 is affixed to a cutting deck 90 c of the mowing machine 90 a , and the power assembly 30 is affixed to a handle portion 94 of the mowing machine 90 a , as shown in FIGS. 1-2 . For use with a residential-style riding mowing machine 90 b , the blower assembly 20 is affixed to a bumper or front bar 92 , as shown in FIGS. 3-4 , and for a professional or zero-turn style mowing machine 90 d as shown in FIG. 6 , the blower assembly 20 is typically affixed to a location on the front cutting deck 90 c with a bracket 48 .
It should be noted that while the Figures show specific placement of the blower assembly 20 on the various types of mowing machines, these positions are suggestive of suitable locations only and not meant to limit the location of the blower assembly to just those locations. The inventor has found that an acceptable placement location of the blower assembly 20 is one in which during actuation of the blower, a concentrated stream of air is directed at an area in front of the cutting deck 90 c, the stream of air angled downwards so as to sufficiently agitate the vegetation to be mowed prior to mowing by the cutting deck 90 c . Hence, it is possible to orient the blower assembly so as to direct a stream of air perpendicular to the forward motion of the operational mowing machine, so long as the stream of air sufficiently agitates vegetation in the area directly in front of the cutting deck 90 c.
Turning now to FIGS. 1, 3-5 , and FIGS. 7-8 , the blower assembly 20 is further comprised of a funnel attachment 22 coupled to a blower 26 . In a typical embodiment, the funnel attachment 22 is removably coupled to the blower 26 , as shown in the Figures, although in other embodiments, the funnel attachment 22 is permanently affixed to the blower 26 . In the embodiment shown in FIG. 1 , the blower assembly 20 is further provided with a protective box 28 housing the blower 26 , the box 28 further including a filter or screen (not shown) so as to allow the free flow of air required for blower operation but which filters out particles that may otherwise clog a motor (not shown) of the blower 26 . In the embodiment shown in FIGS. 3-4 for a residential-style riding mowing machine 90 b , the blower 26 is shown without the blower box 28 . In some embodiments, the blower 26 is further provided with a blower mouth (not shown) that couples to a neck 22 a of the funnel attachment. In other embodiments, where the funnel attachment is not removable, the blower mouth is shaped and elongated so as to serve a same function as the funnel attachment 22 .
FIG. 7 is a cross sectional, side elevational view and FIG. 8 is a cross sectional top elevational view of the funnel attachment 22 . Turning now to FIGS. 7-8 the funnel attachment 22 is further provided with walls 22 d defining a passageway separating a neck 22 a and an opposed mouth 22 c , with a midpoint 22 b positioned between the neck 22 a and the mouth 22 c.
Looking at FIG. 7 , the neck 22 a , in a first diameter 23 A, is about three inches tall, and from the midpoint tapers downwards to the mouth 22 c at a first diameter 23 C, so that the first diameter 23 C at the mouth 22 c is between half to one inch tall. Further, the mouth 22 c itself extends outwards about one inch forming a mouth extension 23 D, although the inventor notes that in some embodiments, the extension 23 D can be eliminated, or increased over 1 inch, as desired.
Looking now at FIG. 8 , in a typical embodiment, the neck 22 a is approximately three inches wide in a second diameter 23 E, and at the midpoint 22 b , the walls 22 d progressively flare out over a length of about 7 to 10 inches, terminating at a second diameter 23 H at the mouth 22 c . At the mouth 22 c , the second diameter 23 H measures between 7 to 15 inches wide. Regarding the second diameter 23 H, the inventor has noted that a width of 15 inches is an approximate ideal maximum width for the mouth 22 c. In FIGS. 7 and 8 , the wall length 23 B 23 G is about 7 inches, although could be effectively shortened or lengthened as desired and not decrease functionality of the funnel attachment. The vertical height tapering shape coupled with the horizontal width flaring shape of the funnel attachment is critical to proper operation of the invention.
The inventor has found that this particular embodiment shown in the Figures, used with a 240 CFM blower, results in a concentrated air stream able to effectively disperse bees in an area measuring about 38 to 48 inches wide located directly in front of the mouth 22 c , the range of widths listed being approximately the cutting widths of the mowing machine cutting decks 90 c . For the push-style mowing machine, the funnel attachment width at the mouth is about 9-10 inches for a 42 inch cut or wider. On a residential-style riding mowing machine, the funnel attachment mouth width is typically 14 inches, and up to 20 inches or more in width for a 45 inch cutting width. The inventor has tested many widths for the second diameter 23 H, and notes that it typically better to use 2 blower assemblies on the mowing machine than attempt to make the funnel mouth second diameter 23 H wide enough to adequately cover a mowing machine with a cutting width wider than 45 inches, since the wider and larger the mouth, the decrease in air pressure for the concentrated stream of air emitted from the mouth.
The funnel attachment 22 can accommodate larger mowing machines as well by simply by altering the length 23 G 23 B of the walls 22 d , or by using multiple blower assemblies 20 , or various combinations of multiple blower assemblies and/or larger funnel attachments 22 . While the inventor has given some specific dimensions related to the funnel attachment 22 , the inventor notes that a tapering height from neck to mouth (the first diameter) coupled with a flaring width shape (the second diameter) for the funnel attachment 22 , where the relatively larger neck height dimension tapers down to a flattened mouth while the smaller initial neck width flares out into a wider mouth, are a critical feature of the invention, and the actual dimensions suggested are suggested guidelines only. It is the unique tapering-flaring shape of the funnel attachment which concentrates moving air generated by the blower or blower means 70 that is forced through the funnel attachment mouth 22 c and emitted as the concentrated stream of air that is strong enough to effectively disperse bees and other animals along the front width of the mowing machine's cutting deck 90 c . The dimensions given are thus an example of one embodiment of the funnel attachment 22 , and are not meant to limit the funnel attachment 22 to these dimensions.
So long as the tapering-flaring shape of the funnel attachment 22 is maintained, a variety of dimensions for the funnel attachment are possible, however, the inventor has found that the given dimensions provide the most effective bee dispersion. In yet other embodiments (not shown), multiple inventions may be used simultaneously, so as to cover an entire width of the cutting bed 90 c , without loss of air pressure due to an overly wide funnel attachment mouth.
The blower assembly 20 in a typical embodiment is removably affixed to the mowing machine 90 a 90 b 90 d with a plurality of attachment means, such as an angled bracket 40 as shown in FIG. 1 for the push-style mowing machine 90 a , a clamp 42 ( FIG. 5 ) for attaching the blower assembly 20 to the bumper bar 92 of the residential-style riding mowing machine ( FIGS. 3-4 ), and the simple bracket 48 on the professional-style riding mowing machine 90 d ( FIG. 6 ). The attachment means shown in the Figures are representative of some suitable methods of attaching the bee displacement assembly to the mowing machines 90 a 90 b 90 d however the inventor has noted and tested many other styles of brackets, clamps, and other attachments means that are suitable for use with the bee displacement assembly, and the Figures are illustrative of just a few possible ways of affixing the bee displacement assembly to the various lawn mowing machines.
In FIG. 1 , the angled bracket 40 is affixed to both the blower box 28 and the mowing machine 90 . The angled bracket 40 is generally L-shaped, and adapted to receive the blower box (housing the blower) and funnel attachment 22 so that the blower assembly 20 can be placed at a lower position 40 a or a higher position 40 b on the angled bracket 40 as desired. The inventor has found that the best operational angle of the funnel attachment ideally emits a stream of concentrated air generally horizontally across the vegetation in front of the cutting deck, rather than forcing the air downwards on the vegetation, since sometimes air that is angled downwards knocks the bees deeper into the vegetation (where they end up getting run over by the mower and killed) but a more horizontal air stream tends to displace the bees so that they fly away from danger.
For the residential-style riding mowing machine 90 b shown in FIGS. 3-4 , and in more detail in FIG. 5 , the clamp 42 is comprised of a blower clamp 42 b affixed to a bumper clamp 42 e by way of adjustable fasteners 42 a 42 c 42 d , the bumper clamp 42 e removably affixed to the bumper 92 of the mowing machine 90 b by fasteners 42 f . The adjustable fasteners 42 a 42 c 42 d allow the blower assembly 20 to be pivotably affixed to the clamp 42 , so that the angle at which the stream of air is emitted through the mouth 22 c may be adjusted, as necessary, shown in FIGS. 3-4 . When not in use, the blower assembly 20 can be adjusted upwards, as shown in FIG. 4 , or simply left in operational position, as shown in FIG. 3 , as desired.
The blower 26 is typically a motorized blower powered by a power assembly 30 (see FIG. 2 ), by way of a wire harness 32 b coupling the blower 26 to an on/off switch assembly 30 c , and by a second wire harness 32 a coupling the on/off switch assembly 30 c to a battery 30 b . The on/off switch assembly 30 c is further provided with a fuse (not shown) housed inside an electrical box. The battery 30 b is provided as a 12 volt battery weighing approximately four pounds, and capable of providing about an hour's worth of blower operation. The wire harnesses 32 a 32 b are provided so as to facilitate easy connection and disconnection of the power assembly 30 . The inclusion of the battery allows manufacturers of push-style mowing machines to incorporate an electric start for the mowing machine. In other embodiments (not shown), lights may be included in the power assembly 30 that are powered by the battery 30 b . The power assembly 30 is affixed to the push-style lawn mowing machine 90 a by way of a power bracket 30 a removably affixing the power assembly 30 to a handle portion 94 of the push-style mowing machine 90 a.
In yet another embodiment, the bee displacement assembly is provided as a kit comprising the blower assembly 22 , a power assembly 30 , and an optional battery charger 30 d , along with a suitable bracket or other attachment means, so as to allow retrofitting existing push-style mowing machines 90 a . For retrofitting existing riding mowing machines 90 b 90 d , the kit includes the blower assembly 22 , the appropriate attachment means, and the on/off power assembly 30 c and appropriate wire harnesses 30 d 30 f so as to allow the blower assembly to be coupled to the mowing machine's existing power supply to power and permit the use of the external on/off control 30 c . The funnel attachment 22 may also be sold without the blower 26 in a variety of dimensions.
Suitable blowers used by the inventor includes the Dayton® series blowers, and the Jabsco Blower, Flex Mount, 250 CFM, 12 VDC sold by W.W. Grainger Inc., of Lake Forest, Ill. 60045-5201, for a blower that is 7'37×7 inches, fitting an enclosure box measuring about 8×8×8 inches. Other blowers in the range of 240 to 250 CFM are suitable for use with the invention. For hook up to the mowing machine's internal battery, of powering the blower using a separate battery, an off the shelf blower and mowing machine can be used, retrofitted with the funnel attachment 22 and affixed to the mowing machine using the appropriate blower 26 or blower assembly 20 , as needed, and also with the appropriate power assembly 30 , depending on the style of mowing machine.
In yet another embodiment, shown in FIGS. 11-13 , a second blower assembly 70 is shown coupled to existing apparatuses of the mowing machine 90 b . The second blower assembly 70 is comprised of a fan 74 enclosed in an interior space of a secondary deck or fan housing 72 , the housing 72 having a pair of opposed through-bores 72 a sized and shaped to receive a drive shaft 70 a and a clutch 70 b of the mowing machine 90 b . The fan housing is further configured with an opening adapted to receive the funnel attachment 22 , or in some embodiments, as shown in FIG. 12 , the funnel attachment 22 and fan housing 72 are formed as a single housing preserving the unique tapering-flaring shape of the funnel attachment 22 .
Turning now to FIG. 12 , the blower assembly 70 is coupled to an engine or motor 70 f as well as to a pulley system 70 g of the mowing machine 90 b via the drive shaft-clutch system. The pulley system 70 g is typically installed on the cutting deck 90 c of the mowing machine, and the drive pulley 70 c and a set of other pulley wheels 70 e linked together by a drive belt 70 d are turned by the motor 70 f turning the drive shaft-clutch system. The pulley system is responsible for powering a plurality of cutting blades housed under the mowing deck 90 c . In the embodiment shown in FIGS. 11-13 , the fan 74 is turned directly by the motor 70 f via the drive shaft 70 a , but the inventor notes that he has tested an embodiment of the blower assembly 70 (not shown) that can be powered by a secondary pulley system, by adding a second pulley and second belt to the existing system, so that the motor turns both pulley systems, and the second system is used to turn the fan 74 and create the concentrated stream of air needed to disperse the bees.
An on/off switch (not shown) is included with the controls of the mowing machine, and in some instances, such as when an existing mowing machine is retrofitted with the bee displacement assembly, the on/off switch may be housed in a control box affixed to the outside of the mowing machine housing. The inventor has experimented with a number of different ways to selectively operate the fan 74 , such as with lever-cable-spline arrangements, although he notes that there are many ways in which selective operation of the second blower assembly 70 can be achieved. In the embodiment shown in the Figures, the bee displacement assembly is on only when the motor is running.
To use the bee displacement assembly using the second blower assembly, an operator starts the motor of the mowing machine 90 b , and turns on the bee displacement assembly. The clutch 70 b engages the drive shaft 70 a and the drive pulley 70 c. The drive pulley engages the belt 70 d , which turns the other pulleys 70 e linked by the belt 70 d to the drive pulley. The cutting blades of the mowing machine are activated, and the drive shaft turns the fan 74 , generating moving air that is then in turn channeled and emitted through the funnel attachment 22 as the concentrated stream of air. When the operator stops the motor, the bee displacement assembly is also turned off.
The bee displacement invention displaces bees by physically agitating vegetation directly in front of the cutting deck 90 c. In yet another embodiment of the bee displacement invention, shown in FIGS. 9-10 , a rake attachment 50 is affixed to the mowing machine by way of a bracket 46 46 a or other attachment means, the rake having a head 50 a and attached tines 50 b projecting from the head 50 a in a downwards orientation (towards the ground). The tines 50 b are positioned so as to agitate the vegetation directly in front of the cutting deck when the mowing machine is in operation, encouraging the bees to move away from the immediate vicinity. In a first embodiment, shown in FIG. 9 , the tines 50 b are arranged in a regular spaced-apart relationship, and are comprised of metal, plastic or other suitably strong, flexible material. The inventor notes that memory metal is an ideal material for the tines, as it is durable and flexible. In a second embodiment, shown in FIG. 10 , the tines 50 b are flexible, and may be comprised of small chains (as shown) that drag against the vegetation which allows for mowing over uneven surfaces as the tines self adjust to the height of the ground, preventing the tines from digging into the ground or otherwise damaging the vegetation. The rake 50 may be used alone or in conjunction with the blower assembly 22 70 . In still another embodiment, the rake 50 is adjustably affixed to the mowing machine 90 a 90 b 90 d so as to allow the operator to lift the rake as needed or desired independently of operation of the blower assembly and the mowing machine. In this way, the operator can decide whether to use just the blower assembly, the rake, or both together.
Looking now at FIG. 14 , a method 60 of displacing bees and other animals using the bee displacement assembly, the invention, configured either with a blower assembly 20 or a second blower assembly 70 is affixed to the desired mowing machine 90 a 90 b 90 d 60 a if the mowing machine is not already outfitted with the bee displacement assembly. Then, the operator must determine if the vegetation agitation means 20 22 50 is in an operational position 60 b . Operational position for the bee displacement assembly using the blower assembly 20 70 and funnel attachment 22 requires the funnel attachment 22 to be positioned so that the mouth 22 c is angled in front of the cutting deck 90 c . For the rake 50 , the rake tines 50 b must be lowered sufficiently so as to contact vegetation in front of the cutting deck. The mowing machine is started along with the bee displacement assembly 60 c . When the funnel attachment is used in conjunction with the blower 26 or the pulley-driven fan 74 shown in FIG. 13 , the bee displacement assembly is actuated, forcing the air generated by the blower or the fan into the neck of the funnel attachment and emitted out the mouth 22 c as the concentrated stream of air. When the funnel attachment is appropriately angled, the stream of air disturbs an area in front of the cutting deck 90 c , and ideally, disturbs an area equal to the width of the cutting deck 90 c . The mowing machine is used in its normal fashion, but the stream of concentrated air emitted from the mouth 22 c sufficiently disturbs vegetation in the target area, causing animals such as bees to move away from the area immediately in front of the cutting deck 90 c . The operator of the mowing machine can selectively operate the bee displacement assembly by actuating the on/off switch assembly 30 c , as a power-saving feature. In other embodiments, the bee displacement assembly is always operational when the mowing machine is operational.
The inventor stresses that bees gathering nectar tenaciously cling to flowers, and ordinary wind pressure, even on very windy days, is inadequate to encourage the bees to leave their respective flowers. Bees are very difficult to see on vegetation being cut, because the mowing machines move quickly, and even the most ardent bee-lover is usually oblivious to the fact that his or her lawn mower is responsible for the deaths of thousands of honeybees over a typical summer all in the name of keeping the lawn neat and tidy. The bee displacement assembly and its embodiments, and the method of moving bees is the creative culmination of the inventor's desire to save the honeybee.
It is to be understood that the above-described arrangements are only illustrative of the application of the principles of the present invention. Numerous modifications and alternative arrangements may be devised by those skilled in the art without departing from the scope of the present invention. While the inventor is concerned with saving bees, there are many insect pollinators that will also be effectively displaced by the invention. Young animals, such as fawns and rabbit kits, hiding in tall grass are often killed by high speed riding or zero-turn mowing machines, and may be encouraged to move out of the way of an oncoming mowing machine when blasted with the concentrated stream of air, or alternatively, the stream of air moves the vegetation sufficiently to allow the operator to visualize and then avoid killing the young animal or destroying a hidden nest in the grass. | A bee displacement assembly provided as a mowing machine with a direct drive operated fan housed inside a housing formed with a funnel leading from an interior space of the housing and terminating in a mouth. The funnel tapers both horizontally and vertically to the mouth such that the mouth approximates a narrow, widened slot. Powering the motor turns the drive shaft that in turn operates the fan, creating a concentrated stream of air inside the fan housing that is channelized in the funnel and emitted out the mouth at an area of uncut vegetation immediately prior to cutting by a cutting deck of the mowing machine. | 0 |
This is a division of application Ser. No. 07/420,851 filed Oct. 13, 1989, now abandoned.
BACKGROUND
The present invention relates to computer chips for controlling access to a cache memory.
In International Business Machine (IBM) compatible personal computers, the refresh controller sends out one refresh address every 15 microseconds. Each refresh cycle takes around 1 microsecond to refresh all of the system's dynamic memory. In order to keep valid data in dynamic random access memory (RAM), 256 refresh cycles are required every four milliseconds. To enter the refresh cycle, a refresh counter sends out one refresh request every 15 microseconds and a hold request signal is then sent back to the CPU to relinquish the bus to the refresh controller. The CPU regains the bus after the refresh cycle is done.
SUMMARY OF THE INVENTION
The present invention provides a cache controller with both burst and hidden refresh modes. In the burst mode, refresh requests are counted, but not acted on, until a predetermined number of refresh requests have been received. At that time, multiple refreshes are done in a single sequence. Although the amount of time taken for actually refreshing the memory is the same, the time needed for arbitration to obtain control of the necessary busses is reduced, giving an overall savings of time. In the hidden refresh mode, a refresh is done, but no hold signal is sent back to stop the central processing unit (CPU) while the refresh is being done. Circuitry is provided which allows local memory accesses, but holds other memory accesses until the refresh is completed. Thus, local memory accesses, which expect data quickly, are not inhibited and other memory accesses, which the CPU expects may take some time, can be held up without the CPU knowing.
For a fuller understanding of the nature and advantages of the invention, reference should be made to the ensuing detailed description taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1. is a timing diagram of a of a prior art advanced technology (AT) refresh cycle;
FIG. 2 is a diagram of a typical system in which a cache controller according to the present invention would operate;
FIG. 3 is a block diagram of the burst refresh control circuitry of the present invention;
FIG. 4 is a timing diagram showing the burst refresh timing;
FIG. 5 is a flow chart of the hidden refresh sequence according to the present invention;
FIG. 6 is a block diagram of the hidden refresh control circuitry of the present invention; and
FIG. 7 is a more detailed drawing of FIG. 6 showing AT cycle,direct memory access and DRAM access arbitration.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In a standard advanced technology (AT) style refresh scheme, the refresh request pulse is sent out every 15.6 usec by a refresh counter. After bus arbitration, HOLD is generated and sent back to the CPU. The CPU relinquishes the bus by issuing HLDA. The REF-, XMEMR-, and REF ADDRESS are generated to refresh both on board and AT bus memory by using RAS-only refresh scheme.
FIG. 1 shows the timing of standard AT refresh cycle.
FIG. 2 shows a typical system in which a cache controller according to the present invention would operate. The CPU 10 is coupled to a local data bus 12 and a local address bus 14. A floating point unit 16 is also coupled to data bus 12. A static RAM (random access memory) 18 is coupled to the local data bus 12 and address bus 14 through buffer 20. The main, dynamic RAM memory 22 is coupled to a memory bus including a memory data bus 24 and a memory address bus 26. This memory bus is controlled by a CPU/memory controller 28 which includes the present invention.
Other busses include an AT bus 30 (with an address portion, SA, and a data portion, SD) and a peripheral data bus 32. Additional data buffers 34 and 36 are provided, and a ROM (read only memory) 38 is provided between the AT and peripheral busses. A circuit 40 acts as a DMA, timer and interrupt controller. Controller 40 is coupled to input/output (I/O) channel 42.
FIG. 3 shows circuitry for controlling the burst mode refresh of the present invention and is contained in blocks 28 and 40 of FIG. 2. A refresh request counter 44 is toggled by each "1" bit on refresh request control line 46 which is coupled to a timer 60 in controller 40. The number of counts required before counter 44 generates an output is controlled by a register 48, which is user programmable. If, for instance, the count is programmed at 4, 4 refresh request signals will be received before a burst refresh request is sent to bus arbitration logic 50 on a control line 52. Arbitration logic 50 will then produce a hold signal to the CPU 10 on a control line 54.
A hold acknowledge signal received back from the CPU on a control line 56 is provided to a refresh cycle counter 64 and RAS generator counter circuit 58. This circuitry provides the refresh signals and control signals to local DRAM. A REF signal is produced on line 62 to a counter 66 in controller 40. Counter 66 produces the refresh signals for the AT bus. When refresh is completed, refresh cycle counter 64 produces a refresh finish signal on a control line 61 to arbitration logic 50, which will release the hold on line 54 to the CPU.
FIG. 4 shows the timing of the present invention for a refresh burst count of 4. The first line shows the refresh request pulse, which is generated every 15 microseconds. As can be seen, 4 of the pulses are generated before the burst refresh request pulse on the second line is produced. Immediately upon the burst refresh pulse, the third line shows 4 refresh clock cycles in sequence. After the conclusion of the 4 cycles, the hold is released and no refresh is done until a next burst refresh request is received.
As can be seen, the amount of time required for bus arbitration logic 50 to gain control of the bus needs to be used only once for every 4 refresh request signals, rather than 4 times as in the prior art. Accordingly, only one-fourth of the normal arbitration time during refresh is required.
A second aspect of the present invention provides a "hidden refresh" mode. In a cache based system, most of the time data is read back from the data cache RAM during a cache read hit cycle, and the DRAM is used only during read miss, DMA, and write cycles. The above DRAM cycles account for only 10 to 20% of the system cycles, therefore the DRAM is usually in the idle state. One way to improve the system performance is to take advantage of the DRAM idle time and refresh it without the attention of the CPU.
When a refresh request is pending and there is no DMA, AT or DRAM access, hidden refresh starts. The hidden refresh is transparent to the CPU and will allow the CPU to continue to operate from its cache memory. No HOLD is sent to the CPU. The CPU must wait for all other accesses requiring the DRAM. All DMA and AT accesses are deferred until the completion of ongoing hidden refresh cycle.
FIG. 5 is a flow chart of hidden refresh operation. When a refresh request is received (step A), the system checks to see whether it is in the hidden refresh mode (step B). If it is not, a normal AT refresh is done (step C). If hidden refresh has been selected, the system checks to see if there is an ongoing DMA cycle (step D) o If there is, the system waits until the cycle is completed. Next, a check is done to see if the DRAM is busy with an access (step E). If it is, again the system waits until the DRAM access is completed. Finally, a check is done to see if there is an AT cycle in progress (step F). If it is, again the system waits until the AT cycle is completed. In each case, a bit is set indicating that a hidden refresh is desired, and thus will gain priority over a subsequent DMA, DRAM or AT cycle.
After ascertaining that there is no competing DMA cycle, DRAM access or AT cycle, the system blocks future AT accesses, DRAM accesses and DMA cycles (step G). Refresh is then started by generating an REF signal on the AT bus (step H). The XMEMR signal is also generated. This signal is used to signal a memory refresh cycle on the I/O channel. The refresh addresses are generated for the off-board memory as well as the RAS signals for the on-board memory and the refresh addresses for the on-board memory. Upon completion of the hidden refresh, the DMA, AT and DRAM accesses are released (step I).
FIG. 6 is a block diagram showing the implementation of the system of FIG. 5. A hidden refresh request is provided to a latch 70, with the output being provided to a DMA arbitration circuit 72. Upon successful arbitration, the output is provided to a DRAM access arbitration circuit 74. Upon successful completion of that arbitration, the signal is provided to an AT access arbitration circuit 76. Thereafter, hidden refresh is enabled and the counter 78 produces the RAS signals for the on-board DRAM along with the address signals, MA0-MA9. A separate signal on a line 80 is provided to an off-board counter 82 which produces the REF, XMEMR and address signals SA0-SA9 for the AT bus.
FIG. 7 shows more detail of how the arbitration of FIG. 6 is done. A DMA arbitration circuit 84 selects between a refresh request on a line 86 and a DMA request on a line 88 which occur at about the same time. A separate input for another signal to be arbitrated is provided on a line 90 but not used for this invention. Essentially, a three-stage count is provided to sequentially select one of latches 92, 94 and 96. This three-stage count is provided with JK latches 98, 100 and 102 in combination with AND gates 104, 106 and 108 coupled as shown under the control of the system clock on line 110.
Upon winning the arbitration, a refresh signal is provided at the output of latch 92 to the input of an AND gate 112. The other input of AND gate 112 on line 114 is the hidden refresh select bit from a register 113 provided to programmably select hidden refresh mode. The output of AND gate 112 is provided to a NOR gate 116 which provides the hidden refresh signal, or a master refresh or a NON-hidden refresh signal to a latch 118. The output of latch 118 is provided to an SR latch composed of NAND gates 120 and 122 configured in a cross-coupled manner as shown. The other input is a signal indicating the end of a refresh or a power-on reset signal on a line 124. The output of NAND gate 122 is provided to a NOR gate 124. The other input of NOR gate 124 is from NAND gate 126. NAND gate 126 is provided with a DRAM not busy signal and a DMA not busy signal. The DMA not busy signal here is not redundant with the above DMA request arbitration. This signal is used to indicate that there is not a DMA access already in progress, which may take some time. The DMA arbitration circuit 84 is used for arbitrating with a substantially simultaneous DMA request signal, which may occur while there is already a DMA access in progress for a separate purpose.
When there is neither a DRAM access nor a DMA cycle, NOR gate 124 is enabled to provide its output to a latch 128. Latch 128 provides its output to an AND gate 130, which receives as its other input an AT not busy signal. This signal indicates that there is no AT cycle in progress. When this condition is satisfied, an output is provided to a latch 132 which provides a hidden refresh signal on line 134 to start the hidden refresh sequence. This sequence is accomplished with the counter circuits 78 and 82 of FIG. 6.
The hidden refresh enable signal is also provided as one input to AND gates 136, 138 and 140. The other input of these AND gates are start signals for an AT cycle, DRAM access cycle, and DMA cycle to respective state machines 142, 144 and 146. Thus, once a hidden refresh is granted, it disables subsequent AT, DRAM and DMA cycles until a refresh end signal is provided on line 124 to propagate through and clear latch 132. The refresh end signal is provided with a refresh cycle counter similar to counter 64 shown in FIG. 3.
FIG. 7 has been drawn with the minimum logic necessary to convey the operation of the present invention. It is to be understood that logical functions have been shown, and could be implemented in many different manners. In addition, additional logic necessary for the overall operation of the system has been omitted to enable a clear understanding of the invention.
As will be understood by those familiar with the art, the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. Accordingly, the disclosure of the preferred embodiment of the invention is intended to be illustrative, but not limiting, of the scope of the invention which is set forth in the following claims. | A cache controller with both burst and hidden refresh modes. In the burst mode, refresh requests are counted, but not acted on, until a predetermined number of refresh requests have been received. At that time, multiple refreshes are done in a single sequence. Although the amount of time taken for actually refreshing the memory is the same, the time needed for arbitration to obtain control of the necessary busses is reduced, giving an overall savings of time. In the hidden refresh mode, a refresh is done, but no hold signal is sent back to stop the CPU while the refresh is being done. Circuitry is provided which allows local memory accesses, but holds other memory accesses until the refresh is completed. Thus, local memory accesses, which expect data quickly, are not inhibited and other memory accesses, which the CPU expects may take some time, can be held up without the CPU knowing. | 6 |
CROSS-REFERENCE TO RELATED APPLICATION(S)
This application is a National Stage Application of PCT Application No. PCT/US12/42849, filed Jun. 17, 2012, which claims priority to U.S. Provisional Application No. 61/501,059, filed on Jun. 24, 2011.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH
This work was supported in part by Strategic Environmental Research and Development Program # ER-1489. The government has certain rights in this work.
BACKGROUND
A well-documented problem in many countries is contaminated subsurface soil by volatile organic compounds (VOCs), semi-volatile organic compounds (SVOCs), pesticides, polychlorinated biphenyls (PCBs), polyaromatic hydrocarbons (PAHs), total petroleum hydrocarbons (TPH), and/or other contaminants. Such contaminants can become sources of water contamination. For example, certain toxic VOCs can move through soil by dissolving into water passing through. Examples of such toxic VOCs include trichloroethylene (TCE), vinyl chloride, tetrachloroethylene (PCE), methylene chloride, 1,2-dichloroethane, 1,1,1-trichloroethane (TCA), 1,1-dichloroethane, 1,1-dichloroethene, carbon tetrachloride, benzene, chloroform, chlorobenzenes, ethylene dibromide, and methyl tertiary butyl ether.
Many techniques have been developed for remediation of contaminated soil, groundwater, or wastewater. Example techniques include dig-and-haul, pump-and-treat, biodegradation, sparging, and vapor extraction. However, using such techniques to meet stringent clean-up standards can be costly, time-consuming, and ineffective for recalcitrant compounds.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a flowchart illustrating a process for oxidizing a contaminant in accordance with embodiments of the technology.
FIG. 2 a is a plot showing degradation of nitrobenzene as an hydroxyl radical probe using various base-persulfate ratios with 5 mM glucose addition in accordance with embodiments of the technology.
FIG. 2 b is a plot showing degradation of nitrobenzene as an hydroxyl radical probe using various base-persulfate ratios without glucose addition in accordance with embodiments of the technology.
FIG. 3 is a plot showing degradation of hexachloroethane (HCA) as a nucleophile/reductant probe using various base-persulfate ratios with 5 mM glucose addition in accordance with embodiments of the technology.
FIG. 4 is a plot showing degradation of HCA as a nucleophile/reductant probe using various base-persulfate ratios without addition of a base in accordance with embodiments of the technology.
FIG. 5 is a plot showing persulfate degradation at various base to persulfate ratios with 5 mM glucose addition in accordance with embodiments of the technology.
FIG. 6 is a plot showing degradation of hexachloroethane as a nucleophile/reductant probe with additions of glucose, fructose, and galactose in accordance with embodiments of the technology.
FIG. 7 is a plot showing degradation of HCA as a nucleophile/reductant probe by pyruvate-activated persulfate at neutral pH in accordance with embodiments of the technology.
DETAILED DESCRIPTION
Various embodiments of contaminant oxidation systems, compositions, and methods are described below. Particular examples are describe below for illustrating the various techniques of the technology. However, a person skilled in the relevant art will also understand that the technology may have additional embodiments, and that the technology may be practiced without several of the details of the embodiments described below with reference to FIGS. 1-7 .
In situ chemical oxidation (ISCO) technology includes a group of chemical processes for treating contaminated soils and groundwater. Permanganate, catalyzed H 2 O 2 propagations (CHP), and activated persulfate (e.g., Na 2 S 2 O 8 ) are oxidants that may be used in ISCO processes. Each of these oxidants has limitations. For example, permanganate has limited reactivity and may be consumed by natural organic matter. CHP is characterized by rapid hydrogen peroxide decomposition in the subsurface, which can limit contact period with contaminants.
Activated persulfate has a number of advantages over permanganate and CHP. Unlike permanganate, persulfate activation generates a suite of reactive oxygen species that can oxidize and/or otherwise degrade many organic contaminants. In addition, persulfate is more stable than hydrogen peroxide in subsurface soil. Persulfate can persist for weeks to months instead of hours to days for hydrogen peroxide to allow its transport down-gradient and increase the potential contact with contaminants.
To the best knowledge of the inventor, activation mechanisms of persulfate in subsurface soil are not well understood. Common persulfate activators include sodium hydroxide (NaOH) or transition metals, e.g., iron (II). However, both activation techniques have certain drawbacks. Without being bound by theory, it is believed that the iron (II) activation of persulfate is similar to a Fenton initiation reaction in which iron (II) mediates the decomposition of persulfate to sulfate radicals (SO 4 •− ) and sulfate anions (SO 4 2− ) as follows:
− O 3 S—O—O—SO 3 − +Fe 2+ →SO 4 •− +SO 4 2− +Fe 3+ (1)
Sulfate radicals can then react with water to generate hydroxyl radical (OH • ):
SO 4 •− +H 2 O→OH • +SO 4 2− (2)
In addition to sulfate radicals and hydroxyl radicals, reductants or nucleophiles (e.g., superoxide (O 2 − ) or alkyl radicals) have been detected in activated persulfate systems.
There are certain limitations of using iron (II) to activate persulfate. First, the iron (III) that forms in reaction (1) precipitates as an iron hydroxide at pH>4. As a result, an acidic medium is needed to start and/or sustain the activation. Secondly, unlike CHP systems in which iron (III) is reduced to iron (II) after formation, iron (III) is stable in persulfate systems, and thus the initiation reaction may stall.
It is also believed that a base (e.g. sodium hydroxide, a strong base) can activate persulfate by first promoting base-catalyzed hydrolysis of persulfate to form hydroperoxide ( − O 3 S—O—O—SO 3 − H + ) which then reduces another persulfate molecule to form a sulfate radical and a sulfate anion. Oxidation of hydroperoxides results in the formation of superoxide. Although such a system has the potential to be highly reactive, base-activated persulfate reaction is very slow. Also, base-activated persulfate reaction eventually stalls, resulting in failure of the ISCO system. Though persulfate has potentials as an ISCO oxidant, conventional persulfate activation techniques may not be effective.
The present technology is directed to activation of a peroxygen compound (e.g., sodium persulfate) or mixtures thereof in an oxidation system containing an oxygenated organic compound. In particular, embodiments of the present technology use an oxygenated organic molecule (e.g., sugar) as an activator to initiate, maintain, and/or propagate degradation or decomposition of the peroxygen compound. As a result, reactive radicals may be formed for oxidation of chemical contaminants such as VOCs, SVOCs, herbicides and pesticides in contaminated soils and water.
The present technology may be applied in remediation of earth, sediment, clay, rock, and the like (hereinafter collectively referred to as “soil”) and groundwater (i.e., water found underground in cracks and spaces in soil, sand and rocks), process water (i.e., water resulting from various industrial processes), or wastewater (i.e., water containing domestic or industrial waste) contaminated with VOCs, SVOCs, pesticides, herbicides, and/or other contaminants. In addition, the present technology may also be applied to degrade contaminants in sludge, sand, and/or tars.
FIG. 1 is a flowchart illustrating a process 100 for oxidizing a contaminate In accordance with embodiments of the present technology. As shown in FIG. 1 , the process 100 includes contacting the contaminant with a oxidation system comprising a peroxygen compound at stage 102 . The contaminant may be present in an environmental medium including soil, groundwater, process water, and/or wastewater. As used herein, a “peroxygen compound” generally refers to a chemical compound having at least one oxygen-oxygen single bond.
The peroxygen compound can be generally water soluble and include at least one of sodium persulfate, potassium persulfate, ammonium persulfate, other monopersulfates and dipersulfates, and mixtures thereof. The concentration of the peroxygen compound can be about 0.5 mg/L to about 250,000 mg/L, or other suitable values based on particular treatment application. In one particular example, sodium persulfate (Na 2 S 2 O 8 ) can be introduced into contaminated soil or other environmental media. In other embodiments, a mixture containing persulfate (Na 2 S 2 O 8 ) can be introduced into contaminated soil or other environmental media.
As shown in FIG. 1 , the process 100 also includes activating the peroxygen compound with an oxygenated organic compound at stage 104 . The phrase “oxygenated organic compound” is used herein to refer to a monomeric or oligomeric carbon containing compound having at least one of an alcohol, ketone, carboxylic acid, ester, anhydride, or other oxygen bearing functional groups. Examples of oxygenated organic compound can include sugars (e.g., glucose, fructose, lactose, and galactose), carbohydrates, acetone, sodium pyruvate, pyruvate acid, citrate, 1-propanol, 2-propanol, t-butyl alcohol, formaldehyde, 2-butanone, 2-pentanone, 2-heptanone, oxalic acid, acetoacetic acid, malic acid, succinic acid, 1-pentanol, 2-pentanol, 3-pentanol, acetaldehyde, propionaldehyde, butyraldehyde, levulinic acid, isobutanol, and mixtures thereof.
In certain embodiments, a mole ratio of the peroxygen compound to oxygenated organic compound can be about from 1:1000 to about 1000:1. In other embodiments, the mole ratio can be from about 500:1 to about 1:500, about 250:1 to about 1:250, about 100:1 to about 1:100, about 50:1 to about 1:50, about 1:20 to about 20:1, or other suitable values. Optionally, in certain embodiments, a pH modifier may also be introduced at stage 105 . The pH modifier may include an acid, a base, a buffer, and/or other suitable compounds or compound mixtures capable of maintaining a target pH (e.g., greater than about 10) in an environmental medium. In other embodiments, the pH modifier may be omitted.
The process 100 can then include decomposing the peroxygen compound to generate oxidizing radicals at stage 106 . Based on conducted experiments discussed below, the inventor has recognized that the oxygenated organic compound can activate and/or otherwise facilitate decomposition of the peroxygen compound. In one example, sugar was observed to activate the decomposition of a persulfate salt to generate sulfate radicals as follows:
−O 3 S—O—O—SO 3 − +sugar→SO 4 •− +SO 4 2− (3)
The generated sulfate radical can then react with water to generate hydroxyl radical (OH • ) as discussed above in reaction (2). In addition, other oxidizing radicals, reductants, or nucleophiles (e.g., superoxide or alkyl radicals) may also be generated.
The process 100 can then include oxidizing the contaminant with the generated oxidizing radicals. Example contaminants that may be oxidized can include chlorinated solvents such as trichloroethylene (TCE), vinyl chloride, tetrachloroethylene (PCE), methylene chloride, 1,2-dichloroethane, 1,1,1-trichloroethane (TCA), carbon tetrachloride, chloroform, chlorobenzenes. Other example VOCs and SVOCs that may be oxidized with embodiments of the oxidation system can include benzene, toluene, xylene, ethyl benzene, ethylene dibromide, methyl tertiary butyl ether, polyaromatic hydrocarbons, polychlorinated biphenyls, pesticides and/or herbicides phthalates, 1,4-dioxane, nitrosodimethyl amine, chlorophenols, chlorinated dioxins and furans, petroleum distillates (e.g., gasoline, diesel, jet fuels, fuel oils).
In certain embodiments, oxidizing the contaminant may be carried out in situ, i.e., in the physical environment where the contaminant(s) are found. In other embodiments, oxidizing the contaminant may be carried out ex situ by removing a contaminated medium from an original location and treating the removed contaminated medium at a different location. In any of the foregoing embodiments, contacting the contaminant can include injecting the peroxygen compound and/or the oxygenated organic compound into the contaminated medium.
In any of the foregoing embodiments, the amount of the introduced peroxygen compound and/or oxygenated organic compound may be adjusted to reduce the concentration of the contaminants in the environmental medium to a desired level. In certain embodiments, oxidizing the contaminant can also include adjusting an injection rate of the peroxygen compound based upon hydrogeological conditions of the contaminated medium, e.g., the ability of the oxidation system to displace, mix, and disperse with existing groundwater and move through the contaminated medium. In other embodiments, the injection rate may also be adjusted to satisfy an oxidant demand and/or chemical oxidant demand of the contaminated medium. In further embodiments, the injection rate may be adjusted based on other suitable conditions.
Even though the process 100 in FIG. 1 is shown as having activating decomposition of the peroxygen compound with the oxygenated organic compound subsequent to contacting contaminant with the peroxygen compound, in other embodiments, the oxygenated organic compound may be introduced into the environmental medium to active the peroxygen compound in combination with the peroxygen compound, sequentially before, or in repeated sequential applications to the peroxygen compound introduction. In further embodiments, the peroxygen compound and the oxygenated organic compound may be combined into a stable form (e.g., granule, powder, or other solid form) and prepared before introduction into the medium by adding a solvent (e.g., water) or other suitable compounds.
EXPERIMENTS
Sodium hydroxide (reagent grade, 98%), sodium bicarbonate, nitrobenzene, potato starch, and hexane (>98%) were obtained from J.T. Baker (Phillipsburg, N.J.). Sodium persulfate (Na 2 S 2 O 8 ) (reagent grade, >98%), magnesium chloride (MgCl 2 ) (99.6%), and hexachloroethane (HCA) (99%) were obtained from Sigma Aldrich (St. Louis, Mo.). A purified solution of sodium hydroxide was prepared by adding 5-10 mM of MgCl 2 to 1 L of 8 M NaOH, which was then stirred for a minimum 8 hours and passed through a 0.45 μM membrane filter. Sodium thiosulfate (99%), potassium iodide, methylene chloride, and mixed hexanes were purchased from Fisher Scientific (Fair Lawn, N.J.). Deionized water was purified to >18 MΩ·cm. Nitrobenzene, which has a high reactivity with hydroxyl radicals (kOH•=3.9×10 9 M −1 s −1 ) and negligible reactivity with sulfate radicals (kSO 4 •− =≦10 6 M −1 s −1 ), was used to detect hydroxyl radicals. HCA was used as a reductant probe.
All reactions were conducted in 20 mL borosilicate vials capped with polytetrafluoroethylene (PTFE) lined septa. Each reaction vial contained sodium persulfate, an oxygenated organic compound (e.g., glucose) used as an activator, and the selected probe (1 mM of nitrobenzene or 2 μM of hexachloroethane). Some reactions contained a strong base (e.g. NaOH). At selected time points, sodium persulfate was measured using iodometric titrations, and the residual probe concentration was analyzed with gas chromatography (GC) after extracting the contents of the reactor with hexane.
Hexane extracts were analyzed for nitrobenzene using a Hewlett Packard Series 5890 GC with a 0.53 mm (id)×15 m SPB-5 capillary column and flame ionization detector (FID). Chromatographic parameters included an injector temperature of 200° C., detector temperature of 250° C., initial oven temperature of 60° C., program rate of 30° C./min, and a final temperature of 180° C. Hexane extracts were analyzed for HCA using a Hewlett Packard Series 5890 GC with electron capture detector (ECD) by performing splitless injections onto a 0.53 mm (id)×30 m Equity-5 capillary column. Chromatographic parameters included an injector temperature of 220° C., detector temperature of 270° C., initial oven temperature of 100° C., program rate of 30° C./min, and a final temperature of 240° C. A 6-point calibration curve was developed using known concentrations of nitrobenzene or hexachloroethane solutions respectively. Sodium persulfate concentrations were determined by iodometric titration with 0.01 N sodium thiosulfate.
The results of FIGS. 2 a - 7 demonstrate that the reactivity of persulfate can be enhanced (and controlled) by the addition of an oxygenated organic compound as an activator. FIG. 2 a shows hydroxyl radical generation (quantified through nitrobenzene degradation) for a range of base to persulfate ratios. As shown in FIG. 2 a , persulfate activation increased with increasing basicity; however, glucose activation of persulfate was significant even with minimal base addition. FIG. 2 b shows hydroxyl radical generation in systems containing a base and no glucose addition. As shown in FIG. 2 b , minimal persulfate activation was observed when no glucose was added.
The results demonstrated that the addition of glucose resulted in increased degradation of the hydroxyl radical probe nitrobenzene, relative to base-activated persulfate. Even more surprising results were found using the reductant probe hexachloroethane (HCA) as shown in FIG. 3 . As shown in FIG. 3 , reductants such as superoxide or alkyl radicals were generated by glucose activation of persulfate.
Degradation of the nucleophile/reductant probe hexachloroethane with persulfate and glucose addition, but without the addition of base, is shown in FIG. 4 . The glucose-activated persulfate system is effective without pH adjustment, although some base might be needed to maintain pH neutrality. The decomposition of persulfate in glucose-activated persulfate systems is shown in FIG. 5 . The results demonstrate that higher glucose amounts may not consume large masses of persulfate. Degradation of the nucleophile/reductant probe hexachloroethane with additions glucose, fructose and galactose is shown in FIG. 6 . The results demonstrate that glucose, fructose, and galactose are all effective in activating persulfate.
Pyruvate was also investigated as a keto acid for activation of persulfate at neutral pH. Hexachloroethane was used as a nucleophile/reductant probe in aqueous solutions containing 0.5 M persulfate and 5 mM pyruvate and 0.5 M persulfate and 50 mM pyruvate. Control systems included hexachloroethane in deionized water and in 0.5 M persulfate without the addition of pyruvate. All systems were adjusted to pH 7. The results, shown in FIG. 7 , demonstrate that pyruvate activates persulfate at neutral pH using both 5 mM and 50 mM pyruvate. Furthermore, it is also believed that a rate of persulfate activation is inversely proportional to the chain length of a keto acid. As such, the rate of persulfate activation can potentially be controlled by selecting the appropriate keto acid as an activator.
From the foregoing, it will be appreciated that specific embodiments of the technology have been described herein for purposes of illustration, but that various modifications may be made without deviating from the disclosure. In addition, many of the elements of one embodiment may be combined with other embodiments in addition to or in lieu of the elements of the other embodiments. | Various embodiments of contaminant removal systems, compositions, and methods are described herein. In one embodiment, a method for oxidizing a contaminant includes contacting the contaminant with a peroxygen compound and initializing, maintaining, or propagating degradation of the peroxygen compound with an oxygenated organic compound, thereby releasing oxidizing radicals. The method also includes oxidizing the contaminant with the released oxidizing radicals. | 2 |
BACKGROUND OF THE INVENTION
The invention concerns a safety system associated with a handgun comprising an electronic device with a timer.
The special field of application of the handgun according to the invention (short gun or long gun) concerns in particular sporting guns.
Handguns have in principle a barrel. Hunting rifles can have a total of four barrels.
At the rearward end of the barrel there is a cartridge chamber for receiving a cartridge. Each barrel has correlated therewith a lock. This lock has a hammer which is tensioned against the force of a spring. By actuating the trigger, the hammer can be released so that, as a result of the spring force, it will accelerate forwardly and actuate the firing pin and thus fire the cartridge. In addition to hand-actuated locks, there are also so-called self-cocking locks.
The problem with handguns is their safety or lack thereof with regard to improper, in particular, unauthorized use. For example, sporting guns are sometimes not used for months or even years. But they are still operative.
DE 44 13 685 A1 discloses a securing device for hunting and sporting guns of the aforementioned kind. For this purpose, a timing relay is provided which, by means of a reversing lever, for example, the safety lever of the gun, or by the cocking lever can be actuated. After the pre-adjusted time has elapsed, various safety and alert functions are triggered. For example, after the time period has elapsed, a decocking device may be actuated so that the weapon is set on safety or is decocked. Also, it is possible to provide a visual or acoustic signal after the time period has elapsed.
Based on this, the object of the invention is to provide a handgun of the aforementioned kind with improved safety.
SUMMARY OF THE INVENTION
The technical solution is characterized in that the timer of the electronic device can be reset to a temporal start position by means of a separate device that is independent of the handgun by a person exclusively authorized for this purpose, and, after the time period of the timer has elapsed, the operating function of the handgun is canceled and the handgun can no longer be actuated.
The basic idea of the handgun according to the invention resides in that it is provided with a time control. In this context, an appropriate timer is to be understood in the most general sense. Time control provides that the handgun is operative only for a predetermined fixed time period. In order to maintain this operative readiness past this predetermined time period, the timer of the electronic device must be reset to a temporal zero point position before the time period has elapsed. From this point on, the predetermined time period will start again. When, on the other hand, the temporal reset does not occur within this time period, the handgun will be transferred into its inoperative state. This is realized in that the mechanical device for firing the cartridge is blocked by an appropriate device. Of course, even after the blocking action of the gun has been activated, the gun can again be returned into the operative state with the above described process in that the timer is activated. Important in connection with this safety system is that the reset of the timer to the zero point position is done by a device that is independent of the gun and is realized by means of a person exclusively authorized for this purpose, in particular, by a gunsmith. The basic idea of the invention resides thus in that a handgun is to be made inoperative when it has not been used a certain period of time, i.e., in regular sporting activity the timer at the shooting range has not been returned to the temporal zero point position.
A clock is preferably provided as a timer. With this clock a certain time period can be exactly adjusted. This clock can be integrated into the electronic device or provided in a separate removable chip of this electronic device. In any case, this clock together with its electronic device is to be designed such that it cannot be manipulated by unauthorized persons.
As an alternative to the clock as a timer of the electronic device, the life span of an integrated battery can be used also. This is so because the electronic device requires electrical energy for its operation. After a certain time period, there is no longer sufficient energy contained in the battery. For example, the electrical energy can last for 6 to 7 months. This life span of the battery defines the pre-described time period. In order to reset the timer to its zero point position, the battery must be either exchanged or recharged in this special case with use of a battery.
A further safety aspect resides in that when the electronic device or a part of this electronic device is not in its operating position on or within the handgun, the electronic device will recognize this and activate the mechanical blocking device for the mechanical device for firing the cartridge. This can be the case, for example, when the removable chip of the electronic device is not in its operating position. In this context, it is also conceivable that in case of safety considerations the chip is simply confiscated so that the gun can no longer be actuated. Or in case of inherited handguns an appropriate device is installed but the chip is not released to the heirs. In this case, it is also conceivable likewise that the gun is no longer operative when the handgun is prepared in this way by an authorized gunsmith.
A first variant proposes that the electronic device is inseparably arranged in or on the handgun. This means that the gun on the shooting range must be handed over to the authorized person for newly adjusting the timer.
An alternative thereto proposes that at least a part of the electronic device is removable from the handgun and reinsertable. This can be preferably an electronic chip which is inserted into the actual electronic device. Here, it is then possible that the chip is removed from the gun in order to be able to realize by means of it the temporal zero point adjustment. For this purpose, the chip is inserted into an appropriate reading device. Time and location are then also determined therein.
In the state of blockage of the electronic device for firing the cartridge, a visual and/or acoustic signal is generated. This is the case when either the chip has not been inserted into the gun or when the prescribed time period has elapsed. This signal can be suppressed, as needed, on the shooting range.
A further preferred embodiment proposes a radio receiver. This radio receiver for this very special handgun can then influence the operating state of the handgun. When, for example, the handgun is in the hands of an unauthorized person, an appropriate radio signal can be emitted. The signal then blocks by means of the electronic device the mechanical device for firing the cartridge. This in and of itself represents an independent invention.
Finally, it is proposed that the handgun has a positioning system. This gun positioning system is basically embodied as a radio system with the exception that it operates bidirectionally and that primarily also positioning data are sent by the gun in order to transmit and to determine the geographic location and also, for example, the gun number or the number of the central register (and thus also the name of the owner). This represents in and of itself also an independent invention.
BRIEF DESCRIPTION OF THE DRAWINGS
One embodiment of a handgun according to the invention will be explained in the following with the aid of the drawing. This drawing shows a schematic longitudinal illustration of the weapon.
DESCRIPTION OF PREFERRED EMBODIMENTS
The gun has a housing 1 in which, in the drawing, to the right a stock 2 and to the left a cartridge chamber 3 with adjoining barrel are located. The cartridge chamber 3 is limited by a breech plate 4 in which the firing pin is located. Since the illustrated embodiment is a double-barreled rifle, a total of two cartridge chambers 3 are provided that are overlapped.
In the housing 1 there are two adjacently positioned cropped locks 5 each having a pivotably supported hammer 6 . By actuation of the slide 7 on the top of the stock, by means of a lever mechanism, the respective hammer 6 can be cocked against the force of a spring 8 into the rearwardly pivoted cocked position in which the respective hammer 6 is positionally fixed. By actuation of one of two triggers 9 , the respective correlated hammer 6 can be released so that, as a result of the force of the spring 8 , it is accelerated forwardly in the direction of the breech plate 4 of the cartridge chamber 3 and actuates there the percussion cap of the cartridge.
In the stock area, an electronic device 10 , namely comprised of an electronic unit 11 arranged fixedly within the stock 2 as well as an electronic chip 12 which is removable and insertable and in electric contact with the electronic unit 11 .
Provided is moreover a positioning device 13 . It is fixedly and inseparably connected with the gun. This positioning device 13 is based on the GPS system or another positioning system.
Finally, a movable locking part 14 is provided which interacts with the hammer 6 .
The function is as follows:
The afore described electronic device 10 with its electronic unit 11 and its electronic chip 12 comprises a timer. The timer is integrated in the chip 12 .
The gun is operative only when the chip 12 is in the inserted position and the timer of the chip 12 defines a time window within which operation of the gun is possible. For the permanent operativeness of the gun, the timer of the chip 12 must be reset from time to time temporally into a start position. This is possible only by means of an authorized person. By means of this temporal zero point, a time period is predetermined within which the gun is operative. When this time period has elapsed, the electronic device 10 will send a signal to the locking part 14 by means of a cable 15 . The latter locks the mechanical device (no matter at which location) for firing the cartridge. Only when the timer of the chip 12 has been reset to its temporal zero position, the locking part 14 releases, and the gun is then operative again.
Accordingly, when, after the predetermined time period has elapsed, the timer of the chip 12 is not newly “reloaded” again, the operational function of the gun is canceled and can therefore also not be actuated anymore.
By means of the positioning device 13 the weapon can be located. Since it is a bidirectional radio system, by means of this positioning device 13 (but also by a radio device of its own) the electronic device 10 can be acted on such that by means of the radio signal the locking device 14 is actuated and therefore the gun is locked. A locating action by means of the positioning device 13 is then still possible.
LIST OF REFERENCE NUMERALS
1 housing
2 stock
3 cartridge chamber
4 breech plate
5 lock
6 hammer
7 slide
8 spring
9 trigger
10 electronic device
11 electronic unit
12 electronic chip
13 positioning device
14 locking part
15 cable | According to the invention, a handgun has an electronic device with a timer. The timer defines a period of time. If the period of time has expired, the mechanical device for triggering the cartridge is mechanically blocked. | 5 |
FIELD OF THE INVENTION
[0001] This invention relates to assemblies for transferring motion from one shaft to another and more specifically to couplings that are flexible or may, if desired, contain flexible components.
BACKGROUND OF THE INVENTION
[0002] Couplings conventionally are used to transfer motion from one machine shaft to another. Numerous issues are presented in designing a suitable coupling, with variables such as torque, speed, misalignment, dampening, backlash, cost, size, reliability, ease of maintenance, and ease of manufacture needing to be considered. Consequently, many couplings either are designed for particular purposes or function optimally only in certain circumstances.
[0003] At least some couplings are rigid, providing essentially no flexibility. Often cylindrical in shape, these couplings include openings on each end of the cylinder to receive shafts. Typically set screws are used to lock the received shafts into position, although some versions of rigid couplers employ alternative fasteners (such as square keys or woodruff keys). Regardless of fastening mechanism, though, these couplings tolerate essentially no shaft misalignment and cannot provide any dampening.
[0004] Other existing couplings are known as “spider” couplings. Also generally cylindrically shaped, these couplings include protruding members and utilize a cushion (the “spider”) between cylindrical hubs. Although the machine shafts are locked in position relative to each hub (as they are in rigid couplings), employing a spider made of elastomeric material accommodates at least modest shaft misalignment and allows, potentially, for some dampening to occur. By contrast, possible failures of the protruding members under load or shock limit the functionality of these couplings.
[0005] Yet other couplings presently available are called helical beam couplings. Formed, basically, of tubes with helixes cut around the tube walls, these couplings nevertheless maintain rigid hub-shaft connections at their ends. Consequently, although they sometimes may admit some parallel misalignment, they typically permit no axial misalignment of shafts or dampening of the motion. Helical beam couplings further likely will not support high torque levels and are relatively expensive.
[0006] Another type of commercially-available coupling is the slotted-disc, or Oldham, coupling. In this device a hard slotted disc replaces the spider of the spider coupling, allowing the ends of the coupling to move independently of one another. Failures of the disc may occur, however, and no axial (and little angular) misalignment of shafts is permitted. Oldham couplings additionally permit only small amounts of dampening.
[0007] Pinhole-disc couplings (also known as Schmidt couplings) likewise are similar to spider couplings. However, rather than utilizing protruding members, pinhole-disc couplings employ dowel pins on half of the face of the coupling hub. Hubs are joined with special flexible discs that clock them at ninety degrees to each other. Again, though the (usually plastic) discs, or the dowel pins, may fail in use; additionally, no axial shaft misalignment is permitted and only limited dampening is available.
[0008] Bellows and gear-and-sleeve couplings provide further alternatives to the couplings heretofore described. Bellows couplings, with their accordion-style shapes, are highly flexible. They permit neither axial shaft misalignment nor dampening to occur, however, and because of their shape are relatively expensive to manufacture. Gear-and-sleeve couplings, by contrast, allow some dampening. Typically consisting of metallic hubs with external gear teeth that slide into tubular sleeves with complementary grooved teeth, these couplings are advantageous when significant axial misalignment is expected. However, they are relatively expensive to manufacture, require substantial maintenance, tend to vibrate at high speeds, and need lubrication on many metal sleeve designs.
[0009] Among other conventional couplings are double-loop ones, comprising two hubs with a flexible double loop of elastomeric material molded so as to provide an offset figure-eight to each hub. These couplings fail to permit dampening and are relatively expensive to manufacture; as well, because the elastomeric material is large, they require substantial space for operation. Tire couplings likewise comprise hubs (albeit large metallic ones) connected by an elastomeric “tire.” Tire walls are clamped to the large hubs while smaller quick-disconnect bushings lock the hubs to the shafts on each end. Similar to the double-loop couplings, these tire couplings require significant space in which to operate and are expensive to produce. They further are heavier than most other couplings and do not support large torques.
[0010] Shear couplings attempt to protect over-driven shafts from damage. These couplings include two metallic cylindrical hubs, the ends of which receive the shafts, and a molded elastomeric member between them. Rather than supporting high-torque operation, the member contains a center section designed to fail when subjected to high torque so as to reduce the risk of the shaft doing so. Shear couplings also do not permit any axial misalignment of shafts and allow only low angular and parallel misalignments.
[0011] Multi-flex couplings, like many others, include two metallic hubs with a central elastomeric element. Each hub has a groove on its face that contains teeth, and the elastomeric element has integrally-formed teeth on its inner and outer sides at each of its ends. The teeth of the elastomeric element fit into each hub. Possibility of failure of the elastomeric elements remains an issue for these couplings, are does their limited ability to tolerate misaligned shafts.
[0012] Roller-chain couplings provide yet other alternative devices. Consisting of hubs with external gear teeth on an end, these couplings are joined y a roller chain set into the gear teeth so as to lock the hubs together. A cover wraps each set of hubs and chain to complete an assembly. Lubrication is required for the couplings, however, and misalignment tolerances are small. Failure of the chain, further, will result in the coupling being unable to transfer rotational motion.
[0013] Frontline Industries, Inc. of Irvington, N.J. advertises yet another coupling under the name “Big Boy.” This coupling consists of a hub with a center hole to mount shafts and multiple bores positioned around the hub face. A center ring, containing twice as many holes as the number of hub bores, accepts threaded, bullet-shaped pins. Each assembly includes a hub, pins installed on each side of the hub, and a cylindrical rubber bushing placed over the pins, which are then inserted into the bores. Among disadvantages of the “Big Boy” coupling are that it appears to require close tolerances for operation and is expensive to manufacture. The coupling also could disengage if axial misalignment exists above a modest level.
[0014] Finally, also advertised as commercially available is the “Superflex Super Elastic Coupling.” This coupling incorporates a flexible center section connected to two metallic hubs with through bolts positioned in an alternating pattern. It is large in size, however, and both expensive and designed for heavy industrial use.
SUMMARY OF THE INVENTION
[0015] The present invention provides alternatives to these and other existing couplings. Designed to accommodate substantial angular misalignment, medium speeds, and high torques, the couplings of the invention also permit simultaneous axial and parallel shaft misalignments. The couplings additionally are reliable, relatively inexpensive to manufacture, and do not require maintenance of close tolerances. They further may be small in size yet scalable if necessary to meet demand for larger sizes. Other beneficial characteristics of the couplings include maintenance of rotational motion transfer notwithstanding failures of portions of the couplings, relatively few parts, minimal backlash, good dampening qualities, no need for lubrication, and ability to withstand high shock force loads without failure.
[0016] Certain preferred embodiments of the invention include pairs of metallic hubs with multiple dowel-like pins and large, offset clearance holes. A center member, advantageously made of elastomeric material with multiple openings, may be fitted between the hubs. Dowel pins also may be pressed, threaded, or otherwise positioned into each hub. The pins preferably (although not necessarily) are tapered toward their free ends to provide additional angular clearance.
[0017] To assemble these couplings, a center member may be slid onto the pins of a hub. Thereafter, a second hub may be rotated sixty degrees so that the pins slip into the holes of the center member. Pins from one hub slip through the clearance holes of the opposing hub but do not touch the opposing hub during normal operation. Openings in each hub receive shafts, with fasteners such as (but not necessarily) key slots and set screws locking them in place.
[0018] This structure transmits rotational force through one shaft to a hub and dowel pins, then to the center member (in shear), to the opposing dowel pins in the opposing hub, and finally to the other shaft. In some embodiments, angular misalignment tolerance may be as great as ten degrees. Parallel misalignment may be tolerated as a function of clearance hole sizes, while axial misalignment is tolerated as a function of dowel pin length. If parallel misalignment is significant, the dowel pins will move diametrically around the clearance holes of the opposing hub as the coupling rotates. Should a pin fail, the remaining pins would enable the coupling to transmit rotational motion (assuming the loads are not so great as to cause the coupling itself to fail).
[0019] Various embodiments of the invention allow the center member to be made of either elastomeric or rigid material. Using elastomeric material to form the center member likely would improve torsional dampening characteristics of the couplings while increasing backlash. Employing rigid plastic or other material for the center member should result in decreased backlash but decreased dampening as well.
[0020] Embodiments of the invention also may permit removal and replacement of the center member. Similarly, they allow for use of dowel pins other than as described above. As an example, rather than tapering, the dowel pins may be headed to limit axial misalignment in certain circumstances.
[0021] It thus is an optional, non-exclusive object of the present invention to provide couplings for transferring rotational motion.
[0022] It also is an optional, non-exclusive object of the present invention to provide couplings adapted to accommodate angular, axial, and parallel shaft misalignments.
[0023] It is another optional, non-exclusive object of the present invention to provide couplings utilizing hub components having both pins and clearance holes.
[0024] It is an additional optional, non-exclusive object of the present invention to provide couplings utilizing a center member received by the pins.
[0025] It is a further optional, non-exclusive object of the present invention to provide couplings in which pins from one hub assembly slip through clearance holes of an opposing assembly.
[0026] Other objects, features, and advantages of the present invention will be apparent to those skilled in the relevant field with reference to the remaining text and the drawings of this application.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] FIG. 1 is an isometric, partially exploded view of a hub of the present invention.
[0028] FIG. 2 is a side view of the hub of FIG. 1 .
[0029] FIG. 3 is an isometric, partially exploded view of a coupling of the present invention utilizing hubs of FIG. 1 .
[0030] FIG. 4 is an end view of the coupling of FIG. 3 .
[0031] FIG. 5 is a side view of the coupling of FIG. 3 .
[0032] FIG. 6 is another side view of the coupling of FIG. 3 illustrating tolerance of substantial angular shaft misalignment.
DETAILED DESCRIPTION
[0033] Illustrated in FIGS. 1-2 is hub assembly 10 . Assembly 10 comprises hub 14 and one or more pins 18 . Also included as part of assembly 10 may be fastener 22 , which is shown in FIGS. 1-2 as comprising a set screw. However, those skilled in the appropriate art understand that devices other than or in addition to a set screw may be utilized as fastener 22 .
[0034] Depicted in hub 18 is bore 26 , defined by collar 28 and designed to receive, in use, a rotating shaft. After such a shaft is received in bore 26 , fastener 22 may be tightened to fix the position of the shaft relative to hub 18 . One or more openings 30 in hub 18 receive pins 18 . Pins 18 typically are pressed into openings 30 and maintained therein with a friction fit. They need not, however, be so pressed, but instead may be connected to hub 14 in any suitable way or integrally formed therewith.
[0035] Also illustrated in hub 14 are one or more clearance holes 34 . Shown as interspersed radially with openings 30 , clearance holes 34 are adapted to receive pins 30 from another hub 14 . In the embodiment of hub 14 detailed in FIG. 1 , three each of openings 30 and clearance holes 34 are present in the hub 14 , with each hole 34 being offset radially from an adjacent opening 30 by sixty degrees. Fewer or greater numbers of openings 30 and clearance holes 34 may exist, however, if necessary or desirable.
[0036] Pins 18 are shown in FIGS. 1-2 as being generally in the form of dowels. Preferred versions of pins 18 are tapered adjacent their free ends 38 . Fixed ends 42 , by contrast, are configured for fitting into openings 30 , preferably (although not necessarily) flush with outer face 46 . As fitted, pins 18 protrude from inner face 50 of hub 14 .
[0037] FIG. 3 illustrates, in exploded form, coupling 54 . Coupling 54 typically comprises a pair of hub assemblies 10 (denominated 10 A and 10 B) together with center member 58 . As constructed, center member 58 is positioned intermediate the hub assemblies 10 and received by both such assemblies 10 A and 10 B.
[0038] In particular, center member 58 includes a plurality of openings 62 , at least one opening 62 for each pin 18 of each hub assembly 10 . Thus, in the exemplary version of coupling 54 depicted in FIG. 3 , center member 58 includes six openings 62 , equaling the total number of pins 18 present in exemplary hub assemblies 10 A and 10 B. These six openings 62 are spaced radially about center member 58 , with one present every sixty degrees. Again, however, fewer or greater numbers of openings 62 , and different spacings, may be utilized instead.
[0039] In use, center member 58 is positioned between respective inner faces 50 A and 50 B of hub assemblies 10 A and 10 B. By appropriately rotating one hub assembly ( 10 A or 10 B), each pin 18 will align with and pass through an opening 62 of center member 58 . Such rotation would equal sixty degrees in the exemplary coupling 54 of FIG. 3 . Each opening 62 advantageously is only slightly larger than the diameter of its associated pin 18 , although other size relationships could exist instead (particularly if pin 18 is not generally cylindrically shaped or opening 62 is non-circular).
[0040] After passing through a corresponding opening 62 of center member 58 , each pin 18 is then received by a corresponding hole 34 of the associated hub assembly 10 A or 10 B. Stated differently, for a particular pin 18 ′ of hub assembly 10 B, the pin 18 ′ passes first through an opening 62 ′ of center member 58 and then through hole 34 ′ of hub assembly 10 A. The result is depicted in FIGS. 4-5 . Generally, the diameter of hole 34 is substantially larger than the diameter of pin 18 so as to provide clearance therefor. If either pin 18 or hole 34 lacks circular cross-section, hole 34 preferably still will provide significant clearance for pin 18 .
[0041] FIG. 6 illustrates the ability of coupling 54 to tolerate substantial angular misalignment of respective shafts. Because holes 34 are larger than ends 38 of pins 18 , pins 18 are able to move some before abutting the boundaries defining holes 34 . Shown in FIG. 6 is hub assembly 10 B misaligned approximately five degrees from axis AX, although greater angular misalignments may also be tolerated. In instances in which substantial parallel misalignment exists, pins 18 will move diametrically within their corresponding clearance holes 34 as coupling 54 rotates.
[0042] Coupling 54 is designed to function satisfactorily at medium speeds and high torques and without lubrication. Hubs 14 preferably (but not necessarily) are made of metal; if so, the metal may be cast, forged, sintered, machined, or otherwise processed as appropriate. Center member 58 preferably is made of flexible material such as (but not limited to) plastics or natural or synthetic rubbers. Alternatively, center member 58 may be made of more rigid plastics or other materials. Center member 58 additionally may be removable if desired for repair, replacement, or otherwise.
[0043] The foregoing is provided for purposes of illustrating, explaining, and describing exemplary embodiments and certain benefits of the present invention. Modifications and adaptations to the illustrated and described embodiments will be apparent to those skilled in the relevant art and may be made without departing from the scope or spirit of the invention. Additionally, although coupling 54 is designed principally for use in aircraft seats with moveable components, it may be used in other seats (vehicular or otherwise) or for other purposes as appropriate or desired. | Addressed are couplings for transferring rotational motion from one shaft to another. The couplings may include flexible components and may be designed to accommodate angular, axial, and parallel misalignments. Included as components of the couplings may be hub portions, each having dowel pins and clearance holes, and a center member positioned intermediate the hub portions. | 5 |
This is a division, of application Ser. No. 710,508, filed Aug. 2, 1976 now U.S. Pat. No. 4,126,216.
BACKGROUND OF THE INVENTION
The phenomenon of stick-slip for generating sound has been a part of the human experience for hundreds of years. When it is properly controlled the result is music as experienced when a musician draws a horse hair bow coated with rosin across a violin string. If, however, the musician presses too hard on the bow and reduces the velocity of traverse across the string, the result is a nerve jangling squawk. A fingernail drawn across a blackboard gives the same effect as does the pressure plate of a clutch at the moment when the non-rotating surface of the clutch throw-out bearing contacts the rotating release fingers of the clutch pressure plate. The fingers of the clutch pressure plate act as tuning forks, which, in conjunction with the spring steel pressure plate, act as a sounding board vibrating as does a cymbal. Together they make a dissonant combination of tones that cannot be ignored and are very objectional.
Prior art has treated the problem of noise in a clutch by introducing various devices in the form of resilient linings and torsional vibration dampeners in proximity with the clutch friction plates. Nowhere, however, has prior art addressed the problem of axial vibrations which originate with the clutch pressure-plate release fingers. This undoubtedly is due to the difficulty encountered in isolating vibration sources in an assembly as complex as an operating clutch. In the case of the present invention, the source of vibrations was discovered while rubbing the clutch release fingers with an alcohol saturated cloth to remove grease. A characteristic sound was produced that was immediately identified with the chirp that is produced when the non-rotating clutch throw-out bearing contacts the relatively rotating clutch release fingers. Armed with this information, attention was focused on possible methods of preventing resonance in the release fingers.
Two courses of action were considered. First, the elimination of the stick-slip condition that prompts the resonance and second, dampening or altering the vibrations induced by stick-slip so that they do not become objectionable. Elimination of stick-slip by treatment of contacting surfaces was given second priority because it was felt that any such treatment would have little permanency in the environment of an operating clutch due to the presence of wear and wear particles. It was reasoned that wear particles could indeed become the equivalent of rosin on a violin bow which enhances the generation of stick-slip.
SUMMARY OF THE INVENTION
This invention, therefore, is primarily directed toward arresting axial vibrations in the clutch release fingers of a clutch pressure plate by dampening out those objectionable audible vibrations and their harmonics which are resonant to that unit. This is accomplished by the addition in intimate contact with the clutch release fingers, a body which has no resonant frequency or harmonic thereof which will vibrate in sympathy with the resonant frequency or harmonics in the audible range of the clutch release fingers.
In theory, many configurations will satisfy this condition such as immersion of the fingers in a liquid, coating the fingers with an appropriate thickness of lead or some other acoustic material, or changing the mass of the fingers to a point where the resonant frequency is beyond the audible range. Practically, however, the condition is most easily attained by weaving an elastomeric o-ring circumferentially in and out between the adjacent radially extending fingers of the pressure plate. An obvious variation of this would be to mold a ring of elastomeric material or acoustical material as an integral part of the clutch release fingers. A metal garter spring or leaf spring in any of several variations could also be designed to replace the o-ring as long as the natural frequency of the substituted spring does not match the natural frequency or harmonics of the clutch pressure plate.
The novelty of the present invention lies principally with the discovery of the problem. Once that is accomplished, the solutions, which are many and varied, are simply applications of the different facets of the science of acoustics.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 shows in cross-section the main parts of a clutch of the pressure plate type.
FIG. 2 shows a plan view of a clutch pressure plate with one embodiment of the invention.
FIG. 3 is a cross-section of FIG. 2 taken along the lines 3--3.
FIG. 4 is a partial plan view of another embodiment of the invention.
FIG. 5 is a cross-section of FIG. 4 taken along the lines 5--5.
FIG. 6 is a partial plan view of still another embodiment of the invention.
FIG. 7 is a partial plan view of still another embodiment of the invention.
FIG. 8 is a partial plan view of still another embodiment of the invention.
FIG. 9 is a partial plan view of still another embodiment of the invention.
FIG. 10 is an enlarged view in cross-section of the area of the pivot points of the clutch pressure plate.
FIG. 11 is a partial plan view of still another embodiment of the invention.
FIG. 12 is a partial plan view of still another embodiment of the invention.
FIG. 13A & 13B is a partial plan view and cross-section of still another embodiment of the invention.
FIG. 14A & 14B is a partial plan view and cross-section of still another embodiment of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 is a diagrammatic view in partial cross-section showing the general relationship of the main parts of a friction clutch of the pressure plate variety to which the present invention is directed. The largest structure of clutch assembly is the flywheel 2, driven by the engine, to which a pressed steel cover 4, is attached. The friction disc 6, is squeezed against the rear axial surface of the flywheel 2, by the pressure plate 8. Pressure for the squeeze is provided by the clutch spring 10 which is a conically shaped spring steel plate provided with radially inwardly extending clutch release fingers 12, at its inner periphery. The squeeze pressure is generated by flattening the cone spring and reacting it against a fulcrum 14, which is held in position by the cover 4. Pressure applied to the clutch release fingers 12 by the clutch throwout bearing 18, when moved by the actuation fork 20, flattens the cone by reaction about the fulcrum 16. As the cone flattens, the outer perimeter of the clutch plate which is the base of the cone, moves in the opposite axial direction from the clutch throwout bearing motion, to release the squeezing action of the pressure plate 8, against the friction disc 6, and the flywheel 2. With the squeeze absent, the flywheel 2 and the friction plate 8 are free to rotate independently of the friction disc 6 which is splined directly to the input shaft of the transmission. This allows, for instance, the engine of a car to be running while the car is standing still. This has the same effect as a car with the engine running, the clutch engaged, and the transmission in neutral. In neither case will power be transmitted from the engine to the drive wheels or vice versa.
In such a drive train, the only time the clutch throw-out bearing 18 rotates is when the actuation fork 20 pushes the non-rotating throw-out bearing 18 against the rotating clutch release fingers 12 to disengage the clutch. The instantaneous slipping when stationary and rotating elements are brought into engagement causes the release fingers 12, which are made of spring steel, to vibrate at their resonant frequency as does a tuning fork when stroked by a violin bow. The second that results from these vibrations is amplified by the sheer number of the release fingers 12 vibrating at the same frequency and by sympathetic vibrations in the spring 10 and associated parts of the clutch assembly.
In the present invention, once the problem has been identified, there are at least three general solutions all of which are prior art in the science of acoustics. First, the vibrations may be dampened by application of acoustical material at strategic points. Second, surface treatment may be applied to the rubbing surfaces that initiate the stick-slip that causes the problem. Third, the resonating parts can be designed so that interfering resonances cancel each other out or the resonances are of such a high or low frequency that they are out of the audible range.
Examples of the first solution are depicted in FIGS. 2-10. FIGS. 2 and 3 show the details of an acoustical ring such as an elastomeric o-ring 22 being circumferentially wound among the radially inward extending clutch release fingers 12 of the clutch spring 10. The o-ring 22 is of a size large enough to fit well outward radially in the interstices between the fingers 12 so that there is no contact with the clutch throw-out bearing 18 (see FIG. 1) where it contacts the clutch release fingers 12 at their convex surfaces 24. This simple and effective installation requires no adhesive or bonding procedure because the o-ring 22 is held in place by centrifugal force as the pressure plate 12 rotates with the engine. The weaving can take place at every second finger 12 as long as each finger 12 is brought into intimate contact on at least one circumferential side with the acoustical o-ring 22.
The interweaving feature of the elastomeric o-ring 22 in the present invention, muffles the vibration of the clutch release fingers 12 by at least two different mechanisms. First, the elastomeric ring 22 urges the adjacent fingers 12 out of phase with each other by pushing in one direction on one finger 12 while it pushes in the other direction at the same instant on the fingers 12 on either side of the first finger 12. The circumstance of being out of phase produces interference between outgoing sound waves which in itself is attenuating and also the opposition to motion reduces the amplitude or loudness of the waves.
Secondly, the impingement of the resilient elastomeric ring 22 against the hardened-steel resilient fingers 12, which are being urged to vibrate by the stick-slip mechanism of the interaction between the relatively moving bodies, tends to continually change the effective mass of the clutch release fingers 12. The more the o-ring is stretched, the greater becomes the apparent mass of the release finger doing the stretching.
It should be noted at this point that the mass in a given system is inversely proportional to the resonant frequency, id est, the larger the bell, the lower the tone. In the present invention, the apparent continuous change in mass results in a continuously changing resonant frequency so that true resonance is not attained for any frequency before the resonant frequency is changed to some other value. In other words, the energy which causes the initial vibration is absorbed or dissipated in continually changing the acceleration of the resonancy to the continuously changing accelerations of continuously differing frequencies. As taught in "The Calculus", this changing of a change is known as the second derivative of the fundamental velocity. These two factors of bringing out of phase and energy dissipation are effective in damping out objectionable vibrations.
FIG. 4 shows an elastomeric grommet 26 inserted in the interstices between the clutch release fingers 12 of the clutch spring 10. The assembly of this configuration is shown in cross-section in FIG. 5. Best results are obtained when the grommet 26 is a squeeze fit axially as well as circumferentially on the clutch spring 10 and the release fingers 12. Damping of the vibrations is achieved in much the same manner as squeezing a vibrating cymbal between a person's fingers.
FIG. 6 shows elastomeric tubes 28 inserted over the clutch release fingers 12 of the clutch spring 10. The elastomeric tubes 28 are stretched over the fingers 12 and are preferably short enough so that they do not cover the area 24 shown in FIG. 3 which contacts the clutch throw-out bearing 18 shown in FIG. 1. If tubes 28 are used which have radial walls that are thicker than the interstices between the release fingers 12, one tube over every third finger 12 is adequate to come into intimate contact with every finger 12 and effectively dampen the objectional vibrations.
FIGS. 7, 8, and 9 show several other versions of acoustical materials which have been applied to the clutch spring 10. In FIG. 7 the acoustical material 30 is an elastomer which has been molded in the interstices between the clutch release fingers 12 and bonded to the circumferential surfaces of the fingers 12. FIG. 8 shows the elastomer 30 as in FIG. 7 which has been connected by a circumferential web 32 of elastomer that has been bonded to the axial surfaces of the clutch spring 10 and the clutch release fingers 12. The web 32 may be on either or both axial surfaces and in addition to the dampening characteristics is an aid to the molding process. FIG. 9 shows the acoustical material as an annulus of adhesive tape 34 applied to an axial surface or surfaces of the clutch spring 10 and the clutch release fingers 12. In all cases the surface 24 shown in FIG. 3, where clutch release fingers 12 are contacted by the throw-out bearing 18 shown in FIG. 1, has been left free of acoustical material.
FIG. 10 is an enlarged cross-section of the clutch assembly at the pivot points 14 and 16 of the clutch spring 10. In this embodiment the acoustical element 36 is held in intimate contact with both clutch spring 10 and the clutch cover 4. Preferably the acoustical element which is made from some easily flexible material such as rubber is positioned radially inward from the fulcrums 14 and 16 so that it is in closer proximity to or impinging on the clutch release fingers. The acoustical element 36 may be a complete o-ring or it may be an interrupted circle with a spring core 38 to urge the acoustical element radially outward for more intimate contact with the clutch spring 10 and the clutch cover 4. Position of the acoustical element 36 may also be secured by molding and bonding it in place or by the application of an adhesive.
FIG. 11 shows in plan view the convex surface 24 of the clutch release fingers 12 of the clutch spring 10 where contact is made with the clutch throw-out bearing 18 shown in FIG. 1. Stick-slip which initiates or excites resonance may be prevented if the contact surface 24 is polished to a surface finish of less than 15 micro-inches R.M.S. Stick-slip may also be prevented if the contact surface 24 is lubricated or coated with some substance with a low coefficient of friction such as polytetrafluorethylene. When stick-slip is eliminated from the initial contact between clutch release fingers 12 and throw-out bearing 18, it is unnecessary to apply damping materials to the clutch assembly because there will be no resonance to dampen. The application of damping materials under these conditions would be valuable only as a back-up measure as the contacting surfaces 24 degenerated from use.
FIG. 12 shows the plan view of a clutch spring 10 in which the circumferential widths of the clutch release fingers differ from each other so that each finger has a different excitation frequency. A wide clutch release finger 40 has a lower resonant or excitation frequency than does a narrow clutch release finger 42. Within this range are intermediate width fingers 44. In such a configuration, the resonant frequency of each clutch release finger is different from the resonant frequency of all the other clutch release finger so that no sympathetic vibrations exist. The vibrations, therefore, are spread out over a wide range with no frequency being dominant or reaching an objectionable level. Each finger resonates in accordance with its own mass. Mass may also be varied by altering the lengths of the interstices 45 between individual fingers 12.
FIG. 13A and FIG. 13B show clutch release fingers 12 of a clutch spring 10 that have been stiffened along their radial axes by uninterrupted radial grooves 46. These radial grooves or ribs 46 as shown in enlarged radial cross-section in FIG. 13B have the effect of increasing the modulus of elasticity of each clutch release finger 12 so that the resonant frequency of each finger 12 can be increased to the point where the resulting sound is not objectionable because it is above the audible range. Comparable ribs and corregations are well known in such applications as automotive engine hoods and sheet metal roofing. In either case the function is primarily to increase rigidity of the structure.
FIG. 14A and FIG. 14B show still another embodiment of the invention in which each clutch release finger 12 is provided with a radial slit along one edge to form a smaller secondary finger 52 which has been displaced axially, in the direction toward the clutch throw-out bearing, to a greater distance than the primary clutch release finger 12 as shown in circumferential cross-section in FIG. 14B. These secondary fingers 52, because of their decreased masses, have resonant frequencies that are not harmonics of the resonant frequency of the primary fingers 12 and are above the audible range. The secondary fingers 52, because of their increased axial displacement are also the first part of the spring 10 to contact the throw-out bearing 18 shown in FIG. 1. This initial contact of secondary fingers 52, is enough to rotate the throw-out bearing 18 so that when the throw-out bearing and the primary release finger 12 establish contact, they are traveling at the same circumferential speed at their points of contact and there is no stick-slip to initiate objectionable resonance in the audible range.
To those skilled in the art to which this invention relates, many changes in construction and widely differing embodiments and applications of the invention will suggest themselves without departing from the spirit and scope of the invention. The disclosures and the description herein are purely illustrative are not intended to be in any sense limiting. | The pressure plate actuation fingers of a friction clutch are provided with means for noise attenuation by the application of acoustical materials, alteration of the mass of vibrating parts, or surface treatment of slipping parts either individually or collectively to prevent the generation of objectionable noise due to resonance and sympathetic vibrations that are initiated by the stick-slip phenomenon as the non-rotating clutch release bearing contacts the relatively rotating actuation fingers. | 5 |
RELATED APPLICATIONS AND CLAIM OF PRIORITY
[0001] This application claims the priority benefit of U.S. Provisional Application No. 60/971,965 filed Sep. 13, 2007, and U.S. Provisional Application No. 60/971,972 filed Sep. 13, 2007, each of which are hereby incorporated by reference.
[0002] Not Applicable
BACKGROUND
[0003] This application discloses an invention that is related, generally and in various embodiments, to a method and system for bypassing a power cell in a multi-cell power supply. In certain applications, multi-cell power supplies utilize modular power cells to process power between a source and a load. Such modular power cells can be applied to a given power supply with various degrees of redundancy to improve the availability of the power supply. For example, FIG. 1 illustrates various embodiments of a power supply (e.g., an AC motor drive) having nine such power cells. The power cells in FIG. 1 are represented by a block having input terminals A, B, and C; and output terminals T 1 and T 2 . In FIG. 1 , a transformer or other multi-winding device 110 receives three-phase, medium-voltage power at its primary winding 112 , and delivers power to a load 130 such as a three-phase AC motor via an array of single-phase inverters (also referred to as power cells). Each phase of the power supply output is fed by a group of series-connected power cells, called herein a “phase-group”.
[0004] The transformer 110 includes primary windings 112 that excite a number of secondary windings 114 - 122 . Although primary winding 112 is illustrated as having a star configuration, a mesh configuration is also possible. Further, although secondary windings 114 - 122 are illustrated as having a delta or an extended-delta configuration, other configurations of windings may be used as described in U.S. Pat. No. 5,625,545 to Hammond, the disclosure of which is incorporated herein by reference in its entirety. In the example of FIG. 1 there is a separate secondary winding for each power cell. However, the number of power cells and/or secondary windings illustrated in FIG. 1 is merely exemplary, and other numbers are possible. Additional details about such a power supply are disclosed in U.S. Pat. No. 5,625,545.
[0005] Any number of ranks of power cells are connected between the transformer 110 and the load 130 . A “rank” in the context of FIG. 1 is considered to be a three-phase set, or a group of three power cells established across each of the three phases of the power delivery system. Referring to FIG. 1 , rank 150 includes power cells 151 - 153 , rank 160 includes power cells 161 - 163 , and rank 170 includes power cells 171 - 173 . A master control system 195 sends command signals to local controls in each cell over fiber optics or another wired or wireless communications medium 190 . It should be noted that the number of cells per phase depicted in FIG. 1 is exemplary, and more than or less than three ranks may be possible in various embodiments.
[0006] FIG. 2 illustrates various embodiments of a power cell 210 which is representative of various embodiments of the power cells of FIG. 1 . The power cell 210 includes a three-phase diode-bridge rectifier 212 , one or more direct current (DC) capacitors 214 , and an H-bridge inverter 216 . The rectifier 212 converts the alternating current (AC) voltage received at cell input 218 (i.e., at input terminals A, B and C) to a substantially constant DC voltage that is supported by each capacitor 214 that is connected across the output of the rectifier 212 . The output stage of the power cell 210 includes an H-bridge inverter 216 which includes two poles, a left pole and a right pole, each with two switching devices. The inverter 216 transforms the DC voltage across the DC capacitors 214 to an AC output at the cell output 220 (i.e., across output terminals T 1 and T 2 ) using pulse-width modulation (PWM) of the semiconductor devices in the H-bridge inverter 216 .
[0007] As shown in FIG. 2 , the power cell 210 may also include fuses 222 connected between the cell input 218 and the rectifier 212 . The fuses 222 may operate to help protect the power cell 210 in the event of a short-circuit failure. According to other embodiments, the power cell 210 is identical to or similar to those described in U.S. Pat. No. 5,986,909 (the “'909 Patent”) and its derivative U.S. Pat. No. 6,222,284 (the “'284 Patent) to Hammond and Aiello, the disclosures of which are incorporated herein by reference in their entirety.
[0008] FIG. 3 illustrates various embodiments of a bypass device 230 connected to output terminals T 1 and T 2 of the power cell 210 of FIG. 2 . In general, when a given power cell of a multi-cell power supply fails in an open-circuit mode, the current through all the power cells in that phase-group will go to zero, and further operation is not possible. A power cell failure may be detected by comparing a cell output voltage to the commanded output, by checking or verifying cell components, through the use of diagnostics routines, etc. In the event that a given power cell should fail, it is possible to bypass the failed power cell and continue to operate the multi-cell power supply at reduced capacity.
[0009] The bypass device 230 is a single pole single throw (SPST) contactor, and includes a contact 232 and a coil 234 . As used herein, the term “contact” generally refers to a set of contacts having stationary portions and a movable portion. Accordingly, the contact 232 includes stationary portions and a movable portion which is controlled by the coil 234 . The bypass device 230 may be installed as an integral part of a converter subassembly in a drive unit. In other applications the bypass device 230 may be separately mounted. When the movable portion of the contact 232 is in a bypass position, a shunt path is created between the respective output lines connected to output terminals T 1 and T 2 of the power cell 210 . Stated differently, when the movable portion of the contact 232 is in a bypass position, the output of the failed power cell is shorted. Thus, when power cell 210 experiences a failure, current from other power cells in the phase group can be carried through the bypass device 230 connected to the failed power cell 210 instead of through the failed power cell 210 itself.
[0010] FIG. 4 illustrates various embodiments of a different bypass device 240 connected to output terminals T 1 and T 2 of the power cell 210 . The bypass device 240 is a single pole double throw (SPDT) contactor, and includes a contact 242 and a coil 244 . The contact 242 includes stationary portions and a movable portion which is controlled by the coil 244 . When the movable portion of the contact 242 is in a bypass position, one of the output lines of the power cell 210 is disconnected (e.g., the output line connected to output terminal T 2 in FIG. 4 ) and a shunt path is created between the output line connected to output terminal T 1 of the power cell 210 and a downstream portion of the output line connected to output terminal T 2 of the power cell 210 . The shunt path carries current from other power cells in the phase group which would otherwise pass through the power cell 210 . Thus, when power cell 210 experiences a failure, the output of the failed power cell is not shorted as is the case with the bypass configuration of FIG. 3 .
[0011] The bypass devices shown in FIGS.3 and 4 do not operate to disconnect power to any of the input terminals A, B or C in the event of a power cell failure. Thus, in certain situations, if the failure of a given power cell is not severe enough to cause the fuses 222 (see FIG. 2 ) to disconnect power to any two of input terminals A, B or C, the failure can continue to cause damage to the given power cell.
SUMMARY
[0012] In one general respect, this application discloses a system including a multi-winding device having a primary winding and a plurality of three-phase secondary windings, a plurality of power cells, wherein each power cell is connected to a different three-phase secondary winding of the multi-winding device, and a bypass device connected to first and second input terminals of at least one of the power cells and to first and second output terminals of at least one of the power cells.
[0013] In another general respect, this application discloses a method including determining that a failure has occurred in a power cell of a multi-cell power supply and applying a pulse of current from a control circuit to a coil. The coil is connected to a first contact which is connected to a first input terminal of the power cell, a second contact which is connected to a second input terminal of the power cell, and a third contact which is connected to first and second output terminals of the power cell.
DESCRIPTION OF THE DRAWINGS
[0014] Various embodiments of the invention are described herein by way of example in conjunction with the following figures.
[0015] FIG. 1 illustrates various embodiments of a power supply;
[0016] FIG. 2 illustrates various embodiments of a power cell of the power supply of FIG. 1 ;
[0017] FIG. 3 illustrates various embodiments of a bypass device connected to an output of the power cell of FIG. 2 ;
[0018] FIG. 4 illustrates various embodiments of a bypass device connected to an output of the power cell of FIG. 2 ;
[0019] FIG. 5 illustrates various embodiments of a system for bypassing a power cell of a power supply;
[0020] FIG. 6 illustrates various embodiments of a system for bypassing a power cell of a power supply;
[0021] FIGS. 7-9 illustrate various embodiments of a bypass device;
[0022] FIG. 10 illustrates various embodiments of a system for bypassing a power cell of a power supply;
[0023] FIG. 11 illustrates various embodiments of a system for bypassing a power cell of a power supply; and
[0024] FIG. 12 illustrates various embodiments of a system for bypassing a power cell of a power supply.
DETAILED DESCRIPTION
[0025] It is to be understood that at least some of the figures and descriptions of the invention have been simplified to focus on elements that are relevant for a clear understanding of the invention, while eliminating, for purposes of clarity, other elements that those of ordinary skill in the art will appreciate may also comprise a portion of the invention. However, because such elements are well known in the art, and because they do not necessarily facilitate a better understanding of the invention, a description of such elements is not provided herein.
[0026] FIG. 5 illustrates various embodiments of a system 250 for bypassing a power cell (e.g., power cell 210 ) of a power supply. As shown in FIG. 5 , the system 250 includes bypass device 252 connected to the output terminals T 1 and T 2 , a bypass device 254 connected to input terminal A, and a bypass device 256 connected to input terminal C. Although the system 250 is shown in FIG. 5 as having respective bypass devices connected to input terminals A and C, it will be appreciated that, according to other embodiments, the respective bypass devices may be connected to any two of the input terminals A, B and C.
[0027] The bypass devices 252 , 254 , 256 may be mechanically-driven, fluid-driven, electrically-driven, or solid state, as is described in the '909 and '284 Patents. For purposes of simplicity, each bypass device will be described hereinafter in the context of a bypass device which includes one or more electrically-driven contactors which are connected to the output of a power cell. As described hereinafter, a given bypass device may be embodied as a single pole single throw (SPST) contactor, a single pole double throw (SPDT) contactor, or a multi-pole contactor.
[0028] Bypass device 252 is a single pole double throw (SPDT) contactor, and includes a contact 258 and a coil 260 . The contact 258 includes stationary portions and a movable portion which is controlled by the coil 260 . The bypass device 252 operates in a manner similar to that described hereinabove with respect to bypass device 240 of FIG. 4 . The bypass device 254 is a single pole single throw (SPST) contactor, and includes a contact 262 and a coil 264 . The contact 262 includes stationary portions and a movable portion which is controlled by the coil 264 . The bypass device 256 is a single pole single throw (SPST) contactor, and includes a contact 266 and a coil 268 . The contact 266 includes stationary portions and a movable portion which is controlled by the coil 268 . In general, in the event of a failure, bypass devices 254 , 256 disconnect the cell input power at substantially the same time that bypass device 252 creates a shunt path for the current that formerly passed through the failed power cell.
[0029] The condition associated with the creation of the described shunt path and the disconnection of cell input power from at least two of the cell input terminals may be referred to as “full-bypass”. When the full bypass condition is present, no further power can flow into the failed cell. As described with respect to FIG. 2 , the fuses 222 of the power cell may operate to help protect the power cell in the event of a short-circuit failure. However, in certain situations (e.g., when fault current is low), the fuses 222 may not clear quickly enough to prevent further damage to the failed power cell. According to various embodiments, the bypass devices 254 , 256 are configured to act quicker than the fuses 222 , and the quicker action generally results in less damage to the failed power cell.
[0030] FIG. 6 illustrates various embodiments of a system 270 for bypassing a power cell (e.g., power cell 210 ) of a power supply. The system 270 includes a single bypass device 272 which achieves the combined functionality of the bypass devices 252 , 254 , 256 of FIG. 5 . The bypass device 272 is a multi-pole contactor which includes a first contact 274 connected to the output terminals T 1 and T 2 of the power cell, a second contact 276 connected to the input terminal A, and a third contact 278 connected to the input terminal C. Each of the contacts 274 , 276 , 278 include stationary portions and a movable portion. Although the second and third contacts 276 , 278 are shown in FIG. 6 as being connected to input terminals A and C, it will be appreciated that, according to other embodiments, the second and third contacts 276 , 278 may be connected to any two of the input terminals A, B and C. The bypass device 272 also includes a single coil 280 which controls the movable portions of the contacts 274 , 276 , 278 .
[0031] The previously discussed methods may be applied with conventional contactors or solenoids, specifically contactors that hold their contacts in a first position when the coil is not energized and hold their contacts in a second position when the coil is energized. However, it may be preferable to employ magnetic latching contactors or solenoids. Magnetically latching contactors or solenoids include permanent magnets which hold their contacts in either the first or second position when the coil is not energized, and upon the application of a brief pulse of voltage to the coil, the contacts transfer to the other position (i.e., first position to second position or second position to first position). A magnetic latching contactor may employ only one coil. In this contactor, the direction of transfer of the contacts may be determined by the polarity of the voltage pulse applied to the coil. Similarly, a magnetic latching contactor may employ two coils, such as the contactor described in U.S. Pat. No. 3,022,450 to Chase. In this type of contactor, the direction of transfer of the contacts may be determined by which of the two coils is energized. In the following exemplary description, a single-coil contactor embodiment is presented by way of example only. A two-coil contactor is equally valid and may be substituted for any of the single-coil contactors. In light of this, all references to the coils will include a possible two-coil reference as well, i.e., “coil(s)”.
[0032] FIGS. 7-9 illustrate various embodiments of a bypass device 300 . The bypass device is a multi-pole contactor, and may be identical to or similar to the bypass device 272 of FIG. 6 . The bypass device 300 includes a first contact which includes stationary portions 302 , 304 and movable portion 306 , a second contact which includes stationary portions 308 , 310 and a movable portion 312 , and a third contact which includes stationary portions 314 , 316 , 318 , 320 and a movable portion 322 . The bypass device 300 also includes a solenoid, or coil(s) 324 which controls the movable portions 306 , 312 , 322 of the first, second and third contacts. The stationary portions 304 , 310 of the first and second contacts may be connected to any two of the input terminals A, B and C of a power cell. The stationary portions 314 , 318 of the third contact may be respectively connected to the output terminals T 1 and T 2 of a power cell. The movable portions 306 , 312 , 322 of the first, second and third contacts are shown in the normal or non-bypass position in FIGS. 7 and 8 , and are shown in the bypass position in FIG. 9 .
[0033] As shown in FIG. 7 , the bypass device 300 also includes electrical terminals 326 connected to the coil(s) 324 , a steel frame 328 which surrounds the coil(s) 324 , a first insulating plate 330 between the steel frame 328 and the stationary portions 304 , 308 , 310 , 312 of the first and second contacts, a second insulating plate 332 between the steel frame 328 and the stationary portions 314 , 316 of the third contact, and first and second support brackets 334 , 336 . The bypass device 300 further includes a non-magnetic shaft 338 which passes through the coil(s) 324 , through openings in the steel frame 328 , through respective openings in first and second insulating plates 330 , 332 , and through respective openings of the first and second support brackets 334 , 336 .
[0034] Additionally, the bypass device 300 also includes a first biasing member 340 between the first support bracket 334 and a first end of the non-magnetic shaft 338 , a second biasing member 342 between the second support bracket 336 and a second end of the non-magnetic shaft, and a position sensing device 344 which is configured to provide an indication of the position (bypass or non-bypass) of the movable portions 306 , 312 , 322 of the first, second and third contacts.
[0035] Although not shown for purposes of simplicity in FIGS. 7-9 , one skilled in the art will appreciate that the bypass device 300 may further include a plunger (e.g., a cylindrical steel plunger) which can travel axially through an opening which extends approximately from the first end of the coil(s) 324 to the second end of the coil(s) 324 , permanent magnets capable of holding the movable portions of the contacts in either the bypass or the non-bypass position without current being applied to the coil(s) 324 , a first insulating bracket which carries the moving portions 306 , 312 of the first and second contacts, a second insulating bracket which carries the moving portion 322 of the third contact, etc.
[0036] In operation, permanent magnets (not shown) hold the plunger in either a first or a second position, which in turn holds the movable portions 306 , 312 , 322 of the contacts in either the non-bypass position or the bypass position. When the electrical terminals 326 receive pulses of current, the pulses of current are applied to the coil(s) 324 , thereby generating a magnetic field. Depending on the polarity of the applied pulse and the position of the plunger, the applied pulse may or may not cause the plunger to change its position. For example, according to various embodiments, if the plunger is in the first position and the movable portions 306 , 312 , 322 of the contacts are in the non-bypass position, a positive current pulse will change the plunger from the first position to the second position, which in turn changes the movable portions 306 , 312 , 322 of the contacts from the non-bypass position to the bypass position. In contrast, if a negative current pulse is applied, the plunger will stay in the first position and the movable portions 306 , 312 , 322 of the contacts will stay in the non-bypass position.
[0037] Similarly, according to various embodiments, if the plunger is in the second position and the movable portions 306 , 312 , 322 of the contacts are in the bypass position, a negative current pulse will change the plunger from the second position to the first position, which in turn changes the movable portions 306 , 312 , 322 of the contacts from the bypass position to the non-bypass position. In contrast, if a positive current pulse is applied, the plunger will stay in the second position and the movable portions 306 , 312 , 322 of the contacts will stay in the bypass position.
[0038] FIG. 10 illustrates various embodiments of a system 350 for bypassing a power cell (e.g., power cell 210 ) of a power supply. The system 350 is similar to the system 250 of FIG. 5 . The system 350 includes a first contact 352 connected to the output terminals T 1 and T 2 of the power cell, a second contact 354 connected to the input terminal A of the power cell, and a third contact 356 connected to the input terminal C of the power supply. Each of the contacts 352 , 354 , 356 include stationary portions and a movable portion. Although the second and third contacts 354 , 356 are shown in FIG. 10 as being connected to input terminals A and C, it will be appreciated that, according to other embodiments, the second and third contacts 354 , 356 may be connected to any two of the input terminals A, B and C.
[0039] The system 350 also includes a first coil(s) 358 which controls the movable portions of the first contact 352 , a second coil(s) 360 which controls the movable portion of the second contact 354 , and a third coil(s) 362 which controls the movable portion of the third contact 356 . According to various embodiments, the coils 358 , 360 , 362 are embodied as contactor coils. According to other embodiments, the coils 358 , 360 , 362 are embodied as part of magnetic latching contactors which do not need to have continuous power applied to the coils in order to hold the plunger in its first or second position and/or to hold the moving portions of the contacts 352 , 354 , 356 in the non-bypass or bypass position. As previously discussed, the magnetic latching contactors may employ a single-coil or a two-coil configuration. The first contact 352 and the first coil(s) 358 may collectively comprise a first contactor, the second contact 354 and the second coil(s) 360 may collectively comprise a second contactor, and the third contact 356 and the third coil(s) 362 may collectively comprise a third contactor.
[0040] The system 350 further includes a first local printed circuit board 364 in communication with the first coil(s) 358 , a second local printed circuit board 366 in communication with the second coil(s) 360 , and a third local printed circuit board 368 in communication with the third coil(s) 362 . Each of local printed circuit boards 364 , 366 , 368 are configured to control the respective movable portions of the contacts 352 , 354 , 356 via the respective coils 358 , 360 , 362 . In general, each of the local printed circuit boards 364 , 366 , 368 is configured to receive commands from, and report status to, a master control device (e.g., master control system 195 of FIG. 1 ) that is held near ground potential. Each of the local printed circuit boards 364 , 366 , 368 are also configured to deliver pulses of energy to the respective coils 358 , 360 , 362 as needed to change the position of the movable portions of the respective contacts 352 , 354 , 356 , and to recognize the position of the movable portions of the respective contacts 352 , 354 , 356 . For example, if the master control device detects that a power cell is to be bypassed, the master control device may send a signal to an individual printed circuit board (e.g., printed circuit board 364 ). Upon receiving the signal, the printed circuit board may control the movable portion of its respective contact, thereby bypassing the power cell. Each of the local printed circuit boards 364 , 366 , 368 may obtain control power from the input lines which are connected to input terminals A, B, C of the power cell, or from a remote power source. As shown in FIG. 10 , one or more position sensing devices (PSD) 365 , 367 , 369 may be utilized to provide the local printed circuit boards 364 , 366 , 368 with the respective positions of the movable portions of the contacts 352 , 354 , 356 . According to various embodiments, the position sensing devices may be embodied as switching devices, Hall Effect sensors, optical sensors, etc.
[0041] For embodiments where the coils 358 , 360 , 362 are part of magnetic latching contactors, the local printed circuit boards 364 , 366 , 368 may each include a DC capacitor which can store enough energy to switch the plunger and/or the movable portions of the respective contacts 352 , 354 , 356 between positions. Each of the local printed circuit boards 364 , 366 , 368 may also include a power supply which restores the stored energy after a switching event, using AC power from the input lines connected to the input terminals A, B, C of the power cell, or from a remote power source.
[0042] FIG. 11 illustrates various embodiments of a system 370 for bypassing a power cell (e.g., power cell 210 ) of a power supply. The system 370 is similar to the system 350 of FIG. 10 . The system 370 includes a first contact 372 connected to the output terminals T 1 and T 2 of the power cell, a second contact 374 connected to the input terminal A of the power cell, and a third contact 376 connected to the input terminal C of the power supply. Each of the contacts 372 , 374 , 376 include stationary portions and a movable portion. Although the second and third contacts 374 , 376 are shown in FIG. 11 as being connected to input terminals A and C, it will be appreciated that, according to other embodiments, the second and third contacts 374 , 376 may be connected to any two of the input terminals A, B and C.
[0043] The system 370 also includes a first coil(s) 378 which controls the movable portions of the first contact 372 , a second coil(s) 380 which controls the movable portion of the second contact 374 , and a third coil(s) 382 which controls the movable portion of the third contact 376 . According to various embodiments, the coils 378 , 380 , 372 are embodied as contactor coils. According to other embodiments, the coils 378 , 380 , 382 are embodied as part of magnetic latching contactors which do not need to have continuous power applied to the coils in order to hold the plunger in its first or second position and/or to hold the moving portions of the contacts 372 , 374 , 376 in the non-bypass or bypass position. As previously discussed, the magnetic latching contactors may employ a single-coil or a two-coil configuration.
[0044] According to various embodiments, the first contact 372 and the first coil(s) 378 are portions of a first bypass device, the second contact 374 and the second coil(s) 380 are portions of a second bypass device, and the third contact 376 and the third coil(s) 382 are portions of a third bypass device. For such embodiments, the system 370 includes a plurality of bypass devices.
[0045] In contrast to the system 350 of FIG. 10 , the system 370 includes a single local printed circuit board 384 which is in communication with the first coil(s) 378 , the second coil(s) 380 , and the third coil(s) 382 . The local printed circuit board 384 is configured to control the respective movable portions of the contacts 372 , 374 , 376 via the respective coils 378 , 380 , 382 . Thus, the local printed circuit board 384 is similar to the local printed circuit boards described with respect to FIG. 10 , but is different in that the local printed circuit board 384 is configured to drive three coils and recognize the respective positions of the movable portions of three contacts. In general, the local printed circuit board 384 is configured to receive commands from, and report status to, a master control device (e.g., master control system 195 of FIG. 1 ) that is held near ground potential.
[0046] The local printed circuit board 384 is also configured to deliver pulses of energy to the coils 378 , 380 , 382 as needed to change the position of the movable portions of the respective contacts 372 , 374 , 376 , and to detect the position of the movable portions of the respective contacts 372 , 374 , 376 . The local printed circuit board 384 may obtain control power from the input lines which are connected to input terminals A, B, C of the power cell, or from a remote power source. As shown in FIG. 11 , one or more position sensing devices 379 , 383 , 385 may be utilized to provide the local printed circuit board 384 with the respective positions of the movable portions of the contacts 372 , 374 , 376 . According to various embodiments, the position sensing devices may be embodied as switching devices, Hall Effect sensors, optical sensors, etc.
[0047] For embodiments where the coils 378 , 380 , 382 are part of magnetic latching contactors, the local printed circuit board 384 may include a DC capacitor which can store enough energy to switch the plunger and/or the movable portions of the contacts 352 , 354 , 356 between positions. The local printed circuit board 384 may also include a power supply which restores the stored energy after a switching event, using AC power from the input lines connected to the input terminals A, B, C of the power cell, or from a remote power source.
[0048] FIG. 12 illustrates various embodiments of a system 390 for bypassing a power cell (e.g., power cell 210 ) of a power supply. The system 390 is similar to the system 370 of FIG. 11 . The system 390 includes a bypass device 392 which may be embodied as a multi-pole contactor. The bypass device 392 may be identical to or similar to the bypass device 300 shown in FIGS. 7-9 . The bypass device 392 includes a first contact 394 connected to the output terminals T 1 and T 2 of the power cell, a second contact 396 connected to the input terminal A of the power cell, and a third contact 398 connected to the input terminal C of the power supply. Each of the contacts 394 , 396 , 398 include stationary portions and a movable portion. Although the second and third contacts 396 , 398 are shown in FIG. 12 as being connected to input terminals A and C, it will be appreciated that, according to other embodiments, the second and third contacts 396 , 398 may be connected to any two of the input terminals A, B and C.
[0049] In contrast to system 370 of FIG. 11 , the system 390 includes a coil(s) 400 which controls the movable portions of the first, second and third contacts 394 , 396 , 398 . According to various embodiments, the coil(s) 400 is embodied as a contactor coil. According to other embodiments, the coil(s) 400 is embodied as part of a magnetic latching contactor which does not need to have continuous power applied to the coil(s) in order to hold the plunger in its first or second position and/or to hold the moving portions of the contacts 394 , 396 , 398 in the non-bypass or bypass position. As previously discussed, the magnetic latching contactors may employ a single-coil or a two-coil configuration.
[0050] The system 390 also includes a single local printed circuit board 402 which is in communication with the coil(s) 400 . The local printed circuit board 402 is configured to control the respective movable portions of the contacts 394 , 396 , 398 via the coil(s) 400 . In general, the local printed circuit board 402 is configured to receive commands from, and report status to, a master control device (e.g., master control system 195 of FIG. 1 ) that is held near ground potential.
[0051] The local printed circuit board 402 is also configured to deliver pulses of energy to the coil(s) 400 as needed to change the position of the movable portions of the respective contacts 394 , 396 , 398 , and to recognize the position of the movable portions of the respective contacts 394 , 396 , 398 . The local printed circuit board 402 may obtain control power from the input lines which are connected to input terminals A, B, C of the power cell. As shown in FIG. 12 , a position sensing device 403 may be utilized to provide the local printed circuit board 402 with the respective positions of the movable portions of the contacts 394 , 396 , 398 . According to various embodiments, the position sensing device may be embodied as a switching device, a Hall Effect sensor, an optical sensor, etc.
[0052] For embodiments where the coil 400 is part of a magnetic latching contactor, the local printed circuit board 402 may also include a DC capacitor which can store enough energy to switch the plunger and/or the movable portions of the contacts 394 , 396 , 398 between positions. The local printed circuit board 402 may also include a power supply which restores the stored energy after a switching event, using AC power from the input lines connected to the input terminals A, B, C of the power cell.
[0053] While several embodiments of the invention have been described herein by way of example, those skilled in the art will appreciate that various modifications, alterations, and adaptions to the described embodiments may be realized without departing from the spirit and scope of the invention defined by the appended claims. | A system for bypassing a power cell of a power supply, the system including a multi-winding device having a primary winding and a plurality of three-phase secondary windings, a plurality of power cells, wherein each power cell is connected to a different three-phase secondary winding of the multi-winding device, and a bypass device connected to first and second input terminals of at least one of the power cells and to first and second output terminals of the at least one of the power cells. | 8 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] Pursuant to 35 U.S.C. §119 (a), this application claims the benefit of earlier filing date and right of priority to Korean Application Number 10-2012-0092161, filed on Aug. 23, 2012, the contents of which are hereby incorporated by reference in their entirety.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] Aspects of the present disclosure relate to cloud computing-based data sharing system and method, and more particularly to cloud computing-based data sharing system and method configured to efficiently share operation information on various industrial devices including a PLC (Programmable Logic Controller) or an HMI (Human-Machine Interface) through a cloud computing environment.
[0004] 2. Description of Related Art
[0005] Various industrial devices including a PLC (Programmable Logic Controller) or an HMI (Human-Machine Interface) are managed and operated by industrial device management units. The industrial device management units are generally formed using a personal computer, and are also installed with an operating software for enabling preparation of a driving program for the industrial device.
[0006] The driving program prepared by the operating software is downloaded by a relevant industrial device and executed. For example, if operating software configured to prepare a PLC driving program is installed at an industrial device management unit, the PLC driving program is prepared using the operating program and downloaded to a PLC.
[0007] Meanwhile, a system including same type or different type of several industrial devices may be required to share various data by operating software installed on each industrial device management unit. For example, in a case a PLC driving program records a value of certain state at a particular location in a memory, and an HMI device reads the value and displays the value on a screen, an operating program capable of preparing the HMI driving program is such that the PLC driving program must learn address of a memory storing a relevant state value.
[0008] That is, an operating software of an industrial device management unit for PLC operation and operating software of the industrial device management unit for HMI operation must share a memory address that stores a particular value. To this end, various methods are conventionally used including a method of sharing data in a file format, a method of separately installing software specially managing the shared data management, and a method of integrating all operating software.
[0009] However, the method of sharing data in a file format by two or more operating software among the abovementioned methods suffers from disadvantages in that access control to the shared data is impossible to make it difficult to guarantee consistency of shared data, and it is inconvenient to reflect amendment through files at one time.
[0010] Furthermore, the method of separately installing, at two or more software, the software specially managing the shared data management also suffers from disadvantages in that it is difficult to manage versions and to maintain interchangeability as participating operating software increases, and complexity increases that manages control operation to several software that individually operate increases.
[0011] The method of integrating all operating software into one also suffers from problems in that costs inevitably increase in light of various characteristics of participating devices, and problems occur of physically overlapped operating spaces when operating software is integrated into one computer device in light of managers being divided for each characteristic.
SUMMARY OF THE INVENTION
[0012] Exemplary aspects of the present disclosure are to substantially solve at least the above problems and/or disadvantages and to provide at least the advantages as mentioned below. Thus, the present disclosure is directed to provide cloud computing-based data sharing system and method configured to efficiently share operation information on various industrial devices including a PLC (Programmable Logic Controller) or an HMI (Human-Machine Interface) through a cloud computing environment.
[0013] In one general aspect of the present disclosure, there is provided a cloud computing-based data sharing system, comprising:
[0000] a plurality of industrial device management units configured to transmit a recent shared data to a cloud server by periodically communicating with the cloud server, to receive a recent shared data of other industrial device management units received from the cloud server and to synchronize the shared data by updating the recent shared data to its own shared data; and
a cloud server configured to compare a received shared data with a pre-stored shared data, in a case a shared data is received form an industrial device management unit among the plurality of industrial device management units through a communication network, to update its shared data as a result of the comparison, and to transmit a notification message including the updated shared data to other industrial device management unit through the communication network.
[0014] Preferably, but not necessarily, the cloud server may include a data base configured to divide, integrally store and/or maintain for each device, the data mutually shared by each industrial device management unit.
[0015] Preferably, but not necessarily, the industrial device management unit may include a storage storing its own shared data, an operating module configured to prepare a driving program of an industrial device, and store the data to be shared with other industrial device management units in the storage, and a data relay module configured to synchronize the shared data by transmitting the shared data stored in the storage to the cloud server by periodically communicating with the cloud server, and to update the shared data stored in the storage using the shared data included in the notification message, in a case the notification message included with the shared data of the other industrial device management units updated from the cloud server is received.
[0016] Preferably, but not necessarily, each of the industrial device management units may be installed with industrial device operating software configured to prepare a driving program of the industrial device, and the shared data includes metadata to be used by the industrial device operating software.
[0017] Preferably, but not necessarily, the metadata may include a storage location data of information accessible by a driving program of the industrial device.
[0018] In another general aspect of the present disclosure, there is provided a cloud computing-based industrial device management device communicating with a cloud server through a communication network, the industrial device management device comprising:
[0000] a storage storing its own shared data;
an operating module configured to prepare a driving program of an industrial device, and store the data to be shared with other industrial device management units in the storage; and
a data relay module configured to synchronize the shared data by transmitting the shared data stored in the storage to the cloud server by periodically communicating with the cloud server, and to update the shared data stored in the storage using the shared data included in the notification message, in a case the notification message included with the shared data of the other industrial device management units updated from the cloud server is received.
[0019] Preferably, but not necessarily, each of the industrial device management units may be installed with industrial device operating software configured to prepare a driving program of the industrial device, and the shared data includes metadata to be used by the industrial device operating software.
[0020] Preferably, but not necessarily, the metadata may include a storage location data of information accessible by a driving program of the industrial device.
[0021] In still another general aspect of the present disclosure, there is provided a data sharing method of a cloud computing-based data sharing system including a plurality of industrial device management devices and a cloud server, the method comprising: periodically communicating, by an industrial device management unit among a plurality of industrial device management units, with the cloud server connected via a network, and transmitting its own recent shared data to the cloud server via the network; comparing, by the cloud server, the transmitted shared data with previously shared data stored in a database and updating the shared data stored in the database as a result of the comparison; transmitting, by the cloud server, a notification message including the updated shared data to other industrial device management units via the network after update of the shared data; and updating, by the industrial device management unit having received the notification message, its own shared data using the shared data included in the received notification message.
[0022] Preferably, but not necessarily, the shared data may include metadata to be used by industrial device operating software.
[0023] Preferably, but not necessarily, the metadata may include a storage location data of information accessible by a driving program of the industrial device.
[0024] The exemplary embodiment of the present disclosure is advantageously configured such that each industrial device management unit maintains shared data at up-to-date state by performing a periodic synchronization with a cloud server in a cloud computing-based environment.
[0025] Furthermore, the exemplary embodiment of the present disclosure is advantageously configured such that a cloud server notifies a change in shared data, in a case there is generated the change in shared data, whereby the shared data can be instantly updated. Particularly, industrial device operating software, configured to prepare a driving program of various industrial devices by being installed at an industrial device management unit, can be used for sharing metadata.
[0026] Still furthermore, the exemplary embodiment of the present disclosure is advantageously configured such that there is no problem of inconsistency in shared data because of no file trans-receiving method, there is no version or interchangeability management problem because of there being no need of installing a separate exclusive shared program, and there is no physical overlapping problem of operating spaces because of no integration of industrial device operating software. As a result, various data sharing for industrial automation can be efficiently and rapidly realized.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] FIG. 1 is a schematic block diagram illustrating a network connection configuration of a cloud computing-based data sharing system according to the present disclosure.
[0028] FIG. 2 is a schematic block diagram illustrating a data synchronization process between a cloud server and an industrial device management unit in a cloud computing-based data sharing system according to the present disclosure.
[0029] FIG. 3 is a schematic block diagram illustrating a detailed network connection configuration of a cloud computing-based data sharing system according to the present disclosure.
[0030] FIG. 4 is a flowchart illustrating a detailed operating process of a data relay module of FIG. 3 .
DETAILED DESCRIPTION
[0031] Hereinafter, exemplary embodiments of the present disclosure will be described in detail with reference to the accompanying drawings.
[0032] FIG. 1 is a schematic block diagram illustrating a network connection configuration of a cloud computing-based data sharing system according to the present disclosure.
[0033] Referring to FIG. 1 , a cloud computing-based data sharing system according to the present disclosure includes a plurality of industrial device management units ( 21 ), a cloud server ( 22 ) and server side storage ( 23 ).
[0034] The industrial device management unit ( 21 ) is an integrated device configured to communicate with the cloud server ( 22 ) via a communication network ( 11 ), and to share data with other industrial device management units. The industrial device management unit ( 21 ) may or may not be connected to one or more industrial devices ( 13 ) depending on its type. The industrial device ( 13 ) may include various types. For example, the industrial device ( 13 ) may be a PLC (Programmable Logic Controller) or an HMI (Human-Machine Interface) device. The industrial device management unit ( 21 ) is generally configured using a personal computer, but may be configured using a mobile terminal but may be configured in various types as long as performance is allowed. The industrial device management unit ( 21 ) is installed with industrial device operating software, where the industrial device operating software is a computer program configured to prepare a driving program for a particular industrial device. A driving program prepared by the industrial device operating software is executed by being downloaded to a relevant industrial device. The industrial device management unit ( 21 ) shares data with other industrial device management units and the shared data can generate an effect of virtually realizing integrated software.
[0035] The cloud server ( 22 ) communicates with each industrial device management unit by being connected thereto via the communication network ( 11 ). The cloud server ( 22 ) interacts with the server side storage ( 23 ) configured to store and maintain data mutually shared with each industrial device management unit ( 21 ), receives the shared data from the each industrial device management unit ( 21 ) to update the server side storage ( 22 ) to a recent shared data, or to transmit the recent shared data stored in the server side storage ( 23 ) in response to request from the each industrial device management unit ( 21 ).
[0036] Each industrial device management unit ( 21 ) basically functions to synchronize the shared data by periodically communicating with the cloud server ( 22 ), where the synchronization of shared data means to maintain same data structure and format relative to mutually different two or more data storage spaces. The types or contents of data that are subjected to synchronization may be variably configured based on needs including operation information, state information, environment information and set information.
[0037] Particularly, the shared data may include metadata to be used by the each industrial device operating software, where the metadata may include storage location or usage of information to be accessed by a driving program of each industrial device. By way of more specific example, in a case the PLC records, at a particular address of a memory, a state value of a predetermined sensor, “0” or “1”, and the HMI device reads the value and displays the value on a screen, an industrial device management unit for operating the PLC and an industrial device management unit for operating the HMI device may share a memory address (metadata) configured to store a state value of a relevant sensor.
[0038] The industrial device management units ( 21 ) sharing the data through the cloud server ( 22 ) may be divided by groups. At this time, the industrial device operating software may function to register itself on a group configured to share the data together. Particularly, the cloud server ( 22 ) transmits, to another industrial device management unit, a notification message notifying that the shared data maintained by itself and the shared data maintained by a predetermined industrial device management unit are different, in a case the shared data maintained by itself and the shared data maintained by a predetermined industrial device management unit are different.
[0039] The notification message may be variably configured if necessary, and for example, the notification message may include a subject (whose data it is) performing the notification and a changed matter of shared data (what or which data was changed).
[0040] In a case a notification message is received from the cloud server ( 22 ), each industrial device management unit ( 21 ) compares the shared data included in the received notification message with its owned shared data to update using a recent shared data, if there is a data that requires update. As a result, each industrial device management unit ( 21 ) can update the shared data based on the notification, in addition to the periodic synchronization, whereby data can be more swiftly and accurately shared. Now, a process of data sharing being realized will be explained according to the present disclosure with reference to FIG. 2 .
[0041] FIG. 2 is a schematic block diagram illustrating a data synchronization process between a cloud server and an industrial device management unit in a cloud computing-based data sharing system according to the present disclosure.
[0042] Referring to FIG. 2 , first, an industrial device management unit ( 21 - 1 ) operating a PLC ( 13 - 1 ) periodically synchronizes its own shared data with the cloud server ( 22 ). The cloud server ( 22 ) in this process performs to notify the determination to another industrial device management unit ( 21 - 2 ) operating the HMI device, if it is determined that update of shard data is necessary because the shared data maintained by the cloud server ( 22 ) and the shared data of the industrial device management unit ( 21 - 1 ) that operates the PLC are different. Then, the industrial device management unit ( 21 - 2 ) that operates the HMI device updates its own shared data using the recent shared data.
[0043] FIG. 3 is a schematic block diagram illustrating a detailed network connection configuration of a cloud computing-based data sharing system according to the present disclosure.
[0044] Referring to FIG. 3 , the industrial device management unit ( 21 ) includes a shared data storage ( 31 ), a data relay module ( 32 ) and industrial device operating software ( 33 ).
[0045] The shared data storage ( 31 ) is a component to allow the industrial device operating software ( 33 ) to store its own shared data, and may have volatile or non-volatile properties. The industrial device operating software ( 33 ) is a computer program to allow preparing a driving program of a particular industrial device, where the prepared driving program is executed by being downloaded to a relevant industrial device.
[0046] Particularly, the industrial device operating software ( 33 ) allows a relevant shared data in the shared data storage ( 31 ), in a case data to be shared with the other industrial device operating software is generated during the execution.
[0047] The data relay module ( 32 ) basically functions to synchronize the shared data of the shared data storage ( 31 ) by periodically communicating with the cloud server ( 22 ). The data relay module ( 32 ) may be configured with some of modules of the industrial device operating software ( 33 ), or may be configured with a separate computer program.
[0048] In the synchronization process of the shared data, the cloud server ( 22 ) updates a changed data using a server side storage ( 23 ), in a case the shared data of its own maintenance is different from the shared data of the industrial device management unit ( 21 ), and transmits the updated shared data to another industrial device management unit via a notification message. In this connection, the data relay module ( 32 ) extracts the changed recent data included in the notification message received from the cloud server ( 22 ), in a case the notification message is received from the cloud server ( 22 ), and updates the shared data of the shared data storage ( 31 ) using the extracted data. Now, operation of the data relay module ( 32 ) will be described in detail with reference to FIG. 4 .
[0049] FIG. 4 is a flowchart illustrating a detailed operating process of a data relay module of FIG. 3 .
[0050] First, as mentioned above, the industrial device operating software ( 33 ) stores a relevant shared data in the shared data storage ( 31 ), in a case a shared data with another industrial device management unit is generated.
[0051] At this time, the industrial device operating software ( 33 ) may perform a process for data identification including attachment of intrinsic ID (Identification) on the relevant data and/or attachment of identification information of a relevant industrial device management unit.
[0052] The data relay module ( 32 ) periodically communicates with the cloud server ( 22 ) to synchronize the shared data stored in the shared data storage ( 31 ) (S 41 , S 42 ). That is, in a case its own shared data is a recent data, the data relay module ( 32 ) uploads its own recent shared data to the cloud server ( 22 ), and receives a relevant shared data to update its own shared data, in a case the shared data maintained by the cloud server ( 22 ) is a recent data.
[0053] Furthermore, the data relay module ( 32 ) updates the shared data of the shared data storage ( 31 ) (S 44 ), in a case a notification message is received from the cloud server ( 22 ) (S 43 ).
[0054] The industrial device operating software ( 33 ) accesses the shared data storage ( 31 ) to check a recent history of the shared data, and operates in response thereto. That is, each industrial device management unit can instantly update to a changed recent shared data through the notification message from the cloud server ( 23 ), and the industrial device operating software ( 33 ) can instantly use the relevant data. As a result, a cooperative work using the shared data of the each industrial device operating software ( 33 ) can be efficiently realized.
[0055] Although exemplary embodiments have been described with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure. More particularly, various variations and modifications are possible in the component parts and/or arrangements of the subject combination arrangement within the scope of the disclosure, the drawings and the appended claims. | Aspects of the present disclosure relate to cloud computing-based data sharing system and method, the system including a plurality of industrial device management units configured to transmit a recent shared data to a cloud server by periodically communicating with the cloud server, to receive a recent shared data of other industrial device management units received from the cloud server and to synchronize the shared data by updating the recent shared data to its own shared data, and a cloud server configured to compare a received shared data with a pre-stored shared data, in a case a shared data is received form an industrial device management unit among the plurality of industrial device management units through a communication network, to update its shared data as a result of the comparison, and to transmit a notification message including the updated shared data to other industrial device management unit through the communication network. | 6 |
This is a continuation of application Ser. No. 687,722 filed on May 19, 1976, now abandoned.
BACKGROUND OF THE INVENTION
Transistors, when used to drive inductive loads in the switching mode, can be damaged by the voltage surge associated with the turn off operation. While the transistor could normally dissipate the energy involved, the breakdown mechanism tends to localize the action. This creates a hot spot in the transistor which in turn further localize the action and burn out occurs at the hot spot. In general when a voltage surge is applied to a transistor, electrical breakdown occurs at that point where the collector most closely approaches the emitter. The resultant current flow is localized and intense local heating at the point of breakdown further localizes the action. Thus a surge of relatively low energy can burn out a transistor of substantial power handling capability.
One approach to the problem has been to arrest the voltage surge in the inductive load with a separate device. For example a large capacitor can be connected across the load so that voltage surges are filtered. Alternatively a diode, poled to conduct during the surge, can act to short circuit the surge. Both of these approaches produce a very slow decay of surge energy and result in an often unacceptably long switching time.
A second approach is to connect a zener diode between the collector and base of the switching transistor. The zener voltage is selected to be as high as possible but lower than transistor breakdown voltage. Using this arrangement results in the voltage surge being arrested by the transistor but while it is active and thus capable of handling a large current distributed over its full area. The action also occurs at a relatively high voltage so that rapid decay of the surge can be achieved. However, it is difficult to match a zener diode with a transistor. The prior art practice has been to use a plurality of low voltage zener diodes in a stack with a single switching transistor. Typically the zener diodes are made using conventional transistor emitter-base structures. Thus the zener diodes are on the order of six volt units. To protect a 60-volt transistor a stack of nine such units would be series connected. Such an arrangement works well but the large number of diodes is cumbersome and expensive. Furthermore there is a problem in that the zener voltage does not track transistor breakdown in terms of the temperature of the switching transistor collector.
SUMMARY OF THE INVENTION
It is an object of the invention to use a protective transistor to prevent destruction of a switching transistor operating an inductive load device.
It is a further object of the invention to protect switching transistors of Darlington connection with a single transistor having a lower breakdown voltage when switching an inductive load.
It is a feature of the invention that a switching transistor can be protected from inductive surges using a single transistor in an arrangement that tracks in terms of temperature.
It is a further feature of the invention that a simple integrated circuit structure can contain both a switching transistor circuit and a protective device that allows safe rapid switching of inductive loads.
These and other features and objects are achieved in a simple transistor switch. A power transistor is common emitter connected to an inductive load either directly or in a Darlington configuration. A protective transistor is coupled between collector and base of the switching transistor. The protective transistor is of the same kind as the switching transistor and has a breakdown voltage somewhat lower than that of the switching transistor. When the switch is turned off an inductive surge raises the collector voltage toward breakdown level; the protective transistor will break down first and pull the switching transistor base voltage toward the collector voltage until the switching transistor is turned on. However, since the voltage is below switching transistor breakdown, the switch will be active and therefore able to dissipate large energy values thus arresting the surge. If the protective transistor is made like the switching transistor, but with a higher Beta, its breakdown will be slightly lower than the switching transistor breakdown and the characteristics will track. Furthermore if the combination is in the form of an IC, the characteristics will track even when the switching transistor becomes heated because of dissipation.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is is a schematic diagram of the circuit of the invention;
FIG. 2 is a schematic diagram of the invention showing an alternative power supply connection;
FIG. 3 is an integrated circuit form of the invention showing topography; and
FIG. 4 is a cross section of the showing of FIG. 3 taken at line 4--4.
DESCRIPTION OF THE INVENTION
FIG. 1 shows a schematic diagram of a relay driver circuit. An electromagnetic relay 9 is shown inside the dashed outline. It comprises a coil 11 and a set of mechanical contacts 10 which perform the ultimate desired switching function. Since the relay is electromechanical and a substantial mechanical force involved, the coil energy requirement is substantial. Accordingly it is often desirable to supply the energy by way of a transistor amplifier. In this way a relatively small toggle current at terminal 8 can suffice for reliable relay operation.
While not shown, suitable conventional circuitry will be connected to terminal 8. This can be in the form of switching elements and can if desired be conventional digital logic circuit devices.
In FIG. 1 transistors 12 and 13 are Darlington connected to drive relay coil 11 in a common-emitter circuit. Typically the supply voltage, V CC will be slightly greater than the voltage required by coil 11. In the off state, transistor 12 must support the full V CC and collectoremitter voltage breakdown must exceed V CC by a safe factor. For example in a circuit rated at 50 volts an output device rated at 56 volts minimum could be used.
In typical prior art circuits a diode or large capacitor would ordinarily be connected across coil 11 to protect transistor 12 from damaging circuit transients. When relay 9 is energized a substantial current flows. When this current is interrupted, as by turning transistor 12 off, the inductive action of coil 11 can generate a voltage spike that can easily damage the transistor. If a diode is connected across coil 11 and poled to conduct on the voltage spike, the spike will be arrested. A large value shunt capacitor will also arrest the spike. However either the diode or capacitor can prolong the relay drop-out time excessively and at best add an external circuit component. One prior art solution to the problem has been to connect a zener diode between collector and base of transistor 12. The zener breakdown is chosen to be slightly below the collector emitter breakdown of transistor 12 yet greater than the desired operating voltage. Thus when the inductive spike rises above the zener breakdown, transistor 12 is turned on briefly so as to absorb the spike energy but in an active mode rather than in breakdown. This action can rapidly absorb the spike and yet protect the transistor. However the problem of matching a zener diode to the transistor is difficult. The resolution to this matching problem has been to use a series array of zener diodes made from diffused transistor base emitters. These diodes break down at about 6 volts so that in a transistor having a 60 volt breakdown, 9 such 6-volt diodes would produce a 54-volt rated circuit. However the nine series connected diodes also presents a fabrication problem.
As shown in the circuit of FIG. 1 a protective transistor 15 is connected between base and collector of transistor 12. In 15 only the emitter and collector are connected, the base being left open. Transistor 15 is selected to be a match for transistor 12 except for having a slightly greater current amplification between base and collector, or Beta. This means that transistor 15 will have a breakdown voltage that is slightly lower than that of transistor 12. Thus transistor 15 acts like a zener diode having a breakdown slightly lower than that of transistor 12 thereby providing the desired protection.
Furthermore if transistor 13 is of the same construction as transistor 12 except for having a smaller area, transistor 15 will protect transistors 13 and 12 from damage from voltage spikes at terminal 14 caused by the inductive load.
Resistor 15 is present in the circuit to control operating bias. When transistors 13 and 15 are in a low conduction state resistors 15 ensures that transistor 12 will be turned off.
FIG. 2 shows a circuit that functions as does the circuit of FIG. 1. However, instead of connecting the relay coil to the collector of transistor 12, the relay coil 10 is connected between the emitter of transistor 12 and the negative power supply terminal -V CC . The positive or grounded terminal +V CC is connected to the collector of transistor 12. The circuit operating characteristics of FIGS. 1 and 2 are identical and both versions are shown to indicate that only the series relationship between the relay coil 10 and the power supply are critical.
While the schematics of FIGS. 1 and 2 show a ground terminal, this is done for the convenience of the circuitry (not shown) that drives terminal 8. As a practical matter as long as suitable drive circuitry is used and conventionally connected, the ground could be omitted entirely or it could be place at any desired circuit node.
While the circuit of FIGS. 1 and 2 can be realized using discrete components the advantages can best be realized in integrated circuit (IC) form.
FIG. 3 shows a three element composite transistor structure using the invention. FIG. 4 is a sectional view of the upper portion designated as the line 4--4 in FIG. 3. These two figures should be considered together in the following description.
In the IC process, the starting material is a wafer 20 of p-type silicon. A heavily doped N-type buried layer 21 is established in the conventional manner to lie under the device trio to be described. A common buried layer is feasible because all three collectors are common. The wafer, with its buried layer inserts, is over coated with an epitaxial layer 22 of N-type silicon having a resistivity suitable for transistor collectors.
An isolation ring 23 of heavily doped p-type material extends completely through the epitaxial layer and is designed to isolate the common transistors as a unit. Collector contact diffusion 30 is of heavy N-type doping that extends through epitaxial layer 22 to contact buried layer 21. As can be seen from FIG. 3, this diffusion creates three separate transistor areas.
It is to be understood that the drawing is not to scale, but is expanded where appropriate to better show structural details. Also while only the region of transistors 12, 13, and 15 of FIG. 1 is illustrated, other associated IC devices may be fabricated into the silicon material to form a complete functional circuit. The oxide film, used in the planar device fabrication process, and the overlying metalization layer have been omitted to show the topographical details. Since the planar process is well known, the process details will be omitted in the following description.
Transistor base diffusions are shown at 24, 25, and 26. FIG. 3 shows where the junctions produced by the diffusions intersect the surface and FIG. 4 shows the cross section of diffusions 25 and 26. A transistor emitter diffusion produces the junction at 27 and is heavily doped N-type. This diffusion almost fills base diffusion 25. This can be done because transistor 15 needs no base contact. The emitter of transistor 12 is actually a series of separate emitters 28 of small area that will ultimately be parallel connected and are located inside base diffusion 24. The emitter of transistor 13 is also composed of separate emitters 29 of small area inside base diffusion 26. Emitters 29 will ultimately be connected in parallel and to the base region 24 of transistor 12. It will be noted that the drawing shows six emitters in transistors 13 and forty emitters in transistors 12. Since the individual emitters of transistors 12 and 13 are the same size these devices will have the same characteristics except for total collector current rating. However, transistor 15 has a much larger emitter diffusion area 27. In the planar process, in terms of impurity penetration, a large area diffusion will penetrate more at the center than will the centers of the smaller areas. This means that diffusion 27 will tend to approach the base diffusion depths more clearly than will diffusions 29 or 28. Accordingly transistor 15 will have a greater Beta and a collector-to-emitter voltage breakdown correspondingly lower then the breakdown voltages of transistors 12 and 13 which, due to similar emitter geometries, will be substantially the same. It has been found that circuits can be manufactured where transistors 15 will have a breakdown of 65 volts whereas transistors 12 and 13 break down at 75 volts. Clearly whatever the voltage breakdown for transistors 12 and 13, transistor 15 will be lower by virtue of physical design and the fact that all three devices are fabricated simultaneously in adjacent silicon areas. Thus the desired characteristics are self tracking because of the process. Also, because of the proximity, any thermal effects will tend to act equally on all three devices which will therefore tend to track.
Diffusion 30 represents a collector contact diffusion. This provides an ohmic low resistance connection via buried layer 21 to the collector regions of all three transistors. Since the collectors are all connected together, region 30 is a single continuous diffusion region surrounding the three transistors.
While not shown, the silicon surface is coated with the conventional planar oxide and a metalization layer that makes contact through holes etched in the oxide to the diffused emitter base and collector electrodes. The metal is contoured so that emitters 28 are parallel connected by means of a series of eight fingers. Base metal contact fingers interdigitate the emitter metal contacts and connect to parallel connected emitters 29 as well as to emitter 27. A metal base finger paralleling emitters 29 would comprise the circuit input terminal 8.
Resistor 15 could be in the form of the resistive metalization or, in planar diffused form, in the silicon substrate outside of isolation ring 23.
The invention has been described as an electronic circuit and its preferred IC form detailed. Clearly there are equivalents and modifications that will occur to a person skilled in the art. For example, while a version using NPN transistors has been shown, PNP structures could be used, along with reversed power supply connections. Furthermore while a Darlington structure is shown, the protective transistor could be used with a single power output transistor. While FIGS. 3 and 4 show the preferred embodiment, wherein a single isolation region contains the active transistors, each transistor could be separately fabricated inside a p-type isolation diffusion and then interconected as desired solely by metalization. Finally, other drive circuitry could be used. Accordingly it is intended that the invention be limited only by the following claims. | A transistor, used in the switching of current in an inductive load, is protected by a similar transistor connected between collector and base. The protective transistor has a lower breakdown voltage than the transistor being protected. When the inductive load produces a voltage surge, the protective transistor breaks down first and turns the protected transistor on so that the surge is absorbed in an active transistor not in breakdown and therefore capable of dissipating the surge without damage. Since the surge is arrested at high voltage the time required to complete the arrest is shortened. | 7 |
[0001] This application claims the benefit of U.S. Provisional Patent Application Ser. No. 60/610,675 filed Sep. 17, 2004 entitled “Unmanned, Vandal-Resistant, Self-Contained, Tower-Based, Wireless, Solar-Powered Surveillance Unit and System,” and it is hereby incorporated by reference in its entirety.
FIELD OF THE INVENTION
[0002] The invention relates to surveillance systems. More specifically, the invention relates to an unmanned, vandal-resistant, self-contained, tower-based, wireless, solar-powered surveillance unit, in which the tower is supported by a heavy but preferably portable base. The invention also relates to a local network that may include one or more of such tower-based surveillance units. The invention also relates to a wide area network, such as the Internet, that may include one or more of such local networks.
BACKGROUND OF THE INVENTION
[0003] Unmanned surveillance systems for monitoring sites remote from a monitoring location are well known. Tower-based systems are disclosed, for example, in U.S. Pat. Nos. 6,375,370; 6,585,428; 6,709,171; and 6,709,172. Each of said patents are hereby incorporated by reference in its entirety. The surveillance systems disclosed in said four patents employ a tower support base having a hollow enclosure that houses various equipment related to the operation of the surveillance system. In order to enhance the vandalism resistance of a tower-based surveillance system, it would be desirable to locate all components of the surveillance system on the tower at a height sufficient to render them difficult to access rather than locating at least some of them at ground level. It would also be desirable to provide a tower-based surveillance system that is totally self-contained (e.g., wireless and solar powered) in order further to enhance vandalism resistance.
SUMMARY OF THE INVENTION
[0004] Aspects of the present invention include an improved unmanned tower-based surveillance unit for monitoring sites remote from a monitoring location, such units being self-contained, solar-powered, and wireless. All components relating to operation of the surveillance unit are located on the tower at a height sufficient to render them difficult to access from the ground. Each unit may be part of a local network of one or more surveillance units that communicate wirelessly with one or more central transmitting and receiving sites, each of which may include monitoring facilities. The local network may be part of a wide-area network, such as the Internet, for example, in order to allow monitoring access, for example, at locations other than at central sites such as at the home or business of a client of an organization that provides remote surveillance monitoring. Such access may employ well-known Internet Transmission Control Protocol/Internet Protocol (TCP/IP) techniques. The assignee of the present invention has adopted the trademarks “Wireless Surveillance over IP” and “WSoIP” for such surveillance monitoring.
BRIEF DESCRIPTION OF THE DRAWINGS
[0005] FIG. 1 is a perspective view of an exemplary embodiment of a tower and base having components affixed thereto that together provide a wireless, solar-powered surveillance unit in accordance with aspects of the present invention.
[0006] FIG. 2 is a close-up perspective view of the tower base of the surveillance unit embodiment of FIG. 1 .
[0007] FIG. 3 is close-up perspective view of a portion of the surveillance unit embodiment of FIG. 1 , showing solar panels and an enclosure for related equipment in greater detail.
[0008] FIG. 4 is a close-up perspective view of the solar panels and enclosure of FIG. 3 from a different vantage point from which the underside of the solar panels is seen.
[0009] FIG. 5 is a close-up perspective view of a portion of the surveillance unit embodiment of FIG. 1 , showing antennas, a camera housing, and an enclosure for related equipment in greater detail.
[0010] FIG. 6 is a conceptual schematic diagram showing a local network and wide-area network, such as the Internet, in which a wireless, solar-powered surveillance unit in accordance with aspects of the present invention may be advantageously employed.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0011] An embodiment of a tower-based surveillance unit 2 that includes various aspects of the present invention will now be described in connection with FIGS. 1 through 5 . A telescoping tubular tower 4 is supported by a heavy concrete base 6 . Although a telescoping tubular tower configuration provides a convenient support for components of the surveillance unit, it is not critical to the invention and other tower configurations may be employed. Alternative tower configurations include, for example, a fixed tubular tower, a telescoping lattice tower, and a fixed lattice tower. If a telescoping or fixed lattice tower is employed, they should employ appropriate coverings to discourage climbing. The heavy tower base may be a non-penetrating (i.e., it does not penetrate the earth) concrete base, for example, having a weight sufficient to support the tower attached to it, while permitting transportation by suitable heavy equipment but which discourages vandalism. Although a 9,000 pound base has been found to be suitable, the weight is not critical and much lighter weights may be usable provided that they cannot be readily moved manually and provide sufficient support for the tower. For some applications, a mobile trailer mounted tower may be acceptable. The tower height is not critical, provided that it is sufficient to allow the various surveillance unit components to be mounted so as to render them difficult to access from the ground and to place the surveillance unit's observation component(s) sufficiently high to observe the site. In the example shown in the figures, the tower height is 70 feet. In practice, a tower height of at least 15 or 20 feet may be required to assure that the lowest components are not reachable from the ground. A tower height of as much as 100 feet may be usable. Although a tilt-over telescoping tubular tower is shown in the figures (see particularly FIGS. 1 and 2 ), this is not critical to the invention and the tower need not be so configured.
[0012] Components mounted on the tower include a set of solar panels 8 and an enclosure 10 for equipment associated with the solar panels. Such equipment in enclosure 10 may include, for example, one or more batteries and circuits for regulating the charging of such batteries by the solar panels. Such arrangements are well known. The equipment may also include, for example, voltage regulators and circuit breakers useful in providing power from the batteries to other components mounted on the tower. Such arrangements for providing power from solar-charged batteries are also well known. Enclosure 10 should be water-tight to protect the equipment contained within it (while providing appropriate venting for cooling, if necessary). Various cables are shown connecting the solar panels to the enclosure and connecting the enclosure to components located higher on the tower. It will be noted that the enclosure 10 is located well above the ground, about twenty feet in this example, and that no cables run downward from the enclosure. Due to their large windload, it is desirable to locate the solar panels below other components on the tower.
[0013] A self-guying arrangement 12 that includes a pair of cross arms is located above the solar panels 8 in order to stiffen the tubular tower and increase its height and wind-load capability. Such a self-guying arrangement is not a necessary aspect of the present invention.
[0014] At and near the top of the tower 4 and above the self-guying arrangement 12 , observation, radio communication, and, optionally, control components are mounted. In this example, a downward-viewing video camera is located within an enclosure 14 supported by an outward- and downward-extending arm 16 . The enclosure 14 includes a transparent cover 18 through which the camera may view the site. The transparent cover and camera enclosure may be impact resistant. Although only one camera support and housing is shown, multiple observation components may be employed. Although this example employs a video camera, such as a high-resolution video camera of the type used for wired CCTV applications, other types of observation components may be employed instead of or in addition to a video camera—for example, a still camera, a microphone, a motion detector, and/or lights. Two antennas are shown, a directional antenna 20 and an omni-directional antenna 22 . Various antennas and antenna configurations may be employed depending on the communications requirements. Electronics, including one or more transmitters or transceivers associated with the video camera and antennas are housed in an enclosure 24 . Various cables are shown connecting the video camera and the antennas to the enclosure. Arrangements for operating transmitters or transceivers with observation devices and associated antennas are well known. In addition to transmitting information from the observation devices, a transceiver may permit instructions to be received in order to control the one or more observation devices (e.g., to power them on and off, to control their direction, etc.). Enclosure 24 should be water-tight to protect the equipment contained within it (while providing appropriate venting for cooling, if necessary).
[0015] One possible network surveillance arrangement is shown in FIG. 6 . A first surveillance unit 2 - 1 is shown in communication with a central receiving (or receiving and transmitting) site 30 . Second and third surveillance units 2 - 2 and 2 - 3 , respectively, are shown in communication with a central receiving (or receiving and transmitting) site 32 . Maximum distances from a remote unit to a central site may be about fifteen miles, depending on terrain, antenna gain, frequency, and transmitter power. The central sites 30 and 32 are shown in communication with one another via a high speed wireless bridge. Each central site may have its own monitoring facility that includes, for example, one or more computers with monitors ( 34 and 36 ) for use by human operators, an NVR (Networked Video Recording) server 38 and a mail server 40 . The NVR server may operate in conjunction with one or more suitable video recording devices, for example, for recording video images received from remote surveillance units. Such arrangements are well known in closed circuit television (CCTV) surveillance systems. In addition to receiving observation information, such as video images, from the remote surveillance units, the central sites may also send information or instructions to ones of the remote surveillance units either automatically or under the control of one or more human operators. Such outward transmissions may, for example, turn various observation units on or off or may change their direction of observation. One of the central sites 30 is shown connected via a firewall 42 , a symmetrical DSL modem 44 , and a high speed Internet connection (DSL, T1, cable, etc.) to the Internet. Using TCP/IP technology, the remote observation information may then be available to one or more client users 46 . As noted above, the assignee of the present invention has adopted the trademarks “Wireless Surveillance over IP” and “WSoIP” for such surveillance monitoring. | A self-contained surveillance unit includes a climb-resistant tower and a heavy, but portable, base supporting the tower. The tower has various components affixed thereto. All components sufficient for operation of the surveillance unit, including observation, wireless-communication and self-powering components, are located on the tower well above the ground at a height sufficient to render them difficult to access from the ground. At least one such self-contained surveillance unit may form part of a surveillance communications network in which the network also has one or more central transmitting and receiving sites having monitoring facilities. | 6 |
FIELD OF THE INVENTION
[0001] This invention relates to novel succinoylamino heterocycles having drug and bio-affecting properties, their pharmaceutical compositions and methods of use. These novel compounds inhibit the processing of amyloid precursor protein and, more specifically, inhibit the production of Aβ-peptide, thereby acting to prevent the formation of neurological deposits of amyloid protein. More particularly, the present invention relates to the treatment of neurological disorders related to β-amyloid production such as Alzheimer's disease and Down's Syndrome.
BACKGROUND OF THE INVENTION
[0002] Alzheimer's disease (AD) is a degenerative brain disorder characterized clinically by progressive loss of memory, temporal and local orientation, cognition, reasoning, judgment and emotional stability. AD is a common cause of progressive dementia in humans and is one of the major causes of death in the United States. AD has been observed in all races and ethnic groups worldwide, and is a major present and future health problem. No treatment that effectively prevents AD or reverses the clinical symptoms and underlying pathophysiology is currently available (for review, Dennis J. Selkoe; Cell Biology of the amyloid (beta)-protein precursor and the mechanism of Alzheimer's disease, Annu Rev Cell Biol, 1994, 10: 373-403).
[0003] Histopathological examination of brain tissue derived upon autopsy or from neurosurgical specimens in effected individuals revealed the occurrence of amyloid plaques and neurofibrillar tangles in the cerebral cortex of such patients. Similar alterations were observed in patients with Trisomy 21 (Down's syndrome), and hereditary cerebral hemorrhage with amyloidosis of the Dutch-type. Neurofibrillar tangles are nonmembrane-bound bundles of abnormal proteinaceous filaments and biochemical and immunochemical studies led to the conclusion that their principle protein subunit is an altered phosphorylated form of the tau protein (reviewed in Selkoe, 1994).
[0004] Biochemical and immunological studies revealed that the dominant proteinaceous component of the amyloid plaque is an approximately 4.2 kilodalton (kD) protein of about 39 to 43 amino acids. This protein was designated Aβ, β-amyloid peptide, and sometimes β/A4; referred to herein as Aβ. In addition to deposition of Aβ in amyloid plaques, Aβ is also found in the walls of meningeal and parenchymal arterioles, small arteries, capillaries, and sometimes, venules. Aβ was first purified, and a partial amino acid reported, in 1984 (Glenner and Wong, Biochem. Biophys. Res. Commun. 120: 885-890). The isolation and sequence data for the first 28 amino acids are described in U.S. Pat. No. 4,666,829.
[0005] Compelling evidence accumulated during the last decade revealed that Aβ is an internal polypeptide derived from a type 1 integral membrane protein, termed β amyloid precursor protein (APP). β APP is normally produced by many cells both in vivo and in cultured cells, derived from various animals and humans. Aβ is derived from cleavage of β APP by as yet unknown enzyme (protease) system(s), collectively termed secretases.
[0006] The existence of at least four proteolytic activities has been postulated. They include β secretase(s), generating the N-terminus of Aβ, a secretase(s) cleaving around the 16/17 peptide bond in Aβ, and γ secretases, generating C-terminal Aβ fragments ending at position 38, 39, 40, 42, and 43 or generating C-terminal extended precursors which are subsequently truncated to the above polypeptides.
[0007] Several lines of evidence suggest that abnormal accumulation of Aβ plays a key role in the pathogenesis of AD. Firstly, Aβ is the major protein found in amyloid plaques. Secondly, Aβ is neurotoxic and may be causally related to neuronal death observed in AD patients. Thirdly, missense DNA mutations at position 717 in the 770 isoform of β APP can be found in effected members but not unaffected members of several families with a genetically determined (familiar) form of AD. In addition, several other β APP mutations have been described in familiar forms of AD. Fourthly, similar neuropathological changes have been observed in transgenic animals overexpressing mutant forms of human β APP. Fifthly, individuals with Down's syndrome have an increased gene dosage of β APP and develop early-onset AD. Taken together, these observations strongly suggest that Aβ depositions may be causally related to the AD.
[0008] It is hypothesized that inhibiting the production of Aβ will prevent and reduce neurological degeneration, by controlling the formation of amyloid plaques, reducing neurotoxicity and, generally, mediating the pathology associated with Aβ production. One method of treatment methods would therefore be based on drugs that inhibit the formation of Aβ in vivo.
[0009] Methods of treatment could target the formation of Aβ through the enzymes involved in the proteolytic processing of β amyloid precursor protein. Compounds that inhibit β or γ secretase activity, either directly or indirectly, could control the production of Aβ. Advantageously, compounds that specifically target γ secretases, could control the production of Aβ. Such inhibition of β or γ secretases could thereby reduce production of Aβ, which, thereby, could reduce or prevent the neurological disorders associated with Aβ protein.
[0010] PCT publication number WO 96/29313 discloses the general formula:
[0011] covering metalloprotease inhibiting compounds useful for the treatment of diseases associated with excess and/or unwanted matrix metalloprotease activity, particularly collagenase and or stromelysin activity.
[0012] Compounds of general formula:
[0013] are disclosed in PCT publication number WO 95/22966 relating to matrix metalloprotease inhibitors. The compounds of the invention are useful for the treatment of conditions associated with the destruction of cartilage, including corneal ulceration, osteoporosis, periodontitis and cancer.
[0014] European Patent Application number EP 0652009A1 relates to the general formula:
[0015] and discloses compounds that are protease inhibitors that inhibit Aβ production.
[0016] U.S. Pat. No. 5,703,129 discloses the general formula:
[0017] which covers 5-amino-6-cyclohexyl-4-hydroxy-hexanamide derivatives that inhibit Aβ production and are useful in the treatment of Alzheimer's disease.
[0018] Thus there remains a need to develop compounds which are useful as inhibitors of the production of Aβ protein or pharmaceutically acceptable salts or prodrugs thereof, for the treatment of degenerative neurological disorders, such as Alzheimer's disease.
[0019] None of the above references teaches or suggests the compounds of the present invention which are described in detail below.
SUMMARY OF THE INVENTION
[0020] One object of the present invention is to provide novel compounds which are useful as inhibitors of the production of Aβ protein or pharmaceutically acceptable salts or prodrugs thereof.
[0021] It is another object of the present invention to provide pharmaceutical compositions comprising a pharmaceutically acceptable carrier and a therapeutically effective amount of at least one of the compounds of the present invention or a pharmaceutically acceptable salt or prodrug form thereof.
[0022] It is another object of the present invention to provide a method for treating degenerative neurological disorders comprising administering to a host in need of such treatment a therapeutically effective amount of at least one of the compounds of the present invention or a pharmaceutically acceptable salt or prodrug form thereof.
[0023] These and other objects, which will become apparent during the following detailed description, have been achieved by the inventors, discovery that compounds of Formula (I):
[0024] or pharmaceutically acceptable salt or prodrug forms thereof, wherein R 3 , R 3a , R 5 , R 5a , R 11 , t, B, L, and Z are defined below, are effective inhibitors of the production of Aβ protein.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0025] Thus, in a first embodiment, the present invention provides a novel compound of Formula (I):
[0026] or a pharmaceutically acceptable salt or prodrug thereof, wherein:
[0027] R 3 is —(CR 7 R 7a ) n —R 4 ,
[0028] —(CR 7 R 7a ) n —S—(CR 7 R 7a ) m —R 4 ,
[0029] —(CR 7 R 7a ) n —O—(CR 7 R 7a ) m —R 4 ,
[0030] —(CR 7 R 7a ) n —N(R 7b )—(CR 7 R 7a ) m —R 4 ,
[0031] —(CR 7 R 7a ) n —S(═O)—(CR 7 R 7a ) m —R 4 ,
[0032] —(CR 7 R 7a ) n —S(═O) 2 —(CR 7 R 7a ) m —R 4 ,
[0033] —(CR 7 R 7a ) n —C(═O)—(CR 7 R 7a ) m —R 4 ,
[0034] —(CR 7 R 7a ) n —N(R 7b )C(═O)—(CR 7 R 7a ) m —R 4 ,
[0035] —(CR 7 R 7a ) n —C(═O)N(R 7b )—(CR 7 R 7a ) m —R 4 ,
[0036] —(CR 7 R 7a ) n —N(R 7b )S(═O) 2 —(CR 7 R 7a ) m —R 4 , or
[0037] —(CR 7 R 7a ) n —S(═O) 2 N(R 7b )—(CR 7 R 7a ) m —R 4 ;
[0038] provided R 3 is not hydrogen when R 5 is hydrogen;
[0039] n is 0, 1, 2, or 3;
[0040] m is 0, 1, 2, or 3;
[0041] R 3a is H, OH, C 1 -C 4 alkyl, C 1 -C 4 alkoxy, C 2 -C 4 alkenyl, or C 2 -C 4 alkenyloxy;
[0042] alternatively, R 3 and R 3a , and the carbon to which they are attached, may be combined to form a 3-8 membered cycloalkyl moiety substituted with 0-2 R 4b ; provided that R 5 and R 5a are not combined to form a 3-8 membered cycloalkyl moiety;
[0043] R 4 is H, OH, OR 14a ,
[0044] C 1 -C 6 alkyl substituted with 0-3 R 4a ,
[0045] C 2 -C 6 alkenyl substituted with 0-3 R 4a ,
[0046] C 2 -C 6 alkynyl substituted with 0-3 R 4a ,
[0047] C 3 -C 10 carbocycle substituted with 0-3 R 4b ,
[0048] C 6 -C 10 aryl substituted with 0-3 R 4b , or
[0049] 5 to 10 membered heterocycle substituted with 0-3 R 4b ;
[0050] R 4a , at each occurrence, is independently selected from: H,
[0051] F, Cl, Br, I, CF 3 ,
[0052] C 3 -C 10 carbocycle substituted with 0-3 R 4b ,
[0053] C 6 -C 10 aryl substituted with 0-3 R 4b , or
[0054] 5 to 10 membered heterocycle substituted with 0-3 R 4b ;
[0055] R 4b , at each occurrence, is independently selected from:
[0056] H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl,
[0057] SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy,
[0058] C 1 -C 4 haloalkyl, C 1 -C 4 haloalkoxy, and C 1 -C 4
[0059] halothioalkoxy;
[0060] R 5 is H, OR 14 ;
[0061] C 1 -C 6 alkyl substituted with 0-3 R 5b ;
[0062] C 1 -C 6 alkoxy substituted with 0-3 R 5b ;
[0063] C 2 -C 6 alkenyl substituted with 0-3 R 5b ;
[0064] C 2 -C 6 alkynyl substituted with 0-3 R 5b ;
[0065] C 3 -C 10 carbocycle substituted with 0-3 R 5c ;
[0066] C 6 -C 10 aryl substituted with 0-3 R 5c ; or
[0067] 5 to 10 membered heterocycle substituted with 0-3 R 5c ;
[0068] provided R 5 is not hydrogen when R 3 is hydrogen;
[0069] R 5a is H, OH, C 1 -C 4 alkyl, C 1 -C 4 alkoxy, C 2 -C 4 alkenyl, or C 2 -C 4 alkenyloxy;
[0070] R 5b , at each occurrence, is independently selected from:
[0071] H, C 1 -C 6 alkyl, CF 3 , OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 ;
[0072] C 3 -C 10 carbocycle substituted with 0-3 R 5c ;
[0073] C 6 -C 10 aryl substituted with 0-3 R 5c ; or
[0074] 5 to 10 membered heterocycle substituted with 0-3 R 5c ;
[0075] R 5c , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, C 1 -C 4 haloalkoxy, and C 1 -C 4 halothioalkoxy;
[0076] alternatively, R 5 and R 5a , and the carbon to which they are attached, may be combined to form a 3-8 membered cycloalkyl moiety substituted with 0-2 R 5b ; provided that R 3 and R 3a are not combined to form a 3-8 membered cycloalkyl moiety;
[0077] R 7 , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , CF 3 , and C 1 -C 4 alkyl;
[0078] R 7a , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , CF 3 , aryl and C 1 -C 4 alkyl;
[0079] R 7b is independently selected from H and C 1 -C 4 alkyl;
[0080] L is a bond, C 1 -C 4 alkyl, C 2 -C 4 alkenyl, C 2 -C 4 alkynyl, —(CH 2 ) p —O—(CH 2 ) q —, or —(CH 2 ) p —NR 10 —(CH 2 ) q —;
[0081] p is 0, 1, 2, or 3;
[0082] q is 0, 1, 2, or 3;
[0083] Z is C 3 -C 10 carbocycle substituted with 0-2 R 12b ;
[0084] C 6 -C 10 aryl substituted with 0-4 R 12b ; and
[0085] 5 to 10 membered heterocycle substituted with 0-5 R 12b , wherein the heterocycle contains 1, 2, 3 or 4 heteroatoms selected from N, O and S;
[0086] R 12b , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, C 1 -C 4 haloalkoxy, C 1 -C 4 halothioalkoxy, aryl substituted with 0-4 R 12c ;
[0087] R 12c , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, C 1 -C 4 haloalkoxy, and C 1 -C 4 halothioalkoxy;
[0088] B is a 4 to 8 membered amino-heterocyclic ring, comprising one N atom, 3 to 7 carbon atoms, and optionally, an additional heteroatom selected from —O—, —S—, —S(═O)—, —S(═O) 2 —, and —N(R LZ )—;
[0089] wherein the amino-heterocyclic ring is saturated or partially saturated; and
[0090] wherein R LZ is either R 10 or the substituent —L—Z;
[0091] R 10 is H, C(═O)R 17 , C(═O)OR 17 , —(C 1 -C 3 alkyl)—C(═O)OR 17 , C(═O)NR 18 R 19 , S(═O) 2 NR 18 R 19 , S(═O) 2 R 17 ;
[0092] C 1 -C 6 alkyl substituted with 0-2 R 10a ;
[0093] C 6 -C 10 aryl substituted with 0-4 R 10b ;
[0094] C 3 -C 10 carbocycle substituted with 0-3 R 10b ; or
[0095] 5 to 10 membered heterocycle optionally substituted with 0-3 R 10b ;
[0096] R 10a , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 , CF 3 , or aryl substituted with 0-4 R 10b ;
[0097] R 10b , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, C 1 -C 4 alkoxy, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, C 1 -C 4 haloalkoxy, and C 1 -C 4 halothioalkoxy;
[0098] R 11 , at each occurrence, is independently selected from:
[0099] C 1 -C 4 alkoxy, Cl, F, Br, I, —OH, CN, NO 2 , NR 18 R 19 , C(═O)R 17 , C(═O)OR 17 , C(═O)NR 18 R 19 , S(═O) 2 NR 18 R 19 , CF 3 ;
[0100] C 1 -C 6 alkyl substituted with 0-1 R 11a ;
[0101] C 6 -C 10 aryl substituted with 0-3 R 11b ;
[0102] C 3 -C 10 carbocycle substituted with 0-3 R 11b ; or
[0103] 5 to 10 membered heterocycle substituted with 0-3 R 11b ;
[0104] alternatively, two R 11 substituents on the same or adjacent carbon atoms may be combined to form a C 3 -C 6 carbocycle or a benzo fused radical, wherein said carbocycle or benzo fused radical is substituted with 0-4 R 13 ;
[0105] additionally, two R 11 substituents on adjacent atoms may be combined to form a 5 to 6 membered heteroaryl fused radical, wherein said 5 to 6 membered heteroaryl fused radical comprises 1 or 2 heteroatoms selected from N, O, and S; wherein said 5 to 6 membered heteroaryl fused radical is substituted with 0-3 R 13 ;
[0106] R 11a , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 , CF 3 , or phenyl substituted with 0-3 R 11b ;
[0107] R 11b , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, C 1 -C 4 haloalkoxy, and C 1 -C 4 halothioalkoxy;
[0108] t is 0, 1, 2 or 3;
[0109] R 13 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, C 1 -C 4 alkoxy, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , and CF 3 ;
[0110] R 14 , at each occurrence, is independently selected from: H, phenyl, benzyl, C 1 -C 6 alkyl, or C 2 -C 6 alkoxyalkyl;
[0111] R 14a is H, phenyl, benzyl, or C 1 -C 4 alkyl;
[0112] R 15 , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl), —S(═O) 2 —(C 1 -C 6 alkyl), and aryl;
[0113] R 16 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl) and —S(═O) 2 —(C 1 -C 6 alkyl);
[0114] alternatively, R 15 and R 16 on the same N atom may be combined to form a 5 to 6 membered heterocyclic fused radical, wherein said 5 to 6 membered heterocyclic fused radical comprises 1 or 2 heteroatoms selected from N and O;
[0115] R 17 is H, aryl, aryl-CH 2 —, C 1 -C 6 alkyl, or C 2 -C 6 alkoxyalkyl;
[0116] R 18 , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl) and —S(═O) 2 —(C 1 -C 6 alkyl);
[0117] R 19 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, phenyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl) —S(═O) 2 —(C 1 -C 6 alkyl); and
[0118] alternatively, R 18 and R 19 on the same N atom may be combined to form a 5 to 6 membered heterocyclic fused radical, wherein said 5 to 6 membered heterocyclic fused radical comprises 1 or 2 heteroatoms selected from N and O.
[0119] [2] In a preferred embodiment the present provides a compound of Formula (I) wherein:
[0120] R 3 is —(CR 7 R 7a ) n —R 4 ,
[0121] —(CR 7 R 7a ) n —S—(CR 7 R 7a ) m —R 4 ,
[0122] —(CR 7 R 7a ) n —O—(CR 7 R 7a ) m —R 4 ,
[0123] —(CR 7 R 7a ) n —N(R 7b )—(CR 7 R 7a ) m —R 4 ,
[0124] —(CR 7 R 7a ) n —S(═O)—(CR 7 R 7a ) m —R 4 ,
[0125] —(CR 7 R 7a ) n —S(═O) 2 —(CR 7 R 7a ) m —R 4 ,
[0126] —(CR 7 R 7a ) n —C(═O)—(CR 7 R 7a ) m —R 4 ,
[0127] —(CR 7 R 7a ) n —NHC(═O)—(CR 7 R 7a ) m —R 4 ,
[0128] —(CR 7 R 7a ) n —C(═O)NH—(CR 7 R 7a ) m —R 4 ,
[0129] —(CR 7 R 7a ) n —NHS(═O) 2 —(CR 7 R 7a ) m —R 4 , or
[0130] —(CR 7 R 7a ) n —S(═O) 2 NH—(CR 7 R 7a ) m —R 4 ;
[0131] provided R 3 is not hydrogen when R 5 is hydrogen;
[0132] n is 0, 1, 2, or 3;
[0133] m is 0, 1, 2, or 3;
[0134] R 3a is H, OH, C 1 -C 4 alkyl, C 1 -C 4 alkoxy, C 2 -C 4 alkenyl, or C 2 -C 4 alkenyloxy;
[0135] alternatively, R 3 and R 3a , and the carbon to which they are attached, may be combined to form a 3-8 membered cycloalkyl moiety substituted with 0-1 R 4b ; provided that R 5 and R 5a are not combined to form a 3-8 membered cycloalkyl moiety;
[0136] R 4 is H, OH, OR 14a ,
[0137] C 1 -C 6 alkyl substituted with 0-3 R 4a ,
[0138] C 2 -C 6 alkenyl substituted with 0-3 R 4a ,
[0139] C 2 -C 6 alkynyl substituted with 0-3 R 4a ,
[0140] C 3 -C 10 carbocycle substituted with 0-3 R 4b ,
[0141] C 6 -C 10 aryl substituted with 0-3 R 4b , or
[0142] 5 to 10 membered heterocycle substituted with 0-3 R 4b ;
[0143] R 4a , at each occurrence, is independently selected from: H,
[0144] F, Cl, Br, I, CF 3 ,
[0145] C 3 -C 10 carbocycle substituted with 0-3 R 4b ,
[0146] C 6 -C 10 aryl substituted with 0-3 R 4b , or
[0147] 5 to 10 membered heterocycle substituted with 0-3 R 4b ;
[0148] R 4b , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, and C 1 -C 4 halothioalkoxy;
[0149] R 5 is H, OR 14 ;
[0150] C 1 -C 6 alkyl substituted with 0-3 R 5b ;
[0151] C 1 -C 6 alkoxy substituted with 0-3 R 5b ;
[0152] C 2 -C 6 alkenyl substituted with 0-3 R 5b ;
[0153] C 2 -C 6 alkynyl substituted with 0-3 R 5b ;
[0154] C 3 -C 10 carbocycle substituted with 0-3 R 5c ;
[0155] C 6 -C 10 aryl substituted with 0-3 R 5c ; or
[0156] 5 to 10 membered heterocycle substituted with 0-3 R 5c ;
[0157] provided R 5 is not hydrogen when R 3 is hydrogen;
[0158] R 5a is H, OH, methyl, ethyl, propyl, butyl, methoxy, ethoxy, propoxy, butoxy, or allyl;
[0159] R 5b , at each occurrence, is independently selected from:
[0160] H, C 1 -C 6 alkyl, CF 3 , OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 ;
[0161] C 3 -C 10 carbocycle substituted with 0-3 R 5c ;
[0162] C 6 -C 10 aryl substituted with 0-3 R 5c ; or
[0163] 5 to 10 membered heterocycle substituted with 0-3 R 5c ;
[0164] R 5c , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, and C 1 -C 4 haloalkoxy;
[0165] alternatively, R 5 and R 5a , and the carbon to which they are attached, may be combined to form a 3-8 membered cycloalkyl moiety substituted with 0-1 R 5b ; provided that R 3 and R 3a are not combined to form a 3-8 membered cycloalkyl moiety;
[0166] R 7 , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , CF 3 , and C 1 -C 4 alkyl;
[0167] R 7a , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , CF 3 , aryl and C 1 -C 4 alkyl;
[0168] R 7b is independently selected from H and C 1 -C 4 alkyl;
[0169] L is a bond, C 1 -C 4 alkyl, C 2 -C 4 alkenyl, C 2 -C 4 alkynyl, —(CH 2 ) p —O—(CH 2 ) q —, or —(CH 2 ) p —NR 10 —(CH 2 ) q —;
[0170] p is 0, 1, 2, or 3;
[0171] q is 0, 1, 2, or 3;
[0172] Z is C 3 -C 10 carbocycle substituted with 0-2 R 12b ;
[0173] C 6 -C 10 aryl substituted with 0-4 R 12b ; and
[0174] 5 to 10 membered heterocycle substituted with 0-5 R 12b , wherein the heterocycle contains 1, 2, 3 or 4 heteroatoms selected from N, O and S;
[0175] R 12b , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, C 1 -C 4 haloalkoxy, aryl substituted with 0-4 R 12c ;
[0176] R 12c , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, and C 1 -C 4 haloalkoxy;
[0177] B is a 4 to 8 membered amino-heterocyclic ring, comprising one N atom, 3 to 7 carbon atoms, and optionally, an additional heteroatom selected from —O—, —S—, —S(═O)—, —S(═O) 2 —, and —N(R LZ )—;
[0178] wherein the amino-heterocyclic ring is saturated or partially saturated; and
[0179] wherein R LZ is either R 10 or the substituent —L—Z;
[0180] R 10 is H, C(═O)R 17 , C(═O)OR 17 , —(C 1 -C 3 alkyl)—C(═O)OR 17 , C(═O)NR 18 R 19 , S(═O) 2 NR 18 R 19 , S(═O) 2 R 17 ;
[0181] C 1 -C 6 alkyl substituted with 0-2 R 10a ;
[0182] C 6 -C 10 aryl substituted with 0-4 R 10b ;
[0183] C 3 -C 10 carbocycle substituted with 0-3 R 10b ; or
[0184] 5 to 10 membered heterocycle optionally substituted with 0-3 R 10b ;
[0185] R 10a , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 , CF 3 , or aryl substituted with 0-4 R 10b ;
[0186] R 10b , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, C 1 -C 4 alkoxy, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 ;
[0187] R 11 , at each occurrence, is independently selected from:
[0188] C 1 -C 4 alkoxy, Cl, F, Br, I, —OH, CN, NO 2 , NR 18 R 19 , C(═O)R 17 , C(═O)OR 17 , C(═O)NR 18 R 19 , S(═O) 2 NR 18 R 19 , CF 3 ;
[0189] C 1 -C 6 alkyl substituted with 0-1 R 11a ;
[0190] C 6 -C 10 aryl substituted with 0-3 R 11b ;
[0191] C 3 -C 10 carbocycle substituted with 0-3 R 11b ; or
[0192] 5 to 10 membered heterocycle substituted with 0-3 R 11b ;
[0193] alternatively, two R 11 substituents on the same or adjacent carbon atoms may be combined to form a C 3 -C 6 carbocycle or a benzo fused radical wherein said benzo benzo fused radical is substituted with 0-4 R 13 ;
[0194] additionally, two R 11 substituents on adjacent atoms may be combined to form a 5 to 6 membered heteroaryl fused radical, wherein said 5 to 6 membered heteroaryl fused radical comprises 1 or 2 heteroatoms selected from N, O, and S; wherein said 5 to 6 membered heteroaryl fused radical is substituted with 0-3 R 13 ;
[0195] R 11a , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 , CF 3 , or phenyl substituted with 0-3 R 11b ;
[0196] R 11b , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkoxy, and C 1 -C 4 haloalkoxy;
[0197] t is 0, 1, 2 or 3;
[0198] R 13 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, C 1 -C 4 alkoxy, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , and CF 3 ;
[0199] R 14 is H, phenyl, benzyl, C 1 -C 6 alkyl, or C 2 -C 6 alkoxyalkyl;
[0200] R 14a is H, phenyl, benzyl, or C 1 -C 4 alkyl;
[0201] R 15 , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl) and —S(═O) 2 —(C 1 -C 6 alkyl), and aryl;
[0202] R 16 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl) and —S(═O) 2 —(C 1 -C 6 alkyl), and phenyl substituted with 0-3 R 13 ;
[0203] alternatively, R 15 and R 16 on the same N atom may be combined to form a 5 to 6 membered heterocyclic fused radical, wherein said 5 to 6 membered heterocyclic fused radical comprises 1 or 2 heteroatoms selected from N and O;
[0204] R 17 is H, aryl, (aryl)CH 2 —, C 1 -C 6 alkyl, or C 2 -C 6 alkoxyalkyl;
[0205] R 18 , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl) and —S(═O) 2 —(C 1 -C 6 alkyl);
[0206] R 19 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, phenyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl) and —S(═O) 2 —(C 1 -C 6 alkyl); and
[0207] alternatively, R 18 and R 19 on the same N atom may be combined to form a 5 to 6 membered heterocyclic fused radical, wherein said 5 to 6 membered heterocyclic fused radical comprises 1 or 2 heteroatoms selected from N and O.
[0208] [3] In a another preferred embodiment the present invention provides a compound of Formula (I) wherein:
[0209] R 3 is —(CHR 7 ) n —R 4 ,
[0210] —(CHR 7 ) n —S—(CHR 7 ) m —R 4 ,
[0211] —(CHR 7 ) n —O—(CHR 7 ) m —R 4 , or
[0212] —(CHR 7 ) n —N(R 7b )—(CHR 7 ) m —R 4 ;
[0213] provided R 3 is not hydrogen when R 5 is hydrogen;
[0214] n is 0, 1, or 2;
[0215] m is 0, 1, or 2;
[0216] R 3a is H;
[0217] alternatively, R 3 and R 3a , and the carbon to which they are attached, may be combined to form a cyclopropyl, cyclobutyl, cyclopentyl, or cyclohexyl moiety; provided that R 5 and R 5a are not combined to form a cycloalkyl moiety;
[0218] R 4 is H, OH, OR 14a ,
[0219] C 1 -C 4 alkyl substituted with 0-2 R 4a ,
[0220] C 2 -C 4 alkenyl substituted with 0-2 R 4a ,
[0221] C 2 -C 4 alkynyl substituted with 0-2 R 4a ,
[0222] C 3 -C 6 cycloalkyl substituted with 0-3 R 4b ,
[0223] phenyl substituted with 0-3 R 4b , or
[0224] 5 to 6 membered heterocycle substituted with 0-3 R 4b ;
[0225] R 4a , at each occurrence, is independently selected from: H,
[0226] F, Cl, Br, I CF 3 ,
[0227] C 3 -C 10 carbocycle substituted with 0-3 R 4b ,
[0228] phenyl substituted with 0-3 R 4b , or
[0229] 5 to 6 membered heterocycle substituted with 0-3 R 4b ;
[0230] R 4b , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, and C 1 -C 4 haloalkoxy;
[0231] R 5 is H, OR 14 ;
[0232] C 1 -C 6 alkyl substituted with 0-3 R 5b ;
[0233] C 2 -C 6 alkenyl substituted with 0-3 R 5b ;
[0234] C 2 -C 6 alkynyl substituted with 0-3 R 5b ;
[0235] C 3 -C 10 carbocycle substituted with 0-3 R 5c ;
[0236] C 6 -C 10 aryl substituted with 0-3 R 5c ; or
[0237] 5 to 10 membered heterocycle substituted with 0-3R 5c ;
[0238] provided R 5 is not hydrogen when R 3 is hydrogen;
[0239] R 5a is H;
[0240] R 5b , at each occurrence, is independently selected from:
[0241] H, C 1 -C 6 alkyl, CF 3 , OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 ;
[0242] C 3 -C 10 carbocycle substituted with 0-3 R 5c ;
[0243] C 6 -C 10 aryl substituted with 0-3 R 5c ; or
[0244] 5 to 10 membered heterocycle substituted with 0-3 R 5c ;
[0245] R 5c , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, and C 1 -C 4 haloalkoxy;
[0246] alternatively, R 5 and R 5a , and the carbon to which they are attached, may be combined to form a cyclopropyl, cyclobutyl, cyclopentyl, or cyclohexyl moiety; provided that R 3 and R 3a are not combined to form a cycloalkyl moiety;
[0247] R 7 , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , CF 3 , and C 1 -C 4 alkyl;
[0248] R 7b is independently selected from: H, methyl, ethyl, propyl, and butyl;
[0249] L is a bond, —CH 2 —, —CH 2 CH 2 —, —CH 2 CH 2 CH 2 —, —CH 2 CH═CH 2 , —(CH 2 ) p —O—(CH 2 ) q —, or —(CH 2 ) p —NR 10 —(CH 2 ) q —;
[0250] p is 0, 1, 2, or 3;
[0251] q is 0, 1, 2, or 3;
[0252] Z is C 3 -C 10 carbocycle substituted with 0-2 R 12b ;
[0253] C 6 -C 10 aryl substituted with 0-4 R 12b ; and
[0254] 5 to 10 membered heterocycle substituted with 0-5 R 12b , wherein the heterocycle contains 1, 2, 3 or 4 heteroatoms selected from N, O and S;
[0255] R 12b , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, C 1 -C 4 haloalkoxy, phenyl substituted with 0-3 R 12c ;
[0256] R 12c , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, and C 1 -C 4 haloalkoxy;
[0257] B is a 5, 6, or 7 membered amino-heterocyclic ring, comprising one N atom, 3 to 6 carbon atoms, and optionally, an additional heteroatom —N(R LZ )—;
[0258] wherein the amino-heterocyclic ring is saturated or partially saturated; and
[0259] wherein R LZ is either R 10 or the substituent —L—Z;
[0260] R 10 is H, C(═O)R 17 , C(═O)OR 17 , —(C 1 -C 3 alkyl)—C(═O)OR 17 ,
[0261] C(═O)NR 18 R 19 , S(═O) 2 NR 18 R 19 , S(═O) 2 R 17 ;
[0262] C 1 -C 6 alkyl substituted with 0-1 R 10a ;
[0263] C 6 -C 10 aryl substituted with 0-4 R 10b ;
[0264] C 3 -C 10 carbocycle substituted with 0-3 R 10b ; or
[0265] 5 to 10 membered heterocycle optionally substituted with 0-3 R 10b ;
[0266] R 10a , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 , CF 3 , or phenyl substituted with 0-4 R 10b ;
[0267] R 10b , at each occurrence, is independently selected from H, OH, C 1 -C 6 alkyl, C 1 -C 4 alkoxy, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , or CF 3 ;
[0268] R 11 , at each occurrence, is independently selected from:
[0269] C 1 -C 4 alkoxy, Cl, F, NR 18 R 19 , C(═O)R 17 , C(═O)OR 17 , C(═O)NR 18 R 19 , S(═O) 2 NR 18 R 19 , CF 3 ;
[0270] C 1 -C 6 alkyl substituted with 0-1 R 11a ;
[0271] C 6 -C 10 aryl substituted with 0-3 R 11b ;
[0272] C 3 -C 10 carbocycle substituted with 0-3 R 11b ; or
[0273] 5 to 10 membered heterocycle substituted with 0-3 R 11b ;
[0274] alternatively, two R 11 substituents on the same or adjacent carbon atoms may be combined to form a C 3 -C 6 carbocycle or a benzo fused radical wherein said benzo fused radical is substituted with 0-4 R 13 ;
[0275] additionally, two R 11 substituents on adjacent atoms may be combined to form a 5 to 6 membered heteroaryl fused radical, wherein said 5 to 6 membered heteroaryl fused radical comprises 1 or 2 heteroatoms selected from N, O, and S; wherein said 5 to 6 membered heteroaryl fused radical is substituted with 0-3 R 13 ;
[0276] R 11a , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 , CF 3 , or phenyl substituted with 0-3 R 11b ;
[0277] R 11b , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, and C 1 -C 4 haloalkoxy;
[0278] t is 0, 1, 2 or 3;
[0279] R 13 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, C 1 -C 4 alkoxy, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , and CF 3 ;
[0280] R 14 is H, phenyl, benzyl, C 1 -C 6 alkyl, or C 2 -C 6 alkoxyalkyl;
[0281] R 14a is H, phenyl, benzyl, or C 1 -C 4 alkyl;
[0282] R 15 , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl), —S(═O) 2 —(C 1 -C 6 alkyl), and aryl;
[0283] R 16 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl) and —S(═O) 2 —(C 1 -C 6 alkyl);
[0284] alternatively, R 15 and R 16 on the same N atom may be combined to form a 5 to 6 membered heterocyclic fused radical, wherein said 5 to 6 membered heterocyclic is selected from pyrrolidonyl, piperidonyl, piperazinyl, and morpholinyl;
[0285] R 17 is H, aryl, (aryl)CH 2 —, C 1 -C 6 alkyl, or C 2 -C 6 alkoxyalkyl;
[0286] R 18 , at each occurrence, is independently selected from: H, C 1 -C 6 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl) and —S(═O) 2 —(C 1 -C 6 alkyl);
[0287] R 19 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, phenyl, benzyl, phenethyl, —C(═O)—(C 1 -C 6 alkyl) and —S(═O) 2 —(C 1 -C 6 alkyl); and
[0288] alternatively, R 18 and R 19 on the same N atom may be combined to form a 5 to 6 membered heterocyclic fused radical, wherein said 5 to 6 membered heterocyclic is selected from pyrrolidonyl, piperidonyl, piperazinyl, and morpholinyl.
[0289] [4] In a another preferred embodiment the present invention provides a compound of Formula (Ic):
[0290] or a pharmaceutically acceptable salt or prodrug thereof, wherein:
[0291] R 3 is C 1 -C 4 alkyl substituted with 0-2 R 4a ,
[0292] C 2 -C 4 alkenyl substituted with 0-2 R 4a , or
[0293] C 2 -C 4 alkynyl substituted with 0-1 R 4a ;
[0294] R 4a , at each occurrence, is independently selected from: H,
[0295] F, Cl, CF 3 ,
[0296] C 3 -C 6 cycloalkyl substituted with 0-3 R 4b ,
[0297] phenyl substituted with 0-3 R 4b , or
[0298] 5 to 6 membered heterocycle substituted with 0-3 R 4b ;
[0299] R 4b , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 4 alkyl, C 1 -C 3 alkoxy, C 1 -C 2 haloalkyl, and C 1 -C 2 haloalkoxy;
[0300] R 5 is C 1 -C 6 alkyl substituted with 0-3 R 5b ;
[0301] C 2 -C 6 alkenyl substituted with 0-2 R 5b ; or
[0302] C 2 -C 6 alkynyl substituted with 0-2 R 5b ;
[0303] R 5b , at each occurrence, is independently selected from:
[0304] H, methyl, ethyl, propyl, butyl, CF 3 , OR 14 , ═O;
[0305] C 3 -C 6 cycloalkyl substituted with 0-2 R 5c ;
[0306] phenyl substituted with 0-3 R 5c ; or
[0307] 5 to 6 membered heterocycle substituted with 0-2 R 5c ;
[0308] R 5c , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 4 alkyl, C 1 -C 3 alkoxy, C 1 -C 2 haloalkyl, and C 1 -C 2 haloalkoxy;
[0309] L is a bond, —CH 2 —, —CH 2 CH 2 —, —CH 2 CH 2 CH 2 —, —CH 2 CH═CH 2 , —(CH 2 ) p —O—(CH 2 ) q —, or —(CH 2 ) p —NR 10 —(CH 2 ) q —;
[0310] p is 0, 1, 2, or 3;
[0311] q is 0, 1, or 2;
[0312] Z is C 3 -C 10 carbocycle substituted with 0-2 R 12b ;
[0313] C 6 -C 10 aryl substituted with 0-4 R 12b ; and
[0314] 5 to 10 membered heterocycle substituted with 0-5 R 12b , wherein the heterocycle contains 1, 2, 3 or 4 heteroatoms selected from N, O and S;
[0315] R 12b , at each occurrence, is independently selected from: H, OH, Cl, F, NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 4 alkyl, C 1 -C 3 alkoxy, C 1 -C 2 haloalkyl, C 1 -C 2 haloalkoxy, phenyl substituted with 0-3 R 12c ;
[0316] R 12c , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, and C 1 -C 4 haloalkoxy;
[0317] B is a 5 or 6 membered amino-heterocyclic ring, comprising one N atom, 3 to 5 carbon atoms, and optionally, an additional heteroatom —N(R LZ )—;
[0318] wherein the amino-heterocyclic ring is saturated or partially saturated; and
[0319] wherein R LZ is either R 10 or the substituent —L—Z;
[0320] R 10 is H, C(═O)R 17 , C(═O)OR 17 , —(C 1 -C 3 alkyl)—C(═O)OR 17 ;
[0321] C 1 -C 4 alkyl substituted with 0-1 R 10a ;
[0322] phenyl substituted with 0-4 R 10b ;
[0323] C 3 -C 6 carbocycle substituted with 0-3 R 10b ; or
[0324] 5 to 6 membered heterocycle optionally substituted with 0-3 R 10b ;
[0325] R 10a , at each occurrence, is independently selected from: H, C 1 -C 4 alkyl, OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 , CF 3 , or phenyl substituted with 0-4 R 10b ;
[0326] R 10b , at each occurrence, is independently selected from: H, OH, C 1 -C 4 alkyl, C 1 -C 3 alkoxy, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , or CF 3 ;
[0327] R 11 , at each occurrence, is independently selected from:
[0328] C 1 -C 4 alkoxy, Cl, F, OH, NR 18 R 19 , C(═O)R 17 , C(═O)OR 17 , CF 3 ;
[0329] C 1 -C 4 alkyl substituted with 0-1 R 11a ;
[0330] phenyl substituted with 0-3 R 11b ;
[0331] C 3 -C 6 carbocycle substituted with 0-3 R 11b ; or
[0332] 5 to 6 membered heterocycle substituted with 0-3 R 11b ;
[0333] alternatively, two R 11 substituents on adjacent carbon atoms may be combined to form a cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, or a benzo fused radical;
[0334] R 11a , at each occurrence, is independently selected from: H, C 1 -C 4 alkyl, OR 14 , F, ═O, NR 15 R 16 , CF 3 , or phenyl substituted with 0-3 R 11b ;
[0335] R 11b , at each occurrence, is independently selected from: H, OH, Cl, F, NR 15 R 16 , CF 3 , C 1 -C 4 alkyl, C 1 -C 3 alkoxy, C 1 -C 2 haloalkyl, and C 1 -C 2 haloalkoxy;
[0336] t is 0, 1, or 2;
[0337] R 13 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, C 1 -C 4 alkoxy, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , and CF 3 ;
[0338] R 14 is H, phenyl, benzyl, C 1 -C 4 alkyl, or C 2 -C 4 alkoxyalkyl;
[0339] R 15 , at each occurrence, is independently selected from: H, C 1 -C 4 alkyl, benzyl, phenethyl, —C(═O)-(C 1 -C 4 alkyl), —S(═O) 2 —(C 1 -C 4 alkyl), and aryl;
[0340] R 16 , at each occurrence, is independently selected from: H, OH, C 1 -C 4 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 4 alkyl) and —S(═O) 2 —(C 1 -C 4 alkyl);
[0341] alternatively, R 15 and R 16 on the same N atom may be combined to form a 5 to 6 membered heterocyclic fused radical, wherein said 5 to 6 membered heterocyclic is selected from pyrrolidonyl, piperidonyl, piperazinyl, and morpholinyl;
[0342] R 17 is H, phenyl, benzyl, 4-fluorophenyl, 4-chlorophenyl, 4-methylphenyl, 4-trifluorophenyl, (4-fluorophenyl)methyl, (4-chlorophenyl)methyl, (4-methylphenyl)methyl, (4-trifluorophenyl)methyl, methyl, ethyl, propyl, butyl, methoxymethyl, methyoxyethyl, ethoxymethyl, or ethoxyethyl;
[0343] R 18 , at each occurrence, is independently selected from: H, methyl, ethyl, propyl, butyl, phenyl, benzyl, and phenethyl;
[0344] R 19 , at each occurrence, is independently selected from: H, methyl, and ethyl; and
[0345] alternatively, R 18 and R 19 on the same N atom may be combined to form a 5 to 6 membered heterocyclic fused radical, wherein said 5 to 6 membered heterocyclic is selected from pyrrolidonyl, piperidonyl, piperazinyl, and morpholinyl.
[0346] [5] In another embodiment the present invention provides a compound of Formula (Ic):
[0347] or a pharmaceutically acceptable salt or prodrug thereof, wherein:
[0348] R 3 is C 1 -C 4 alkyl, C 2 -C 4 alkenyl, or C 2 -C 4 alkynyl;
[0349] R 5 is C 1 -C 6 alkyl, C 2 -C 6 alkenyl, or C 2 -C 6 alkynyl;
[0350] L is a bond, —CH 2 —, —CH 2 CH 2 —, —CH 2 CH 2 CH 2 —, —CH 2 CH═CH 2 , —(CH 2 ) p —O—(CH 2 ) q —, or —(CH 2 ) p —NR 10 —(CH 2 ) q —;
[0351] p is 0, 1, 2, or 3;
[0352] q is 0, 1, or 2;
[0353] Z is C 3 -C 10 carbocycle substituted with 0-2 R 12b ;
[0354] C 6 -C 10 aryl substituted with 0-4 R 12b ; and
[0355] 5 to 10 membered heterocycle substituted with 0-5 R 12b , wherein the heterocycle contains 1, 2, 3 or 4 heteroatoms selected from N, O and S;
[0356] R 12b , at each occurrence, is independently selected from: H, OH, Cl, F, NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , methyl, ethyl, propyl, butyl, methoxy, ethoxy, propoxy, C 1 -C 2 haloalkyl, C 1 -C 2 haloalkoxy, phenyl substituted with 0-3 R 12c ;
[0357] R 12c , at each occurrence, is independently selected from: H, OH, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , C 1 -C 6 alkyl, C 1 -C 4 alkoxy, C 1 -C 4 haloalkyl, and C 1 -C 4 haloalkoxy;
[0358] B is a 6 membered amino-heterocyclic ring, comprising one N atom, 4 or 5 carbon atoms, and optionally, an additional heteroatom —N(R LZ )—;
[0359] wherein the amino-heterocyclic ring is saturated or partially saturated; and
[0360] wherein R LZ is either R 10 or the substituent —L—Z;
[0361] R 10 is H, C(═O)R 17 , C(═O)OR 17 , —(C 1 -C 3 alkyl)—C(═O)OR 17 ;
[0362] C 1 -C 4 alkyl substituted with 0-1 R 10a ;
[0363] phenyl substituted with 0-4 R 10b ;
[0364] C 3 -C 6 carbocycle substituted with 0-3 R 10b ; or
[0365] 5 to 6 membered heterocycle optionally substituted with 0-3 R 10b ;
[0366] R 10a , at each occurrence, is independently selected from: H, C 1 -C 4 alkyl, OR 14 , Cl, F, Br, I, ═O, CN, NO 2 , NR 15 R 16 , CF 3 , or phenyl substituted with 0-4 R 10b ;
[0367] R 10b , at each occurrence, is independently selected from: H, OH, C 1 -C 4 alkyl, C 1 -C 3 alkoxy, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , or CF 3 ;
[0368] R 11 , at each occurrence, is independently selected from:
[0369] C 1 -C 4 alkoxy, Cl, F, OH, NR 18 R 19 , C(═O)R 17 , C(═O)OR 17 , CF 3 ;
[0370] C 1 -C 4 alkyl substituted with 0-1 R 11a ;
[0371] phenyl substituted with 0-3 R 11b ;
[0372] C 3 -C 6 carbocycle substituted with 0-3 R 11b ; or
[0373] 5 to 6 membered heterocycle substituted with 0-3 R 11b ;
[0374] R 11a , at each occurrence, is independently selected from: H, C 1 -C 4 alkyl, OR 14 , F, ═O, NR 15 R 16 , CF 3 , or phenyl substituted with 0-3 R 11b ;
[0375] R 11b , at each occurrence, is independently selected from: H, OH, Cl, F, NR 15 R 16 , CF 3 , C 1 -C 4 alkyl, C 1 -C 3 alkoxy, C 1 -C 2 haloalkyl, and C 1 -C 2 haloalkoxy;
[0376] t is 0, 1, or 2;
[0377] R 13 , at each occurrence, is independently selected from: H, OH, C 1 -C 6 alkyl, C 1 -C 4 alkoxy, Cl, F, Br, I, CN, NO 2 , NR 15 R 16 , and CF 3 ;
[0378] R 14 is H, phenyl, benzyl, methyl, ethyl, propyl, butyl;
[0379] R 15 , at each occurrence, is independently selected from: H, methyl, ethyl, propyl, butyl, and phenyl substituted with 0-3 substituents selected from OH, OCH 3 , Cl, F, Br, I, CN, NO 2 , NH 2 , N(CH 3 )H, N(CH 3 ) 2 , CF 3 , OCF 3 , C(═O)CH 3 , SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , CH 3 , CH 2 CH 3 , CO 2 H, and CO 2 CH 3 ;
[0380] R 16 , at each occurrence, is independently selected from: H, OH, C 1 -C 4 alkyl, benzyl, phenethyl, —C(═O)—(C 1 -C 4 alkyl) and —S(═O) 2 —(C 1 -C 4 alkyl);
[0381] alternatively, R 15 and R 16 on the same N atom may be combined to form a 5 to 6 membered heterocyclic fused radical, wherein said 5 to 6 membered heterocyclic is selected from pyrrolidonyl, piperidonyl, piperazinyl, and morpholinyl;
[0382] R 17 is H, phenyl, benzyl, 4-fluorophenyl, 4-chlorophenyl, 4-methylphenyl, 4-trifluorophenyl, (4-fluorophenyl)methyl, (4-chlorophenyl)methyl, (4-methylphenyl) methyl, (4-trifluorophenyl) methyl, methyl, ethyl, propyl, butyl, methoxymethyl, methyoxyethyl, ethoxymethyl, or ethoxyethyl;
[0383] R 18 , at each occurrence, is independently selected from: H, methyl, ethyl, propyl, butyl, phenyl, benzyl, and phenethyl;
[0384] R 19 , at each occurrence, is independently selected from: H, methyl, ethyl, and
[0385] alternatively, R 18 and R 19 on the same N atom may be combined to form a 5 to 6 membered heterocyclic fused radical, wherein said 5 to 6 membered heterocyclic is selected from pyrrolidonyl, piperidonyl, piperazinyl, and morpholinyl.
[0386] [6] In another preferred embodiment the present invention provides a compound of Formula (Ib):
[0387] or a pharmaceutically acceptable salt or prodrug thereof, wherein:
[0388] R 3 is —CH 3 , —CH 2 CH 3 , —CH 2 CH 2 CH 3 , —CH 2 CH 2 CH 2 CH 3 , —CH 2 (CH 3 ) 2 , —CH(CH 3 )CH 2 CH 3 , —CH 2 CH(CH 3 ) 2 , —CH 2 C(CH 3 ) 3 , —CF 3 , —CH 2 CF 3 , —CH 2 CH 2 CF 3 , —CH 2 CH 2 CH 2 CF 3 ;
[0389] —CH═CH 2 , —CH 2 CH═CH 2 , —CH 2 C(CH 3 )═CH 2 , —CH 2 CH═C(CH 3 ) 2 , —CH 2 CH 2 CH═CH 2 , —CH 2 CH 2 C(CH 3 )═CH 2 , —CH 2 CH 2 CH═C(CH 3 ) 2 , cis-CH 2 CH═CH(CH 3 ), cis-CH 2 CH 2 CH═CH(CH 3 ), trans-CH 2 CH═CH(CH 3 ), trans-CH 2 CH 2 CH═CH(CH 3 );
[0390] —C≡CH, —CH 2 C≡CH, —CH 2 C≡C(CH 3 ); cyclopropyl-CH 2 —, cyclobutyl-CH 2 —, cyclopentyl-CH 2 —, cyclohexyl-CH 2 —, cyclopropyl-CH 2 CH 2 —, cyclobutyl-CH 2 CH 2 —, cyclopentyl-CH 2 CH 2 —, cyclohexyl-CH 2 CH 2 —;
[0391] phenyl-CH 2 —, (2-F-phenyl)CH 2 —, (3-F-phenyl)CH 2 —, (4-F-phenyl)CH 2 —, (2-Cl-phenyl)CH 2 —, (3-Cl-phenyl)CH 2 —, (4-Cl-phenyl)CH 2 —, (2,3-diF-phenyl)CH 2 —, (2,4-diF-phenyl)CH 2 —, (2,5-diF-phenyl)CH 2 —, (2,6-diF-phenyl)CH 2 —, (3,4-diF-phenyl)CH 2 —, (3,5-diF-phenyl)CH 2 —, (2,3-diCl-phenyl)CH 2 —, (2,4-diCl-phenyl)CH 2 —, (2,5-diCl-phenyl)CH 2 —, (2,6-diCl-phenyl)CH 2 —, (3,4-diCl-phenyl)CH 2 —, (3,5-diCl-phenyl)CH 2 —, (3-F-4-Cl-phenyl)CH 2 —, (3-F-5-Cl-phenyl)CH 2 —, (3-Cl-4-F-phenyl)CH 2 —, phenyl-CH 2 CH 2 —, (2-F-phenyl)CH 2 CH 2 —, (3-F-phenyl)CH 2 CH 2 —, (4-F-phenyl)CH 2 CH 2 —, (2-Cl-phenyl)CH 2 CH 2 —, (3-Cl-phenyl)CH 2 CH 2 —, (4-Cl-phenyl)CH 2 CH 2 —, (2,3-diF-phenyl)CH 2 CH 2 —, (2,4-diF-phenyl)CH 2 CH 2 —, (2,5-diF-phenyl)CH 2 CH 2 —, (2,6-diF-phenyl)CH 2 CH 2 —, (3,4-diF-phenyl)CH 2 CH 2 —, (3,5-diF-phenyl)CH 2 CH 2 —, (2,3-diCl-phenyl)CH 2 CH 2 —, (2,4-diCl-phenyl)CH 2 CH 2 —, (2,5-diCl-phenyl)CH 2 CH 2 —, (2,6-diCl-phenyl)CH 2 CH 2 —, (3,4-diCl-phenyl)CH 2 CH 2 —, (3,5-diCl-phenyl)CH 2 CH 2 —, (3-F-4-Cl-phenyl)CH 2 CH 2 —, or (3-F-5-Cl-phenyl)CH 2 CH 2 —;
[0392] R 5 is —CH 3 , —CH 2 CH 3 , —CH 2 CH 2 CH 3 , —CH 2 (CH 3 ) 2 , —CH 2 CH 2 CH 2 CH 3 , —CH(CH 3 )CH 2 CH 3 , —CH 2 CH(CH 3 ) 2 , —CH 2 C(CH 3 ) 3 , —CH 2 CH 2 CH 2 CH 2 CH 3 , —CH(CH 3 )CH 2 CH 2 CH 3 , —CH 2 CH(CH 3 )CH 2 CH 3 , —CH 2 CH 2 CH(CH 3 ) 2 , —CH(CH 2 CH 3 ) 2 , —CF 3 , —CH 2 CF 3 , —CH 2 CH 2 CF 3 , —CH 2 CH 2 CH 2 CF 3 , —CH 2 CH 2 CH 2 CH 2 CF 3 , —CH═CH 2 , —CH 2 CH═CH 2 , —CH═CHCH 3 , —CH 2 C(CH 3 )═CH 2 , cis-CH 2 CH═CH(CH 3 ), trans-CH 2 CH═CH(CH 3 ), trans-CH 2 CH═CH(C 6 H 5 ), —CH 2 CH═C(CH 3 ) 2 , cis-CH 2 CH═CHCH 2 CH 3 , trans-CH 2 CH═CHCH 2 CH 3 , cis-CH 2 CH 2 CH═CH(CH 3 ), trans-CH 2 CH 2 CH═CH(CH 3 ), trans-CH 2 CH═CHCH 2 (C 6 H 5 ), —C≡CH, —CH 2 C≡CH, —CH 2 C≡C(CH 3 ), —CH 2 C≡C (C 6 H 5 ), —CH 2 CH 2 C≡CH, —CH 2 CH 2 C≡C(CH 3 ), —CH 2 CH 2 C≡C(C 6 H 5 ), —CH 2 CH 2 CH 2 C≡CH, —CH 2 CH 2 CH 2 C≡C(CH 3 ), —CH 2 CH 2 CH 2 C≡C(C 6 H 5 ), cyclopropyl-CH 2 —, cyclobutyl-CH 2 —, cyclopentyl-CH 2 —, cyclohexyl-CH 2 —, (2-CH 3 -cyclopropyl)CH 2 —, (3-CH 3 -cyclobutyl)CH 2 —, cyclopropyl-CH 2 CH 2 —, cyclobutyl-CH 2 CH 2 —, cyclopentyl-CH 2 CH 2 —, cyclohexyl-CH 2 CH 2 —, (2-CH 3 -cyclopropyl)CH 2 CH 2 —, (3-CH 3 -cyclobutyl)CH 2 CH 2 —, phenyl-CH 2 —, (2-F-phenyl)CH 2 —, (3-F-phenyl)CH 2 —, (4-F-phenyl)CH 2 —, furanyl-CH 2 —, thienyl-CH 2 —, pyridyl-CH 2 —, 1-imidazolyl-CH 2 —, oxazolyl-CH 2 —, isoxazolyl-CH 2 —, phenyl-CH 2 CH 2 —, (2-F-phenyl)CH 2 CH 2 —, (3-F-phenyl)CH 2 CH 2 —, (4-F-phenyl)CH 2 CH 2 —, furanyl-CH 2 CH 2 —, thienyl-CH 2 CH 2 —, pyridyl-CH 2 CH 2 —, 1-imidazolyl-CH 2 CH 2 —, oxazolyl-CH 2 CH 2 —, or isoxazolyl-CH 2 CH 2 —;
[0393] L is a bond, —CH 2 —, —CH 2 CH 2 —, —CH 2 CH 2 CH 2 —, —CH 2 CH═CH 2 , O, —CH 2 O—, —(CH 2 ) 2 —O—, —(CH 2 ) 3 —O—, —(CH 2 )—O—(CH 2 ) 2 —, —(CH 2 ) 2 —O—(CH 2 )—, —(CH 2 ) 2 —O—(CH 2 ) 2 —, NH, NMe, —CH 2 NH—, —(CH 2 ) 2 —NH—, —(CH 2 ) 3 —NH—, —(CH 2 )—NH—(CH 2 ) 2 —, —(CH 2 ) 2 —NH—(CH 2 )—, —(CH 2 ) 2 —NH—(CH 2 ) 2 —, and —N(benzoyl)-;
[0394] Z is cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, phenyl 2-F-phenyl, 3-F-phenyl, 4-F-phenyl, 2-Cl-phenyl, 3-Cl-phenyl, 4-Cl-phenyl, 2,3-diF-phenyl, 2,4-diF-phenyl, 2,5-diF-phenyl, 2,6-diF-phenyl, 3,4-diF-phenyl, 3,5-diF-phenyl, 2,3-diCl-phenyl, 2,4-diCl-phenyl, 2,5-diCl-phenyl, 2,6-diCl-phenyl, 3,4-diCl-phenyl, 3,5-diCl-phenyl, 2,3-diMe-phenyl, 2,4-diMe-phenyl, 2,5-diMe-phenyl, 2,6-diMe-phenyl, 3,4-diMe-phenyl, 3,5-diMe-phenyl, 2,3-diMeO-phenyl, 2,4-diMeO-phenyl, 2,5-diMeO-phenyl, 2,6-diMeO-phenyl, 3,4-diMeO-phenyl, 3,5-diMeO-phenyl, 3-F-4-Cl-phenyl, 3-F-5-Cl-phenyl, 3-Cl-4-F-phenyl, 2-MeO-phenyl, 3-MeO-phenyl, 4-MeO-phenyl, 2-EtO-phenyl, 3-EtO-phenyl, 4-EtO-phenyl, 2-Me-phenyl, 3-Me-phenyl, 4-Me-phenyl, 2-Et-phenyl, 3-Et-phenyl, 4-Et-phenyl, 2-CF 3 -phenyl, 3-CF 3 -phenyl, 4-CF 3 -phenyl, 2-NO 2 -phenyl, 3-NO 2 -phenyl, 4-NO 2 -phenyl, 2-CN-phenyl, 3-CN-phenyl, 4-CN-phenyl, 2-MeS-phenyl, 3-MeS-phenyl, 4-MeS-phenyl, 2-CF 3 O-phenyl, 3-CF 3 O-phenyl, 4-CF 3 O-phenyl, 2-Me-5-Cl-phenyl, 3-CF 3 -4-Cl-phenyl, 3-CF 3 -5-F-phenyl, 3-MeO-4-Me-phenyl, furanyl, thienyl, pyrid-2-yl, pyrid-3-yl, pyrid-4-yl, pyrimidyl, pyrazinyl, 2-Me-pyridyl, 3-Me-pyridyl, 3-CF 3 -pyrid-2-yl, 5-CF 3 -pyrid-2-yl, 4-Me-pyridyl, pyrrolidinyl, 1-imidazolyl, oxazolyl, isoxazolyl, 1-benzimidazolyl, 2-keto-1-benzimidazolyl, 4-benzo[1,3]dioxol-5-yl, morpholino, N-piperidyl, 4-piperidyl, naphthyl, 4(phenyl)phenyl-, 4(4-CF 3 -phenyl)phenyl-, 3,5-bis-CF 3 -phenyl-, 4-iPr-phenyl-, N-piperidino-CH 2 —, 1-Me-pyrrolidin-2-yl, and 1-pyrrolidinyl;
[0395] B is a 5 or 6 membered amino-heterocyclic ring, comprising one N atom, 3 to 5 carbon atoms, and optionally, an additional heteroatom —N(R LZ )—;
[0396] wherein the amino-heterocyclic ring is saturated or partially saturated; and
[0397] wherein R LZ is either R 10 or the substituent —L—Z;
[0398] R 10 is H, methyl, ethyl, phenyl, benzyl, phenethyl, 4-F-phenyl, (4-F-phenyl)CH 2 —, (4-F-phenyl)CH 2 CH 2 —, 4-Cl-phenyl, (4-Cl-phenyl)CH 2 —, (4-Cl-phenyl)CH 2 CH 2 —, 4-CH 3 -phenyl, (4-CH 3 -phenyl)CH 2 —, (4-CH 3 -phenyl)CH 2 CH 2 —, 4-CF 3 -phenyl, (4-CF 3 -phenyl)CH 2 —, (4-CF 3 -phenyl)CH 2 CH 2 —, —CH 2 C(═O)Et, —C(═O)Me, or 4-Cl-benzhydryl;
[0399] R 11 , at each occurrence, is independently selected from: H, OH, methyl, ethyl, —CN, —C(═O)Me, —C(═O)OEt, —C(═O)Et, —CH 2 OH, —C(═O)NH 2 , —C(═O)OH, —C(═O)N(Et) 2 , phenyl, benzyl, phenethyl, 4-F-phenyl, (4-F-phenyl)CH 2 —, (4-F-phenyl)CH 2 CH 2 —, 4-Cl-phenyl, (4-Cl-phenyl)CH 2 —, (4-Cl-phenyl)CH 2 CH 2 —, 4-CH 3 -phenyl, (4-CH 3 -phenyl)CH 2 —, (4-CH 3 -phenyl)CH 2 CH 2 —, 4-CF 3 -phenyl, (4-CF 3 -phenyl)CH 2 —, (4-CF 3 -phenyl)CH 2 CH 2 —, and —N(Me) 2 —,; and
[0400] t is 0, 1, or 2;
[0401] alternatively, two R 11 substituents on the same or adjacent carbon atoms may be combined to form a cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, or a benzo fused radical.
[0402] [7] In another preferred embodiment the present invention provides a compound of Formula (Ib):
[0403] or a pharmaceutically acceptable salt or prodrug thereof, wherein:
[0404] R 3 is —CH 2 CH 2 CH 3 , —CH 2 CH 2 CH 2 CH 3 , —CH 2 (CH 3 ) 2 , —CH 2 CH(CH 3 ) 2 , —CH 2 CH═CH 2 , —CH 2 CH 2 CH═CH 2 , —CH 2 CH 2 CH═C(CH 3 ) 2 , cis-CH 2 CH═CH(CH 3 ), cis-CH 2 CH 2 CH═CH(CH 3 ), trans-CH 2 CH═CH(CH 3 ), trans-CH 2 CH 2 CH═CH(CH 3 ); cyclopropyl-CH 2 —, cyclobutyl-CH 2 —, cyclopentyl-CH 2 —, cyclohexyl-CH 2 —, cyclopropyl-CH 2 CH 2 —, cyclobutyl-CH 2 CH 2 —, cyclopentyl-CH 2 CH 2 —, or cyclohexyl-CH 2 CH 2 —;
[0405] R 5 is —CH 2 (CH 3 ) 2 , —CH 2 CH 2 CH 2 CH 3 , —CH(CH 3 )CH 2 CH 3 , —CH 2 CH(CH 3 ) 2 , —CH 2 C (CH 3 ) 3 , —CH 2 CH 2 CH 2 CH 2 CH 3 , —CH(CH 3 )CH 2 CH 2 CH 3 , —CH 2 CH(CH 3 )CH 2 CH 3 , —CH 2 CH 2 CH(CH 3 ) 2 , —CH (CH 2 CH 3 ) 2 , —CH 2 CH═CH 2 , —CH 2 C(CH 3 )═CH 2 , cis-CH 2 CH═CH(CH 3 ), trans-CH 2 CH═CH(CH 3 ), —CH 2 CH═C(CH 3 ) 2 , cyclopropyl-CH 2 —, cyclobutyl-CH 2 —, cyclopentyl-CH 2 —, cyclohexyl-CH 2 —, (2-CH 3 -cyclopropyl)CH 2 —, or (3-CH 3 -cyclobutyl)CH 2 —,
[0406] L is a bond, —CH 2 —, —CH 2 CH 2 —, —CH 2 CH 2 CH 2 —, —CH 2 CH═CH 2 , O, —CH 2 O—, —(CH 2 ) 2 —O—, —(CH 2 ) 3 —O—, —(CH 2 )—O—(CH 2 ) 2 —, —(CH 2 ) 2 —O—(CH 2 )—, —(CH 2 ) 2 —O—(CH 2 ) 2 —, NH, NMe, —CH 2 NH—, —(CH 2 ) 2 —NH—, —(CH 2 ) 3 —NH—, —(CH 2 )—NH—(CH 2 ) 2 —, —(CH 2 ) 2 —NH—(CH 2 )—, —(CH 2 ) 2 —NH—(CH 2 ) 2 —, and —N(benzoyl)-;
[0407] Z is cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, phenyl 2-F-phenyl, 3-F-phenyl, 4-F-phenyl, 2-Cl-phenyl, 3-Cl-phenyl, 4-Cl-phenyl, 2,3-diF-phenyl, 2,4-diF-phenyl, 2,5-diF-phenyl, 2,6-diF-phenyl, 3,4-diF-phenyl, 3,5-diF-phenyl, 2,3-diCl-phenyl, 2,4-diCl-phenyl, 2,5-diCl-phenyl, 2, 6-diCl-phenyl, 3,4-diCl-phenyl, 3,5-diCl-phenyl, 2,3-diMe-phenyl, 2,4-diMe-phenyl, 2,5-diMe-phenyl, 2,6-dime-phenyl, 3,4-diMe-phenyl, 3,5-diMe-phenyl, 2,3-diMeO-phenyl, 2,4-diMeO-phenyl, 2,5-diMeO-phenyl, 2,6-diMeO-phenyl, 3,4-diMeO-phenyl, 3,5-diMeO-phenyl, 3-F-4-Cl-phenyl, 3-F-5-Cl-phenyl, 3-Cl-4-F-phenyl, 2-MeO-phenyl, 3-MeO-phenyl, 4-MeO-phenyl, 2-EtO-phenyl, 3-EtO-phenyl, 4-EtO-phenyl, 2-Me-phenyl, 3-Me-phenyl, 4-Me-phenyl, 2-Et-phenyl, 3-Et-phenyl, 4-Et-phenyl, 2-CF 3 -phenyl, 3-CF 3 -phenyl, 4-CF 3 -phenyl, 2-NO 2 -phenyl, 3-NO 2 -phenyl, 4-NO 2 -phenyl, 2-CN-phenyl, 3-CN-phenyl, 4-CN-phenyl, 2-MeS-phenyl, 3-MeS-phenyl, 4-MeS-phenyl, 2-CF 3 O-phenyl, 3-CF 3 O-phenyl, 4-CF 3 O-phenyl, 2-Me-5-Cl-phenyl, 3-CF 3 -4-Cl-phenyl, 3-CF 3 -5-F-phenyl, 3-MeO-4-Me-phenyl, furanyl, thienyl, pyrid-2-yl, pyrid-3-yl, pyrid-4-yl, pyrimidyl, pyrazinyl, 2-Me-pyridyl, 3-Me-pyridyl, 3-CF 3 -pyrid-2-yl, 5-CF 3 -pyrid-2-yl, 4-Me-pyridyl, pyrrolidinyl, 1-imidazolyl, oxazolyl, isoxazolyl, 1-benzimidazolyl, 2-keto-1-benzimidazolyl, 4-benzo[1,3]dioxol-5-yl, morpholino, N-piperidyl, 4-piperidyl, naphthyl, 4(phenyl)phenyl-, 4(4-CF 3 -phenyl)phenyl-, 3,5-bis-CF 3 -phenyl-, 4-iPr-phenyl-, N-piperidino-CH 2 —, 1-Me-pyrrolidin-2-yl, and 1-pyrrolidinyl;
[0408] B is a 5 or 6 membered amino-heterocyclic ring, comprising one N atom, 3 to 5 carbon atoms, and optionally, an additional heteroatom —N(R LZ )—;
[0409] wherein the amino-heterocyclic ring is saturated or partially saturated; and
[0410] wherein R LZ is the substituent —L—Z;
[0411] R 11 , at each occurrence, is independently selected from: H, OH, methyl, ethyl, —CN, —C(═O)Me, —C(═O)OEt, —C(═O)Et, —CH 2 OH, —C(═O)NH 2 , —C(═O)OH, —C(═O)N(Et) 2 , and —N(Me) 2 —;
[0412] t is 0 or 1.
[0413] In another preferred embodiment the present invention provides a compound of the present invention wherein B is
[0414] In another preferred embodiment the present invention provides a compound of the present invention wherein B is
[0415] In another preferred embodiment the present invention provides a compound selected from one of the Examples in Table 5a, Table 5b, Table 5c, Table 5d, Table 5e, Table 5f or Table 5g.
[0416] In another even further more preferred embodiment the present invention provides for a compound selected from:
[0417] 5-Methyl-2-propyl-3-[4-(3-trifluoromethyl-phenyl)-piperazine-1-carbonyl]-hexanoic acid amide;
[0418] 3-[4-(5-Chloro-2-methyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2-propyl-hexanoic acid amide;
[0419] 3-[3-Hydroxy-4-(3-trifluoromethyl-phenyl)-piperidine-1-carbonyl]-5-methyl-2-propyl-hexanoic acid amide;
[0420] 3-[4-(3,4-Dichloro-phenyl)-piperazine-1-carbonyl]-5-methyl-2-propyl-hexanoic acid amide;
[0421] 3-[4-(4-Chloro-3-trifluoromethyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2-propyl-hexanoic acid amide;
[0422] 3-[4-(4-Chloro-3-trifluoromethyl-phenyl)-4-hydroxy-piperidine-1-carbonyl]-5-methyl-2-propyl-hexanoic acid amide;
[0423] 5-Methyl-3-(4-phenyl-piperidine-1-carbonyl)-2-propyl-hexanoic acid amide;
[0424] 3-(3-Benzyl-pyrrolidine-1-carbonyl)-5-methyl-2-propyl-hexanoic acid amide;
[0425] 5-Methyl-3-(4-phenyl-piperidine-1-carbonyl)-2-propyl-hexanoic acid amide; and
[0426] 3-(3-Benzyl-pyrrolidine-1-carbonyl)-5-methyl-2-propyl-hexanoic acid amide.
[0427] In another preferred embodiment
[0428] R 3 is R 4 ,
[0429] R 3a is H, methyl, ethyl, propyl, or butyl;
[0430] R 4 is C 1 -C 6 alkyl, C 2 -C 6 alkenyl, C 2 -C 6 alkynyl
[0431] R 5 is C 1 -C 6 alkyl, C 2 -C 6 alkenyl, C 2 -C 6 alkynyl
[0432] R 5a is H, methyl, ethyl, propyl, or butyl; and
[0433] the total number of carbon atoms in R 3 , R 3a , R 5 and R 5a equals seven or more.
[0434] In another preferred embodiment
[0435] R 3 is C 3 -C 4 alkyl or C 3 -C 4 alkenyl,
[0436] R 3a is H;
[0437] R 5 is C 3 -C 5 alkyl or C 3 -C 5 alkenyl, and
[0438] R 5a is H.
[0439] In another preferred embodiment
[0440] R 3 is R 4 ;
[0441] R 3a is H;
[0442] R 4 is C 1 -C 4 alkyl substituted with 1-2 R 4a ,
[0443] R 4a , at each occurrence, is independently selected from C 3 -C 6 cycloalkyl substituted with 0-3 R 4b , phenyl substituted with 0-3 R 4b , or 5 to 6 membered heterocycle substituted with 0-3 R 4b ;
[0444] R 4b , at each occurrence, is independently selected from H, OH, Cl, F, NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , methyl, ethyl, propyl, butyl, methoxy, ethoxy, propoxy, C 1 -C 2 haloalkyl, and C 1 -C 2 haloalkoxy;
[0445] R 5 is C 2 -C 4 alkyl substituted with 0-3 R 5b ;
[0446] C 2 -C 4 alkenyl substituted with 0-2 R 5b ; or
[0447] C 2 -C 4 alkynyl substituted with 0-2 R 5b ;
[0448] R 5b , at each occurrence, is independently selected from:
[0449] H, methyl, ethyl, propyl, butyl, CF 3 , OR 14 , ═O;
[0450] C 3 -C 6 cycloalkyl substituted with 0-2 R 5c ;
[0451] phenyl substituted with 0-3 R 5c ; or
[0452] 5 to 6 membered heterocycle substituted with 0-2 R 5c ; and
[0453] R 5c , at each occurrence, is independently selected from H, OH, Cl, F, NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , methyl, ethyl, propyl, butyl, methoxy, ethoxy, propoxy, C 1 -C 2 haloalkyl, and C 1 -C 2 haloalkoxy.
[0454] In another preferred embodiment
[0455] R 3 is R 4 ;
[0456] R 3a is H;
[0457] R 4 is C 2 -C 4 alkyl substituted with 0-2 R 4a ,
[0458] C 2 -C 4 alkenyl substituted with 0-2 R 4a ,
[0459] C 2 -C 4 alkynyl substituted with 0-2 R 4a ,
[0460] R 4a , at each occurrence, is independently selected from is H, F, CF 3 ,
[0461] C 3 -C 6 cycloalkyl substituted with 0-3 R 4b ,
[0462] phenyl substituted with 0-3 R 4b , or
[0463] 5 to 6 membered heterocycle substituted with 0-3 R 4b ;
[0464] R 4b , at each occurrence, is independently selected from H, OH, Cl, F, NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , methyl, ethyl, propyl, butyl, methoxy, ethoxy, propoxy, C 1 -C 2 haloalkyl, and C 1 -C 2 haloalkoxy;
[0465] R 5 is C 1 -C 4 alkyl substituted with 1-2 R 5b ;
[0466] R 5b , at each occurrence, is independently selected from:
[0467] C 3 -C 6 cycloalkyl substituted with 0-2 R 5c ;
[0468] phenyl substituted with 0-3 R 5c ; or
[0469] 5 to 6 membered heterocycle substituted with 0-2 R 5c ; and
[0470] R 5c , at each occurrence, is independently selected from H, OH, Cl, F, NR 15 R 16 , CF 3 , acetyl, SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , methyl, ethyl, propyl, butyl, methoxy, ethoxy, propoxy, C 1 -C 2 haloalkyl, and C 1 -C 2 haloalkoxy.
[0471] Also included in the present invention in a preferred embodiment are compounds as set forth above wherein the total number of carbon atoms in R 3 , R 3a , R 5 , and R 5a , equals four or more.
[0472] Also included in the present invention in a preferred embodiment are compounds as set forth above wherein the total number of carbon atoms in R 3 , R 3a , R 5 , and R 5a , equals seven or more.
[0473] Also included in the present invention in a preferred embodiment are compounds as set forth above wherein R 3a and R 5a are hydrogen, and R 3 and R 5 are not hydrogen.
[0474] It is understood that any and all embodiments of the present invention may be taken in conjunction with any other embodiment to descibe additional even more preferred embodiments of the present invention.
[0475] In a second embodiment, the present invention provides a pharmaceutical composition comprising a compound of Formula (I) and a pharmaceutically acceptable carrier.
[0476] In a third embodiment, the present invention provides a method for the treatment of neurological disorders associated with β-amyloid production comprising administering to a host in need of such treatment a therapeutically effective amount of a compound of Formula (I).
[0477] In a preferred embodiment the neurological disorder associated with β-amyloid production is Alzheimer's Disease.
[0478] In a fourth embodiment, the present invention provides a method for inhibiting γ-secretase activity for the treatment of a physiological disorder associated with inhibiting γ-secretase activity comprising administering to a host in need of such inhibition a therapeutically effective amount of a compound of Formula (I) that inhibits γ-secretase activity.
[0479] In a preferred embodiment the physiological disorder associated with inhibiting γ-secretase activity is Alzheimer's Disease.
[0480] In a fifth embodiment, the present invention provides a compound of Formula (I) for use in therapy.
[0481] In a preferred embodiment the present invention provides a compound of Formula (I) for use in therapy of Alzheimer's Disease.
[0482] In a sixth embodiment, the present invention provides for the use of a compound of Formula (I) for the manufacture of a medicament for the treatment of Alzheimer's Disease.
Definitions
[0483] As used herein, the term “Aβ” denotes the protein designated Aβ, β-amyloid peptide, and sometimes β/A4, in the art. Aβ is an approximately 4.2 kilodalton (kD) protein of about 39 to 43 amino acids found in amyloid plaques, the walls of meningeal and parenchymal arterioles, small arteries, capillaries, and sometimes, venules. The isolation and sequence data for the first 28 amino acids are described in U.S. Pat. No. 4,666,829. The 43 amino acid sequence is:
1 Asp Ala Glu Phe Arg His Asp Ser Gly Tyr 11 Glu Val His His Gln Lys Leu Val Phe Phe 21 Ala Glu Asp Val Gly Ser Asn Lys Gly Ala 31 Ile Ile Gly Leu Met Val Gly Gly Val Val 41 Ile Ala Thr.
[0484] However, a skilled artisan knows that fragments generated by enzymatic degradation can result in loss of amino acids 1-10 and/or amino acids 39-43. Thus, an amino acid sequence 1-43 represents the maximum sequence of amino acids for Aβ peptide.
[0485] The term “APP”, as used herein, refers to the protein known in the art as β amyloid precursor protein. This protein is the precursor for Aβ and through the activity of “secretase” enzymes, as used herein, it is processed into Aβ. Differing secretase enzymes, known in the art, have been designated β secretase, generating the N-terminus of Aβ, a secretase cleaving around the 16/17 peptide bond in Aβ, and “γ secretases”, as used herein, generating C-terminal Aβ fragments ending at position 38, 39, 40, 41, 42, and 43 or generating C-terminal extended precursors which are subsequently truncated to the above polypeptides.
[0486] The compounds herein described may have asymmetric centers. Compounds of the present invention containing an asymmetrically substituted atom may be isolated in optically active or racemic forms. It is well known in the art how to prepare optically active forms, such as by resolution of racemic forms or by synthesis from optically active starting materials. Many geometric isomers of olefins, C═N double bonds, and the like can also be present in the compounds described herein, and all such stable isomers are contemplated in the present invention. Cis and trans geometric isomers of the compounds of the present invention are described and may be isolated as a mixture of isomers or as separated isomeric forms. All chiral, diastereomeric, racemic forms and all geometric isomeric forms of a structure are intended, unless the specific stereochemistry or isomeric form is specifically indicated.
[0487] The term “substituted,” as used herein, means that any one or more hydrogens on the designated atom is replaced with a selection from the indicated group, provided that the designated atom's normal valency is not exceeded, and that the substitution results in a stable compound. When a substituent is keto (i.e., ═O), then 2 hydrogens on the atom are replaced.
[0488] When any variable (e.g. , R 4b , R 5b , R 11b , R 12b , etc.) occurs more than one time in any constituent or formula for a compound, its definition at each occurrence is independent of its definition at every other occurrence. Thus, for example, if a group is shown to be substituted with 0-2 R 5b , then said group may optionally be substituted with up to two R 5b groups and R 5b at each occurrence is selected independently from the definition of R 5b . Also, combinations of substituents and/or variables are permissible only if such combinations result in stable compounds.
[0489] When a bond to a substituent is shown to cross a bond connecting two atoms in a ring, then such substituent may be bonded to any atom on the ring. When a substituent is listed without indicating the atom via which such substituent is bonded to the rest of the compound of a given formula, then such substituent may be bonded via any atom in such substituent. Combinations of substituents and/or variables are permissible only if such combinations result in stable compounds.
[0490] As used herein, “alkyl” or “alkylene” is intended to include both branched and straight-chain saturated aliphatic hydrocarbon groups having the specified number of carbon atoms; for example, “C 1 -C 6 alkyl” denotes alkyl having 1, 2, 3, 4, 5 and 6 carbon atoms. Examples of alkyl include, but are not limited to, methyl, ethyl, n-propyl, i-propyl, n-butyl, i-butyl, sec-butyl, t-butyl, pentyl, and hexyl. Preferred “alkyl” group, unless otherwise specified, is “C 1 -C 4 alkyl”, more preferred is methyl, ethyl, propyl, and butyl.
[0491] As used herein, “alkenyl” or “alkenylene” is intended to include hydrocarbon chains of either a straight or branched configuration and one or more unsaturated carbon-carbon bonds which may occur in any stable point along the chain. Examples of “C 2 -C 6 alkenyl” include, but are not limited to, ethenyl, 1-propenyl, 2-propenyl, 1-butenyl, 2-butenyl, 3-butenyl, 3-methyl-2-butenyl, 2-pentenyl, 3-pentenyl, hexenyl, and the like.
[0492] As used herein, “alkynyl” or “alkynylene” is intended to include hydrocarbon chains of either a straight or branched configuration and one or more carbon-carbon triple bonds which may occur in any stable point along the chain. Examples of “C 2 -C 6 alkynyl” include, but are not limited to, ethynyl, 1-propynyl, 2-propynyl, 1-butynyl, 2-butynyl, 3-butynyl, and the like.
[0493] “Alkoxy” or “alkyloxy” represents an alkyl group as defined above with the indicated number of carbon atoms attached through an oxygen bridge. Examples of alkoxy include, but are not limited to, methoxy, ethoxy, n-propoxy, i-propoxy, n-butoxy, s-butoxy, t-butoxy, n-pentoxy, and s-pentoxy. Preferred alkoxy groups are methoxy, ethoxy, n-propoxy, i-propoxy, n-butoxy, s-butoxy, t-butoxy. Similarly, “alkylthio” or “thioalkoxy” represents an alkyl group as defined above with the indicated number of carbon atoms attached through a sulphur bridge.
[0494] “Halo” or “halogen” as used herein refers to fluoro, chloro, bromo, and iodo. Unless otherwise specified, preferred halo is fluoro and chloro. “Counterion” is used to represent a small, negatively charged species such as chloride, bromide, hydroxide, acetate, sulfate, and the like.
[0495] “Haloalkyl” is intended to include both branched and straight-chain saturated aliphatic hydrocarbon groups having the specified number of carbon atoms, substituted with 1 or more halogen (for example —C v F w where v=1 to 3 and w=1 to (2v+1)). Examples of haloalkyl include, but are not limited to, trifluoromethyl, trichloromethyl, pentafluoroethyl, pentachloroethyl, 2,2,2-trifluoroethyl, 2,2-difluoroethyl, heptafluoropropyl, and heptachloropropyl. “Haloalkoxy” is intended to mean a haloalkyl group as defined above with the indicated number of carbon atoms attached through an oxygen bridge; for example trifluoromethoxy, pentafluoroethoxy, 2,2,2-trifluoroethoxy, and the like. “Halothioalkoxy” is intended to mean a haloalkyl group as defined above with the indicated number of carbon atoms attached through a sulphur bridge.
[0496] “Cycloalkyl” is intended to include saturated ring groups, having the specified number of carbon atoms. For example, “C 3 -C 6 cycloalkyl” denotes such as cyclopropyl, cyclobutyl, cyclopentyl, or cyclohexyl.
[0497] As used herein, “carbocycle” is intended to mean any stable 3, 4, 5, 6 and 7-membered monocyclic or bicyclic or 7, 8, 9, 10, 11, 12 and 13-membered bicyclic or tricyclic, any of which may be saturated, partially unsaturated, or aromatic. Examples of such carbocycles include, but are not limited to, cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl, adamantyl, cyclooctyl, [3.3.0]bicyclooctane, [4.3.0]bicyclononane, [4.4.0]bicyclodecane (decalin), [2.2.2]bicyclooctane, fluorenyl, phenyl, naphthyl, indanyl, adamantyl, or tetrahydronaphthyl (tetralin). Preferred “carbocycle” are cyclopropyl, cyclobutyl, cyclopentyl, and cyclohexyl.
[0498] As used herein, the term “heterocycle” or “heterocyclic ring” is intended to mean a stable 5, 6, and 7-membered monocyclic or bicyclic or 7, 8, 9, 10, 11, 12, 13 and 14-membered bicyclic heterocyclic ring which is saturated partially unsaturated or unsaturated (aromatic), and which consists of carbon atoms and 1, 2, 3 or 4 heteroatoms, preferably 1, 2, or 3 heteroatoms, independently selected from the group consisting of N, O and S and including any bicyclic group in which any of the above-defined heterocyclic rings is fused to a benzene ring. The nitrogen and sulfur heteroatoms may optionally be oxidized. The heterocyclic ring may be attached to its pendant group at any heteroatom or carbon atom which results in a stable structure. The heterocyclic rings described herein may be substituted on carbon or on a nitrogen atom if the resulting compound is stable. If specifically noted, a nitrogen in the heterocycle may optionally be quaternized. It is preferred that when the total number of S and O atoms in the heterocycle exceeds 1, then these heteroatoms are not adjacent to one another. It is preferred that the total number of S and O atoms in the heterocycle is not more than 1.
[0499] Examples of heterocycles include, but are not limited to, 1H-indazole, 2-pyrrolidonyl, 2H,6H-1,5,2-dithiazinyl, 2H-pyrrolyl, 3H-indolyl, 4-piperidonyl, 4aH-carbazole, 4H-quinolizinyl, 6H-1,2,5-thiadiazinyl, acridinyl, azocinyl, benzimidazolyl, benzofuranyl, benzothiofuranyl, benzothiophenyl, benzoxazolyl, benzthiazolyl, benztriazolyl, benztetrazolyl, benzisoxazolyl, benzisothiazolyl, benzimidazalonyl, carbazolyl, 4aH-carbazolyl, b-carbolinyl, chromanyl, chromenyl, cinnolinyl, decahydroquinolinyl, 2H,6H-1,5,2-dithiazinyl, dihydrofuro[2,3-b]tetrahydrofuran, furanyl, furazanyl, imidazolidinyl, imidazolinyl, imidazolyl, 1 H-indazolyl, indolenyl, indolinyl, indolizinyl, indolyl, isobenzofuranyl, isochromanyl, isoindazolyl, isoindolinyl, isoindolyl, isoquinolinyl, isothiazolyl, isoxazolyl, morpholinyl, naphthyridinyl, octahydroisoquinolinyl, oxadiazolyl, 1,2,3-oxadiazolyl, 1,2,4-oxadiazolyl, 1,2,5-oxadiazolyl, 1,3,4-oxadiazolyl, oxazolidinyl, oxazolyl, oxazolidinylperimidinyl, phenanthridinyl, phenanthrolinyl, phenarsazinyl, phenazinyl, phenothiazinyl, phenoxathiinyl, phenoxazinyl, phthalazinyl, piperazinyl, piperidinyl, pteridinyl, piperidonyl, 4-piperidonyl, pteridinyl, purinyl, pyranyl, pyrazinyl, pyrazolidinyl, pyrazolinyl, pyrazolyl, pyridazinyl, pyridooxazole, pyridoimidazole, pyridothiazole, pyridinyl, pyridyl, pyrimidinyl, pyrrolidinyl, pyrrolinyl, pyrrolyl, quinazolinyl, quinolinyl, 4H-quinolizinyl, quinoxalinyl, quinuclidinyl, carbolinyl, tetrahydrofuranyl, tetrahydroisoquinolinyl, tetrahydroquinolinyl, 6H-1,2,5-thiadiazinyl, 1,2,3-thiadiazolyl, 1,2,4-thiadiazolyl, 1,2,5-thiadiazolyl, 1,3,4-thiadiazolyl, thianthrenyl, thiazolyl, thienyl, thienothiazolyl, thienooxazolyl, thienoimidazolyl, thiophenyl, triazinyl, 1,2,3-triazolyl, 1,2,4-triazolyl, 1,2,5-triazolyl, 1,3,4-triazolyl, xanthenyl. Preferred 5 to 10 membered heterocycles include, but are not limited to, pyridinyl, pyrimidinyl, triazinyl, furanyl, thienyl, thiazolyl, pyrrolyl, pyrazolyl, imidazolyl, oxazolyl, isoxazolyl, tetrazolyl, benzofuranyl, benzothiofuranyl, indolyl, benzimidazolyl, 1 H-indazolyl, oxazolidinyl, isoxazolidinyl, benzotriazolyl, benzisoxazolyl, oxindolyl, benzoxazolinyl, quinolinyl, and isoquinolinyl. Preferred 5 to 6 membered heterocycles include, but are not limited to, pyridinyl, pyrimidinyl, triazinyl, furanyl, thienyl, thiazolyl, pyrrolyl, piperazinyl, piperidinyl, pyrazolyl, imidazolyl, oxazolyl, isoxazolyl, tetrazolyl; more preferred 5 to 6 membered heterocycles include, but are not limited to, pyridinyl, pyrimidinyl, triazinyl, furanyl, thienyl, thiazolyl, piperazinyl, piperidinyl, pyrazolyl, imidazolyl, and tetrazolyl. Also included are fused ring and spiro compounds containing, for example, the above heterocycles.
[0500] As used herein, the term “aryl”, “C 6 -C 10 aryl” or aromatic residue, is intended to mean an aromatic moiety containing the specified number of carbon atoms; for example phenyl, pyridinyl or naphthyl; preferably phenyl or naphthyl. Unless otherwise specified, “aryl” may be unsubstituted or substituted with 0 to 3 groups selected from H, OH, OCH 3 , Cl, F, Br, I, CN, NO 2 , NH 2 , N(CH 3 )H, N(CH 3 ) 2 , CF 3 , OCF 3 , C(═O)CH 3 , SCH 3 , S(═O)CH 3 , S(═O) 2 CH 3 , CH 3 , CH 2 CH 3 , CO 2 H, and COCH 3 .
[0501] The phrase “amino-heterocyclic ring”, as used herein, is intended to denote a heterocyclic ring of Formula (I″)
[0502] comprising at least one nitrogen atom, carbon atoms and optionally a second additional heteroatom selected from oxygen, nitrogen and sulfur; wherein the total number of members of “amino-heterocycle ring” B does not exceed 8. When “amino-heterocycle ring” B comprises one nitrogen atom, then amino-heterocyclic ring B also contains 3, 4, 5, 6 or 7 carbons. Alternatively, when “amino-heterocycle ring” B comprises one nitrogen atom and a second additional heteroatom, then amino-heterocyclic ring B contains 3, 4, 5, or 6 carbons. It is preferred that the total number of atoms of amino-heterocyclic ring B is 5, 6, or 7; it is more preferred that the total number of atoms of amino-heterocyclic ring B is five or six.
[0503] It is further understood that amino-heterocyclic ring B may be saturated or partially unsaturated (i.e. two adjacent atoms in the ring form a double bond) wherein the backbone of amino-heterocyclic ring B may contain one, two or three double bonds, but not fully unsaturated. Examples of amino-heterocyclic ring B include, but are not limited to piperidine, piperazine, and pyrrolidine.
[0504] It is further understood that amino-heterocyclic ring B may contain a second additional heteroatom selected from oxygen, nitrogen and sulfur; for example —O—, —S—, —S(═O)—, —S(═O) 2 —, —N═, and —N(R LZ )—. When the second additional heteroatom is selected from oxygen and sulfur; then substituent —L—Z of Formula (I) is attached to amino-heterocyclic ring B through a ring carbon. When the second additional heteroatom is selected from nitrogen, then substituent —L—Z of Formula (I) is attached to amino-heterocyclic ring B through the second nitrogen or through a ring carbon. When substituent —L—Z of Formula (I) is attached to amino-heterocyclic ring B through the second nitrogen the second nitrogen is designated as —N(R LZ )—. Alternatively, when substituent —L—Z of Formula (I) is attached to amino-heterocyclic ring B through a ring carbon then the second nitrogen is designated as —N(R 10 )— or —N═.
[0505] It is further understood that amino-heterocyclic ring B may be substituted with 0, 1, 2, or 3 R 11 groups. Such R 11 groups are substituted on amino-heterocyclic ring B through the ring carbon atoms. It is understood when amino-heterocyclic ring B is substituted with 2 or 3 R 11 groups then two such R 11 groups may be substituted in the same or adjacent carbon.
[0506] The compounds herein described may have asymmetric centers. One enantiomer of a compound of Formula (I) may display superior chemical activity over the opposite enantiomer. When required, separation of the racemic material can be achieved by methods known in the art. For example, the carbon atoms to which R 3 and R 5 are attached may describe chiral carbons which may display superior chemical activity over the opposite enantiomer. For example, where R 3 and R 5 are not H, then the configuration of the two centers may be described as (2R,3R), (2R,3S), (2S,3R), or (2S,3S). All configurations are considered part of the invention; however, the (2R,3S) and the (2S,3R) are preferred and the (2R,3S) is more preferred.
[0507] The phrase “pharmaceutically acceptable” is employed herein to refer to those compounds, materials, compositions, and/or dosage forms which are, within the scope of sound medical judgment, suitable for use in contact with the tissues of human beings and animals without excessive toxicity, irritation, allergic response, or other problem or complication, commensurate with a reasonable benefit/risk ratio.
[0508] As used herein, “pharmaceutically acceptable salts” refer to derivatives of the disclosed compounds wherein the parent compound is modified by making acid or base salts thereof. Examples of pharmaceutically acceptable salts include, but are not limited to, mineral or organic acid salts of basic residues such as amines; alkali or organic salts of acidic residues such as carboxylic acids; and the like. The pharmaceutically acceptable salts include the conventional non-toxic salts or the quaternary ammonium salts of the parent compound formed, for example, from non-toxic inorganic or organic acids. For example, such conventional non-toxic salts include those derived from inorganic acids such as hydrochloric, hydrobromic, sulfuric, sulfamic, phosphoric, nitric and the like; and the salts prepared from organic acids such as acetic, propionic, succinic, glycolic, stearic, lactic, malic, tartaric, citric, ascorbic, pamoic, maleic, hydroxymaleic, phenylacetic, glutamic, benzoic, salicylic, sulfanilic, 2-acetoxybenzoic, fumaric, toluenesulfonic, methanesulfonic, ethane disulfonic, oxalic, isethionic, and the like.
[0509] The pharmaceutically acceptable salts of the present invention can be synthesized from the parent compound which contains a basic or acidic moiety by conventional chemical methods. Generally, such salts can be prepared by reacting the free acid or base forms of these compounds with a stoichiometric amount of the appropriate base or acid in water or in an organic solvent, or in a mixture of the two; generally, nonaqueous media like ether, ethyl acetate, ethanol, isopropanol, or acetonitrile are preferred. Lists of suitable salts are found in Remington's Pharmaceutical Sciences, 17th ed., Mack Publishing Company, Easton, Pa., 1985, p. 1418, the disclosure of which is hereby incorporated by reference.
[0510] “Prodrugs” are intended to include any covalently bonded carriers which release the active parent drug according to Formula (I) in vivo when such prodrug is administered to a mammalian subject. Prodrugs of a compound of Formula (I) are prepared by modifying functional groups present in the compound in such a way that the modifications are cleaved, either in routine manipulation or in vivo, to the parent compound. Prodrugs include compounds of Formula (I) wherein a hydroxy, amino, or sulfhydryl group is bonded to any group that, when the prodrug or compound of Formula (I) is administered to a mammalian subject, cleaves to form a free hydroxyl, free amino, or free sulfhydryl group, respectively. Examples of prodrugs include, but are not limited to, acetate, formate and benzoate derivatives of alcohol and amine functional groups in the compounds of Formula (I), and the like.
[0511] “Stable compound” and “stable structure” are meant to indicate a compound that is sufficiently robust to survive isolation to a useful degree of purity from a reaction mixture, and formulation into an efficacious therapeutic agent.
[0512] As used herein the term “effective amount” means an amount of a compound/composition according to the present invention effective in producing the desired therapeutic effect.
[0513] As used herein the term treating or “treatment” refers to: (i) preventing a disease, disorder or condition from occurring in an animal which may be predisposed to the disease, disorder and/or condition but has not yet been diagnosed as having it; (ii) inhibiting the disease, disorder or condition, i.e., arresting its development; and (iii) relieving the disease, disorder or condition, i.e., causing regression of the disease, disorder and/or condition.
[0514] As used herein the term “patient” or “host” includes both human and other mammals.
Synthesis
[0515] The compounds of the present invention can be prepared in a number of ways well known to one skilled in the art of organic synthesis. The compounds of the present invention can be synthesized using the methods described below, together with synthetic methods known in the art of synthetic organic chemistry, or variations thereon as appreciated by those skilled in the art. Preferred methods include, but are not limited to, those described below. All references cited herein are hereby incorporated in their entirety herein by reference.
[0516] The novel compounds of this invention may be prepared using the reactions and techniques described in this section. The reactions are performed in solvents appropriate to the reagents and materials employed and are suitable for the transformations being effected. Also, in the description of the synthetic methods described below, it is to be understood that all proposed reaction conditions, including choice of solvent, reaction atmosphere, reaction temperature, duration of the experiment and workup procedures, are chosen to be the conditions standard for that reaction, which should be readily recognized by one skilled in the art. It is understood by one skilled in the art of organic synthesis that the functionality present on various portions of the molecule must be compatible with the reagents and reactions proposed. Such restrictions to the substituents which are compatible with the reaction conditions will be readily apparent to one skilled in the art and alternate methods must then be used.
[0517] Patent publication WO 00/07995 and U.S. patent application Ser. No. 09/505,788 both describe synthesis of succinate derivatives. The synthetic disclosure of each of these applications is hereby incorporated by reference.
[0518] Disubstituted succinate derivatives can be prepared by a number of known procedures. The procedure of Evans (D. A. Evans et al, Org. Synth. 86, p83 (1990)) is outlined in Scheme 1 where acylation of an oxazolidinone with an acylating agent such as an acid chloride provides structures 1. Alkylation to form 2 followed by cleavage of the chiral auxiliary and subsequent alkylation of the dianion of the carboxylic acid 3 provides a variety of disubstituted succinates which can be separated and incorporated into structures of Formula (I) by those skilled in the art. Additional examples are found in P. Becket, M. J. Crimmin, M. H. Davis, Z. Spavold, Synlett, (1993), 137-138, incorporated herein by reference.
[0519] Diastereomerically pure succinate derivatives can be accessed using the chemistry outlined below, adapted from P. Becket, M. J. Crimmin, M. H. Davis, Z. Spavold, Synlett, (1993), 137-138 incorporated herein by reference. This reference provides the synthesis below to obtain compound 9. Compound 11 is used as an intermediate and is prepared from 9 by hydrogenation of the allyl group followed by coupling of 9-fluorenemethanol under standard conditions using DCC and DMAP in CH 2 Cl 2 . Deprotection of the tert-butyl ester is accomplished by treatment with 50% trifluoroacetic acid.
[0520] Succinates compounds wherein R 3 and R 3a combine to form a cycloalkyl or carbocyclic moiety are known in the literature. For example, a dimethyl succinate having a 3-membered cyclopropyl can be formed by a thermal or photolytic decomposition of a methyl 3(carbomethoxymethyl)-1-pyrazoline-3-carboxylate. See Bull. Soc. Chim. Fr. (1971), (6), 2290-5. A succinic acid derivative containing a 4-membered cyclobutyl group can be formed by the method published in U.S. Pat. No. 3,828,025. A succinic acid derivative containing a 5-membered cyclopentyl group can be formed using the methods described in Le Moal, H. et al., Bull. Soc. Chim. Fr., 1964, 579-584; Borenstein, M. R., et al., Heterocycles, 22, 1984, 2433-2438. Other examples of derivatives of succinate X wherein ring C is a five-membered cyclopentyl group or a 6-membered cyclohexyl group have been employed as matrix metalloproteinase inhibitors. See Bioorg. Med. Chem. Lett. (1998), 8(12), 1443-1448; Robinson, R. P., et al., Bioorg. Med. Chem. Lett. (1996), 6(14), 1719-1724. It is understood that these references are only illustrative of the availability of some carbocyclic and cycloalkyl containing succinates, however numerous references are known in literature which provide preparations of other substituted carbocyclic and cycloalkyl containing succinates and their derivatives.
[0521] Scheme 2a illustrates one method for the introduction of a substitution on a carbon adjacent to the cyclic group in succinate X via a deprotonation followed by standard alkylation procedures known to one skilled in the art. Treatment of IX with a base followed by addition of an R 5 -LG, wherein LG is a leaving group such as a halide, mesylate, or a tosylate, and subsequent deprotection of the benzyl group by hydrogenation employing, for example, H 2 and Pd/C, would give the desired cyclic containing succinate X.
[0522] Additional methods useful for the preparation of succinate derivatives are known by those skilled in the art. Such references include McClure and Axt, Bioorganic & Medicinal Chemistry Letters, 8 (1998) 143-146; Jacobson and Reddy, Tetrahedron Letters, Vol 37, No. 46, 8263-8266 (1996); Pratt et al., SYMLETT, May 1998, p. 531; WO 97/18207; and WO 98/51665. The synthetic disclosures of WO97/18207 and WO 98/51665 are hereby incorporated by reference for the preparation of succinate derivatives. A further alkylation of disubstituted succinates such as 204 provides intermediates such as 205 useful as substrates suitable for cyclization reactions known to one skilled in the art, such as ring closing metathesis (RCM) reactions using Grubbs'catalyst as illustrated in Scheme 2b. It will be appreciated by those skilled in the art that the analogous preparation of other cyclization substrates and the use of alternative ring forming methodologies will provide access to carbo- analogs of intermediates 206 and 207. Examples of cyclized succinate derivatives can be found in U.S. Provisional Patent Application No. 60/208,536, incorporated herein by reference for the purpose of enabling cyclized succinate derivatives.
[0523] The compounds of the present invention may be synthesized using the succinates 4 and substituted heterocyclic amines as is shown in Scheme 3.
[0524] Additional examples may be prepared by adding a bifunctional amine followed by preparation of extended derivatives, as is demonstrated in Schemes 4 and 5, using piperazine and 4-piperidinone, respectively. In addition, these transformations may be carried out in parallel on solid phase starting with resin 13 of Scheme 8.
[0525] Additional examples of the compounds of claim 1 can be synthesized as is shown in Scheme 6, thus acylation of the Kenner Safety Catch linker (see Backes, B. J.; Virgilio, A. A.; Ellman, J. A. J.Amer.Chem.Soc. 1996, 118, 3055-3056, Backes, B. J.; Ellman, J. A. J.Amer.Chem.Soc. 1994, 116, 11171-11172, Backes, B. J.; Ellman, J. J.Org.Chem. 1999, 64, 2322-2330) with functionalized aminocyclic amides such as 24 provides the protected succinate 25. Deprotection followed by amide formation gives the succinamide which can be further elaborated upon cleavage to prepare a varitey of compounds such as 27 which are examples of the current invention.
[0526] A wide variety of substituted piperidine derivatives are items of commerce. Additional derivatives are simply prepared starting from benzyl protected 3- or 4-piperidone as is shown in Scheme 7. Addition of lithium or Grignard reagents provides the functionalized piperidinols, which can be used to prepare compounds of this invention. Additionally, dehydration followed by deprotection of the benzyl group and hydrogenation of the olefin provides additional reagents, see for example references 1) V. Breu, H.-P. Maerki, E. Vieira and W. Wostl, WO 00/64873 A1 (2000); 2) B. Lohri and E. Vieira, WO 00/63173 A1 (2000); 3) R. Guller, A. Binggeli, V. Breu, D. Bur, W. Fischli, G. Hirth, C. Jenny, M. Kansy, F. Montavon, M. Muller, C. Oefner, H. Stadler, E. Vieira, M. Wilhelm, W. Wostl and H. P. Marki, Bioorg. Med. Chem. Lett., 9, 1403 (1999); and 4) E. Vieira, A. Binggeli, V. Breu, D. Bur, W. Fischli, R. Guller, G. Hirth, H. P. Marki, M. Muller, C. Oefner, M. Scalone, H. Stadler, M. Wilhelm and W. Wostl, Bioorg. Med. Chem. Lett., 9, 1397 (1999)
[0527] Additionally, the acid 11 can be coupled onto a variety of solid supports to initiate solid-phase parallel synthesis. The solid-phase synthesis of the compounds of claim 1 is shown in Scheme 8, where coupling of 11 to Peptide Amide Linker (PAL) resin (commercially available from Perkin Elmer Biosystems) produces the resin-bound succinamide 37. This coupling can be accomplished using a variety of coupling agents such as diisopropylcarbodiimide (DICI) with the additive 1-hydroxybenzotriazole (HOBt), HATU (O-(7-azabenzotriazol-1-yl)-1,1,3,3,-tetramethyluronium hexafluorophosphate) in the presence of a base such as diisopropylethylamine (DIEA) or triethylamine, PyBOP (benzotriazole-1-yl-oxy-tris-pyrrolidino-phosphonium hexafluorophosphate) or other coupling agents known to those skilled in the art (DICI with hydroxybenzotriazole is preferred). Preferred solvents for coupling reactions include N,N-dimethylformamide (DMF), N-methylpyrrolidinone (NMP), and dichloromethane (DCM).
[0528] The fluorenylmethyl ester is removed from the compounds by treatment with piperidine and the resultant carboxylic acid can be reacted with a variety of animes to form the corresponding amides. Treatment with trifluoroacetic acid in dichloromethane then releases the desired compounds 14 from the solid support.
[0529] Additional methods useful for the preparation of succinate derivatives are known by those skilled in the art. Such references include, McClure and Axt, Bioorganic & Medicinal Chemistry Letters, 8 (1998) 143-146; Jacobson and Reddy, Tetrahedron Letters, Vol 37, No. 46, 8263-8266 (1996); Pratt et al., SYNLETT, May 1998, p. 531; WO 97/18207; and WO 98/51665. The synthetic disclosures of WO97/18207 and WO 98/51665 are hereby incorporated by reference.
EXAMPLES
[0530] Succinate 10 of Scheme 2
[0531] Succinate 9 is prepared according to the literature procedure (P. Becket, M. J. Crimmin, M. H. Davis, Z. Spavold, Synlett, (1993), 137-138). Succinate 9 (17.8 g, 66 mmol) is dissolved in 250 mL of ethyl acetate and placed in a Parr shaker bottle. To the solution is added 890 mg of 5% palladium on carbon, and the bottle is pressurized to 40 psi with hydrogen gas and shaken for 2.5 h at rt. The hydrogen is removed and the palladium catalyst is removed by filtration through a pad of celite. Concentration of the ethyl acetate solution provides 17.5 g (98%) of succinate 10. No further purification is necessary. MS (M−H) + =271.
[0532] Succinate 11 of Scheme 1
[0533] Succinate 10 (6.3 g, 23.1 mmol) is dissolved in 125 mL of CH 2 Cl 2 and 4.8 g (23.3 mmol) of dicyclohexylcarbodiimide is added. The solution is stirred at rt for 30 min and then 4.6 g (23.4 mmol) of 9-fluorenemethanol is added followed by 122 mg (1 mmol) of 4-dimethylaminopyridine. After 5 h of stirring at rt, the reaction solution was diluted with an additional 100 mL of CH 2 Cl 2 and filtered through a pad of celite to remove precipitated dicyclohexylurea. The solution was then washed 3× with 50 mL of a 1N HCl solution, 3× with 50 mL of a saturated sodium bicarbonate solution, and 2× with 50 mL of brine. The crude product was dried over MgSO 4 and concentrated onto 15 g of silica gel. Chromatography eluting with a gradient of 2.5% to 5% ethyl acetate/hexanes provided 6.4 g (61%) of the diester as an oil. The purified diester (6.4 g 14.2 mmol) is then dissolved in 25 mL of CH 2 Cl 2 , 25 mL of trifluoroacetic acid is added, and the reaction solution is stirred at rt for 2 h. The reaction solution is directly concentrated in vacuo to an oil which is then redissolved in 25 mL of toluene and reconcentrated, followed by drying in vacuo to provide 6.3 g (98%) of the desired succinate 9 as an oil which solidifies on standing. MS (M+Na) + =471, (M+2Na) + =439.
[0534] General Procedure for Solid-phase Synthesis According to Scheme 8
[0535] General: The phrase “washed under standard conditions” when applied to a resin refers to rinsing the resin as a slurry three times in DMF followed by 3 times in methanol followed by three times in dichloromethane using approximately 10 mL of solvent per gram of resin.
[0536] Resin 37 of Scheme 8: Commercial Fmoc-PAL resin (Perkin Elmer Biosystems) (9 grams, 0.42 mmol/g, 3.78 mmol) is washed for 20 min with 3×50 mL of 20% piperidine in DMF. The resulting free amine resin is then washed under standard conditions. The resin is then slurried in 100 mL of DMF and and 4.47 grams (11.34 mmol) of succinate 11 is then added, followed by HOBt (1.74 g, 11.34 mmol) and diisopropylcarbodiimide (1.82 mL, 11.34 mmol). The resin is placed on a shaker table for 16 h and then washed under standard conditions and dried in vacuo.
[0537] Resin 38 of Scheme 8: Resin 12 of scheme 3 is washed for 20 min with 3×50 mL of 20% piperidine in DMF. The resulting free carboxylic acid resin is then washed under standard conditions.
[0538] Products 39 of Scheme 8: Six grams of resin is suspended in a 2:3 mixture of DMF and CH 2 Cl 2 and pipetted into 118 of the wells of two commercial polyfiltronics 96-well filter blocks, approximately 50 mg of resin per well. The solvents are removed by filtration, and 200 μL of DMF is added to each reaction well, followed by 110 μL of a 1 M solution of the desired amine in DMF. A stock solution of PyBOP (6.56 g, 12.6 mmol) dissolved in 24 mL of DMF is then prepared, and 200 μL of this solution (0.10 mmol) is added to each well. Diisopropylethylamine (0.21 mmol, 36.5 μL) is then added to each well and the reaction block is sealed and mixed on a shaker table for 16 h. The plates are then washed under standard conditions. The compounds are then cleaved from the solid support employing 1 mL of a 95:5 trifluoroacetic acid/triethylsilane solution for 3 h. The cleavage solution is drained from the well and the resin is washed with an additional 0.5 mL of DCM and the combined filtrates are concentrated. The samples are redissolved in 1 mL of methanol and reconcentrated to remove any volatile impurities.
Examples 1-106
[0539] For each reagent listed in Table 1, the corresponding product 39 was prepared. The products of Examples 1-106 were verified by the presence of the desired compound in ESI MS (M+H + or M+Na + ).
Example 1
[0540] 3(R)-(4-Benzo[1,3]dioxol-5-ylmethyl-piperazine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 418.1.
Example 2
[0541] 5-Methyl-3(R)-(piperazine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 284.1.
Example 3
[0542] 5-Methyl-3(R)-(4-phenyl-piperazine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 360.1.
Example 4
[0543] 3(R)-[4-(2-Methoxy-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 390.1.
Example 5
[0544] 5-Methyl-2(S)-propyl-3(R)-[4-(3-trifluoromethyl-phenyl)-piperazine-1-carbonyl]-hexanoic acid amide. MS [M+H] + 428.1.
Example 6
[0545] 3(R)-[4-(4-Fluoro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 378.1.
Example 7
[0546] 5-Methyl-3(R)-[4-(4-nitro-phenyl)-piperazine-1-carbonyl]-2(S)-propyl-hexanoic acid amide. MS [M+H] + 405.1.
Example 8
[0547] 5-Methyl-3(R)-(4-methyl-piperazine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 298.1.
Example 9
[0548] 3(R)-(4-Benzyl-piperazine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 374.1
Example 10
[0549] 3(R)-[4-(2-Hydroxy-ethyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 328.1
Example 11
[0550] 5-Methyl-2(S)-propyl-3(R)-(4-pyridin-2-yl-piperazine-1-carbonyl)-hexanoic acid amide. MS [M+H] + 361.1.
Example 12
[0551] 3(R)-[4-(2-Chloro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 394.1.
Example 13
[0552] 5-Methyl-3(R)-(3-methyl-4-phenyl-piperazine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 374.1.
Example 14
[0553] 3(R)-[4-(4-Methoxy-phenyl)-3-methyl-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 404.2.
Example 15
[0554] 5-Methyl-2(S)-propyl-3(R)-(4-p-tolyl-piperazine-1-carbonyl)-hexanoic acid amide. MS [M+H] + 374.1.
Example 16
[0555] 3(R)-[4-(3-Methoxy-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 390.1.
Example 17
[0556] [4-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-piperazin-1-yl]-acetic acid ethyl ester. MS [M+H] + 370.1.
Example 18
[0557] 5-Methyl-3(R)-(3-methyl-4-m-tolyl-piperazine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 388.2.
Example 19
[0558] 3(R)-(4-Acetyl-piperazine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 326.1.
Example 20
[0559] 3(R)-(4-Ethyl-piperazine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 312.2.
Example 21
[0560] 5-Methyl-3(R)-[4-(3-phenyl-allyl)-piperazine-1-carbonyl]-2(S)-propyl-hexanoic acid amide. MS [M+H] + 400.2.
Example 22
[0561] 3(R)-{4-[2-(2-Hydroxy-ethoxy)-ethyl]-piperazine-1-carbonyl}-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 372.2
Example 23
[0562] 5-Methyl-2(S)-propyl-3(R)-(4-{2-[(pyridin-2-ylmethyl)-amino]-ethyl}-piperazine-1-carbonyl)-hexanoic acid amide. MS [M+H] + 418.1.
Example 24
[0563] 3(R)-[4-(5-Chloro-2-methyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 408.1.
Example 25
[0564] 5-Methyl-3 (R)-(octahydro-quinoxaline-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 338.5.
Example 26
[0565] 5-Methyl-3(R)-(4-(2-keto-1-benzimidazolinyl)-piperidine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 415.1.
Example 27
[0566] 5-Methyl-3(R)-(2-methyl-piperidine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 297.1.
Example 28
[0567] 1-(3(S)-Carbamoyl- 2 (R)-isobutyl-hexanoyl)-piperidine-2-carboxylic acid ethyl ester. MS [M+H] + 355.1.
Example 29
[0568] 3(R)-(2-Hydroxymethyl-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 313.1.
Example 30
[0569] 1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-piperidine-3-carboxylic acid amide. MS [M+H] + 326.1.
Example 31
[0570] 1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-piperidine-3-carboxylic acid. MS [M+H] + 327.1.
Example 32
[0571] 1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-piperidine-3-carboxylic acid ethyl ester. MS [M+H] + 355.1.
Example 33
[0572] 1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-piperidine-3-carboxylic acid diethylamide. MS [M+H] + 382.2.
Example 34
[0573] 3(R)-(3,5-Dimethyl-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 311.1.
Example 35
[0574] 3(R)-(3-Hydroxymethyl-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 313.1.
Example 36
[0575] 3(R)-(4-Hydroxy-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 299.1.
Example 37
[0576] 1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-piperidine-4-carboxylic acid ethyl ester. MS [M+H] + 355.1.
Example 38
[0577] 5-Methyl-3(R)-(4-methyl-piperidine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 297.1.
Example 39
[0578] 3(R)-(4-Benzyl-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 373.1.
Example 40
[0579] 3(R)-(4-Aminomethyl-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 312.1.
Example 41
[0580] 3(R)-[4-(2-Hydroxy-ethyl)-piperidine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 327.1.
Example 42
[0581] 3(R)-([1,4′]Bipiperidinyl-1′-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 366.2.
Example 43
[0582] 5-Methyl-3(R)-(octahydro-quinoline-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 337.1.
Example 44
[0583] 5-Methyl-3(R)-[4-(2-piperidin-4-yl-ethyl)-piperidine-1-carbonyl]-2(S)-propyl-hexanoic acid amide. MS [M+H] + 394.2.
Example 45
[0584] 3(R)-(3-Hydroxy-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 299.1.
Example 46
[0585] 3(R)-{2-[2-(3,5-Bis-trifluoromethyl-phenylamino)-ethyl]-piperidine-1-carbonyl}-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 538.1.
Example 47
[0586] 3(R)-{2-[2-(4-Isopropyl-phenylamino)-ethyl]-piperidine-1-carbonyl}-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 441.2.
Example 48
[0587] 3(R)-(4-Dimethylamino-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 326.2.
Example 49
[0588] 5-Methyl-3(R)-[4-(3-phenyl-propyl)-piperidine-1-carbonyl]-2(S)-propyl-hexanoic acid amide. MS [M+H] + 401.2.
Example 50
[0589] 5-Methyl-2(S)-propyl-3(R)-(4-propyl-piperidine-1-carbonyl)-hexanoic acid amide. MS [M+H] + 325.2.
Example 51
[0590] 5-Methyl-3(R)-(4-phenyl-4-propionyl-piperidine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 415.1.
Example 52
[0591] 1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-4-dimethylamino-piperidine-4-carboxylic acid amide. MS [M+H] + 369.2.
Example 53
[0592] 5-Methyl-2(S)-propyl-3(R)-(4-pyrrolidin-1-yl-piperidine-1-carbonyl)-hexanoic acid amide. MS [M+H] + 352.2.
Example 54
[0593] 1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-piperidine-4-carboxylic acid amide. MS [M+H] + 326.1.
Example 55
[0594] 5-Methyl-3(R)-(piperidine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 327.1.
Example 56
[0595] 5-Methyl-3(R)-(2-piperidin-1-ylmethyl-piperidine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 380.2.
Example 57
[0596] 1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-4-phenylamino-piperidine-4-carboxylic acid amide. MS [M+H] + 417.1.
Example 58
[0597] 3(R)-{4-[(2-Amino-ethylamino)-methyl]-piperidine-1-carbonyl}-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 355.2.
Example 59
[0598] 1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-4-cyclohexylamino-piperidine-4-carboxylic acid amide. MS [M+H] + 423.2.
Example 60
[0599] 1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-4-ethylamino-piperidine-4-carboxylic acid amide. MS [M+H] + 369.2.
Example 61
[0600] 5-Methyl-3(R)-(3-methyl-3-phenyl-piperidine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 373.1.
Example 62
[0601] 3(R)-[3-Hydroxy-4-(3-trifluoromethyl-phenyl)-piperidine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 443.1.
Example 63
[0602] 3(R)-(3-Bromo-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 361.3.
Example 64
[0603] 3(R)-(3-Hydroxy-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 298.4.
Example 65
[0604] 3(R)-[4-(4-Chloro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 394.1.
Example 66
[0605] 3(R)-[4-(2-Ethoxy-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 404.6.
Example 67
[0606] 3(R)-[4-(4-Fluoro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 378.1.
Example 68
[0607] 3(R)-[4-(2,4-Dimethyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 388.2.
Example 69
[0608] 3(R)-[4-(4-Chloro-phenyl)-3-methyl-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 408.1.
Example 70
[0609] 3(R)-[4-(3,4-Dichloro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 430.0.
Example 71
[0610] 3(R)-[4-(3,4-Dimethyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 388.2.
Example 72
[0611] 3(R)-[4-(2,6-Dimethyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 388.2.
Example 73
[0612] 3(R)-[4-(3-Chloro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 394.1.
Example 74
[0613] 3(R)-[4-(2-Fluoro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 378.1.
Example 75
[0614] 3(R)-[4-(2-Chloro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 394.1.
Example 76
[0615] 3(R)-[4-(2-Nitro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 405.1.
Example 77
[0616] 3(R)-[4-(2-Methyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 374.1.
Example 78
[0617] 3(R)-[4-(2-Ethyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 388.2.
Example 79
[0618] 3(R)-[4-(3-Methyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 374.1.
Example 80
[0619] 3(R)-[4-(4-Chloro-3-trifluoromethyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 462.0.
Example 81
[0620] 3(R)-[4-(4-Methyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 374.1.
Example 82
[0621] 5-Methyl-2(S)-propyl-3(R)-(4-pyrimidin-2-yl-piperazine-1-carbonyl)-hexanoic acid amide. MS [M+H] + 361.1.
Example 83
[0622] 3(R)-[4-(2,3-Dimethyl-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 388.2.
Example 84
[0623] 5-Methyl-2(S)-propyl-3(R)-(4-pyridin-4-yl-piperazine-1-carbonyl)-hexanoic acid amide. MS [M+H] + 361.1.
Example 85
[0624] 3(R)-[4-(3,5-Dichloro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 428.1.
Example 86
[0625] 5-Methyl-2(S)-propyl-3(R)-[4-(4-trifluoromethyl-phenyl)-piperazine-1-carbonyl]-hexanoic acid amide. MS [M+H] + 428.1.
Example 87
[0626] 5-Methyl-2(S)-propyl-3(R)-(4-pyrazin-2-yl-piperazine-1-carbonyl-carbonyl)-hexanoic acid amide. MS [M+H] + 362.1.
Example 88
[0627] 3(R)-[4-(2-Cyano-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 385.1.
Example 89
[0628] 3(R)-[4-(2,4-Dimethoxy-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 420.1.
Example 90
[0629] 3(R)-(4-Benzo[1,3]dioxol-5-yl-piperazine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 404.1.
Example 91
[0630] 5-Methyl-3(R)-(3-methyl-4-p-tolyl-piperazine-1-carbonyl)-2(S)-propyl-hexanoic acid amide. MS [M+H] + 388.2.
Example 92
[0631] 3(R)-[4-(3-Methoxy-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 390.1.
Example 94
[0632] 3(R)-[4-(4-Chloro-3-trifluoromethyl-phenyl)-4-hydroxy-piperidine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 477.0.
Example 96
[0633] 3(R)-{4-[(4-Chloro-phenyl)-phenyl-methyl]-piperazine-1-carbonyl}-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 485.1.
Example 97
[0634] 5-Methyl-3(R)-[2-(1-methyl-pyrrolidin-2-ylmethyl)-piperidine-1-carbonyl]-2(S)-propyl-hexanoic acid amide. MS [M+H] + 380.0.
Example 98
[0635] 5-Methyl-2(S)-propyl-3(R)-[4-(5-trifluoromethyl-pyridin-2-yl)-piperazine-1-carbonyl]-hexanoic acid amide. MS [M+H] + 429.1.
Example 99
[0636] 5-Methyl-2(S)-propyl-3(R)-[4-(3-trifluoromethyl-pyridin-2-yl)-piperazine-1-carbonyl]-hexanoic acid amide. MS [M+H] + 428.492.
Example 100
[0637] 3(R)-(4-Cyano-4-phenyl-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 384.1.
Example 101
[0638] 3(R)-(4-Hydroxy-4-phenyl-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 375.1.
Example 102
[0639] 5-Methyl-2(S)-propyl-3(R)-(4-pyrrolidin-1-yl-piperidine-1-carbonyl)-hexanoic acid amide. MS [M+H] + 352.2.
Example 103
[0640] 3(R)-(4-Acetyl-4-phenyl-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 401.1.
Example 104
[0641] 3(R)-[4-(4-Chloro-phenyl)-4-hydroxy-piperidine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 392.1.
Example 105
[0642] 3(R)-[4-(3-Hydroxy-propyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 342.1.
Example 106
[0643] 3(R)-[4-(3-Chloro-phenyl)-piperazine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide. MS [M+H] + 395.1.
TABLE 1 39 Reagent Name Molecular Weight Example for (un)substituted Ring B of Product 1 1-piperonylpiperazine 418.1 2 piperazine 284.1 3 1-phenylpiperazine 360.1 4 1-(2-methoxyphenyl)piperazine 390.1 5 n-(3-trifluoromethylphenyl)piperazine 428.1 6 1-(4-fluorophenyl)piperazine 378.1 7 1-(4-nitrophenyl)piperazine 405.1 8 1-methylpiperazine 298.1 9 1-benzylpiperazine 374.1 10 n-(2-hydroxyethyl)piperazine 328.1 11 1-(2-pyridyl)piperazine 361.1 12 1-(2-chlorophenyl)-piperazine, monohydrochloride 394.1 13 2-methyl-1-phenylpiperazine 374.1 14 1-(4-methoxyphenyl)-2-methylpiperazine 404.2 15 1-(p-tolyl)-piperazine dihydrochloride 374.1 16 1-(3-methoxyphenyl)piperazine dihydrochloride 390.1 17 n-(carboethoxymethyl)piperazine 370.1 18 2-methyl-1-(3-methylphenyl)piperazine 388.2 19 1-acetylpiperaine 326.1 20 n-ethylpiperazine 312.2 21 trans-1-cinnamylpiperazine 400.2 22 1-hydroxyethylethloxypiperazine 372.2 23 1-(2-(2-pyridylmethylamino)-ethyl)-piperazine 418.1 24 1-(5-chloro-ortho-tolyl)-piperazine 408.1 25 perhydroquinoxaline 338.5 26 4-(2-keto-1-benzimidazolinyl)piperidine 415.1 27 2-methylpiperidine 297.1 28 ethyl pipecolinate 355.1 29 2-piperidinemethanol 313.1 30 nipecotamide 326.1 31 nipecotic acid 327.1 32 ethyl nipecotate 355.1 33 n,n-diethylnipecotamide 382.2 34 3,5-dimethylpiperidine 311.1 35 3-piperidinemethanol 313.1 36 4-hydroxypiperidine 299.1 37 ethyl isonipecotate 355.1 38 4-methylpiperidine 297.1 39 4-benzylpiperidine 373.1 40 4-(aminomethyl)piperidine 312.1 41 4-piperidineethanol 327.1 42 4-piperidinopiperidine 366.2 43 decahydroquinoline 337.1 44 4,4′-ethylenedipiperidine 2HCl 394.2 45 3-hydroxypiperidine 299.1 46 N-[2-(2-piperidyl)ethyl]-3,5-bis-(trifluoromethyl)aniline 538.1 47 2-(2-(4-isopropylanilino)ethyl)-piperidine 444.2 48 4-(dimethylamino)-piperidine 326.2 49 4-(3-phenylpropyl)-piperidine 401.2 50 4-n-propylpiperidine 325.2 51 4-phenyl-4-propionylpiperidine HCl 415.1 52 4-carbamoyl-4-(dimethylamino)piperidine dihydrochloride 369.2 53 4-(1-pyrrolidinyl)piperidine 352.2 54 isonipecotamide 326.1 55 d1-pipecolinic acid 327.1 56 2-(piperidinomethyl)-piperidine 380.2 57 4-anilino-4-carbamylpiperidine 417.1 58 n-(4-piperidylmethyl)-ethylenediamine 355.2 59 4-(cyclohexylamino)-isonipecotamide 423.2 60 4-(ethylamino)-isonipecotamide 369.2 61 3-methyl-3-phenylpiperidine 373.1 62 4-(3-(trifluoromethyl)phenyl)-3-piperidinol HCl 443.1 63 4-bromopiperidine HBr 361.3 64 (r)-(+)-3-hydroxypiperidine HCl 298.4 65 1-(4-chlorophenyl)piperazine 2HCl 394.1 66 1-(2-ethoxyphenyl)piperazine HCl 404.6 67 1-(4-fluorophenyl)piperazine 2HCl 378.1 68 1-(2,4-dimethylphenyl)piperazine 388.2 69 1-(4-chlorophenyl)-2-methylpiperazine 408.1 70 n-(3,4-dichlorophenyl)piperazine 430.0 71 1-(3,4-dimethylphenyl)piperazine 388.2 72 1-(2,6-dimethylphenyl)piperazine 388.2 73 1-(3-chlorophenyl)piperazine HCl 394.1 74 1-(2-fluorophenyl)piperazine 378.1 75 1-(2-chlorophenyl)piperazine 394.1 76 1-(2-nitrophenyl)piperazine 405.1 77 1-(2-methylphenyl)piperazine 374.1 78 1-(2-ethylphenyl)piperazine 388.2 79 1-(3-methylphenyl)piperazine 374.1 80 1-(3-trifluoromethyl-4-chlorophenyl)-piperazine 462.0 81 1-(4-methylphenyl)piperazine 374.1 82 1-(2-pyrimidyl)piperazine 362.1 83 1-(2,3-dimethylphenyl)piperazine 388.2 84 1-(4-pyridyl)piperazine 361.1 85 1-(3,5-dichlorophenyl)piperazine 428.1 86 1-(4-trifluoromethylphenyl)piperazine 428.1 87 1-(2-pyrazinyl)piperazine 362.1 88 1-(2-cyanophenyl)piperazine 385.1 89 1-(2,4-dimethoxyphenyl)piperazine 420.1 90 1-(3,4-methylenedioxyphenyl)piperazine hydrochloride 404.1 91 1-(4-methylphenyl)-2-methylpiperazine 388.2 92 1-(3-methoxyphenyl)piperazine 2HCl 390.1 93 1,3-dihydro-1-(1,2,3,6-tetrahydro-4-pyridinyl)-2h-benzimidazole-2-one 413.1 94 4-[4-chloro-3-(trifluoromethyl)phenyl]-4-piperidinol 477.0 95 4-(2-keto-1-benzimidazolinyl)piperidine 415.1 96 1-(4-chlorobenzhydryl)piperazine 485.1 97 (s)-(−)-1-methyl-2-(1-piperidino-methyl)pyrrolidine 380.0 98 1-[5-(trifluoromethyl)pyrid-2-yl]-piperazine 429.1 99 1-[3-(trifluoromethyl)pyrid-2-yl]piperazine 429.1 100 4-cyano-4-phenylpiperidine HCl 384.1 101 4-hydroxy-4-phenylpiperidine 375.1 102 4-(1-pyrrolidinyl)piperidine 352.2 103 4-acetyl-4-phenylpiperidine HCl 401.1 104 4-(4-chlorophenyl)-1,2,3,6-tetrahydropyridine HCl 392.1 105 1-piperazinepropanol 342.1 106 1-(3-chlorophenyl)piperazine 395.1
5-Methyl-2(S)-propyl-3(R)-[4-(3-trifluoromethyl-benzylamino)-piperidine-1-carbonyl]-hexanoic acid amide.
[0644] [0644]
[0645] Fmoc-Pal resin (1.000 g, 0.355 mmol/g) was washed and deprotected with 50% Piperidine/DMF for 10 min. The resin was washed and suspended in DMF. Addition of 3 eq (1.065 mmoles, M.W.=394, 419.6 mg) of Succinic acid fluorenylmethyl ester (11) followed by 3 eq (1.065 mmoles, M.W.=153, 163 mg) of HOBt and 3 eq (1.065 mmoles, M.W.=126.2, d=0.806, 352 μL) of N,N-Diisopropylcarbodiimide and the reaction solution was allowed to shake overnight. A small sample was monitored by Ninhydrin test (negative). The resin was washed thoroughly with DMF, MeOH, CH 2 Cl 2 and DMF. About 100 mg (sub=0.033mmoles) of resin was taken and deprotected with 50% Piperidine/DMF for 10 min. The resin was washed thoroughly and suspended in DMF. Then 5 eq (0.165 mmoles, M.W.=153.61, 253 mg) of 4-Piperidone monohydrate.HCl was added followed by 5 eq (0.165 mmoles, M.W.=520.3, 86 mg) of PyBOP and 10 eq (0.33 mmoles, M.W.=129.25, d=0.742, 58 μL) of DIEA. Another 5 eq of DIEA was added to neutralize the HCL salt, and the reaction solution was allowed to shake overnight.
[0646] The resin was washed thoroughly with DMF, MeOH and CH 2 Cl 2 and suspended in DCM. It was reductively alkylated with 5 eq (0.165 mmoles, M.W.=175.16, d=1.222, 24 μL) of 3-trifluoromethyl benzylamine followed by 5 eq (0.165 mmoles, M.W.=212, 35mg) of NaBH(OAc) 3 and 1% AcOH (v/v, 10 μL) and allowed to shake overnight. Next day, a small sample was checked with Chloranil test (positive). The resin was washed thoroughly with DMF, MeOH and CH 2 Cl 2 and dried well under vacuum. The resin was treated with a mixture of TFA/CH 2 Cl 2 (9:1) for 2 h, filtered and concentrated in vacuum to give the crude compound. Purification by preparative LC/MS provided the title compound of example 107 as a powder(8 mg). MS (M+H) + =456.6.
Examples 108-116
[0647] For each reagent listed in Table 2, the corresponding product was prepared according to the preparation of the compound of Example 107. The products of Examples 108-116 were verified by the presence of the desired compound in ESI MS (M+H) + .
TABLE 2 (M + H) + Ex # AMINE Final Product observed 108 1-Naphthalene 5-Methyl-3(R)-{4[(naphthalen-1- 438.4 methylamine ylmethyl)-amino]-piperidine-1- carbonyl}-2(S)-propyl-hexanoic acid amide 109 3,4-Methylene 3(R)-[4-(Benzo[1,3]dioxol-5- 418.4 dioxyaniline ylamino)-piperidine-1-carbonyl]-5- methyl-2(S)-propyl-hexanoic acid amide. 110 Aniline 5-Methyl-3(R)-(4-phenylamino- 374.4 piperidine-1-carbonyl)-2(S)- propyl-hexanoic acid amide. 111 m-Anisidine 3(R)-[4-(3-Methoxy-phenylamino)- 404.4 piperidine-1-carbonyl]-5-methyl- 2(S)-propyl-hexanoic acid amide. 112 Isopropylamine 3(R)-(4-Isopropylamino-piperidine- 340.4 1-carbonyl)-5-methyl-2(S)-propyl- hexanoic acid amide. 113 3-Methoxy-4- 3(R)-[4-(3-Methoxy-4-methyl- 418.4 methylaniline phenylamino)-piperidine-1- carbonyl]-5-methyl-2(S)-propyl- hexanoic acid amide. 114 Benzhydrylamine 3(R)-[4-(Benzhydryl-amino)- 464.4 piperidine-1-carbonyl]-5-methyl- 2(S)-propyl-hexanoic acid amide 115 3-Fluoro-5- 3(R)-[4-(3-Fluoro-5- 474.4 (trifluoromethyl) trifluoromethyl-benzylamino)- benzylamine piperidine-1-carbonyl]-5-methyl- 2(S)-propyl-hexanoic acid amide. 116 4- 5-Methyl-2(S)-propyl-3(R)-[4-(4- 442.4 Trifluoromethyl trifluoro-methyl-phenylamino)- aniline piperidine-1-carbonyl]-hexanoic acid amide.
Example 117
N-[1-(3(S)-Carbamoyl-2(R)-isobutyl-hexanoyl)-piperidin-4-yl]-N-naphthalen-1-ylmethyl-benzamide.
[0648] Fmoc-Pal resin (1.000 g, 0.355 mmol/g) was washed and deprotected with 50% Piperidine/DMF for 10 min. The resin was washed and suspended in DMF. Addition of 3 eq (1.065 mmoles, M.W.=394, 419.6 mg) of Succinic acid fluorenylmethyl ester (11) followed by 3 eq (1.065 mmoles, M.W.=153, 163 mg) of HOBt and 3 eq (1.065 mmoles, M.W.=126.2, d=0.806, 352 μL) of N,N-Diisopropylcarbodiimide and the reaction solution was allowed to shake overnight. A small sample was monitored by Ninhydrin test (negative). The resin was washed thoroughly with DMF, MeOH, CH 2 Cl 2 and DMF. About 100 mg (sub=0.033 mmoles) of resin was taken and deprotected with 50% Piperidine/DMF for 10 min. The resin was washed thoroughly and suspended in DMF. Then 5 eq (0.165 mmoles, M.W.=153.61, 253 mg) of 4-Piperidone monohydrate.HCl was added followed by 5 eq (0.165 mmoles, M.W.=520.3, 86 mg) of PyBOP and 10 eq (0.33 mmoles, M.W.=129.25, d=0.742, 58 μL) of DIEA. Another 5 eq of DIEA was added to neutralize the HCL salt, and the reaction solution was allowed to shake overnight.
[0649] The resin was washed thoroughly with DMF, MeOH and CH 2 Cl 2 and suspended in DCM. It was reductively alkylated with 5 eq (0.165 mmoles, M.W.=157.16, 26 mg) of 1-naphthylmethylamine followed by 5 eq (0.165 mmoles, M.W.=212, 35 mg) of NaBH(OAc) 3 and 1% AcOH (v/v, 10 μL) and allowed to shake overnight. Next day, a small sample was checked with Chloranil test (positive).
[0650] The resin was washed thoroughly with DMF, MeOH and CH 2 Cl 2 and dried well under vacuum. The resin was then suspended in DMF and acylated with 12 eq (0.075 mmoles, M.W.=129.25, d=0.742, 131 μL) of DIEA and 10 eq (0.625 mmoles, M.W.=140.57, d=1.211, 73 μL) of Benzoyl Chloride and allowed to shake overnight. The resin was then washed thoroughly with DMF, MeOH and CH 2 Cl 2 and dried well under vacuum. The resin was cleaved with a mixture of TFA/ CH 2 Cl 2 (9:1) for 3 h, filtered and concentrated in vacuum to give the crude compound. Purification by preparative LC/MS provided the title compound of example 117 as a white powder MS (M+H) + =542.4.
Examples 118-122
[0651] For each reagent listed in Table 3, the corresponding product was prepared according to the preparation of the compound of Example 117. The products of Examples 118-122 were verified by the presence of the desired compound in ESI MS (M+H) + .
TABLE 3 (M + H) + Ex # AMINE Final Product observed 118 3,4-Methylene N-Benzo[1,3]dioxol-5-yl-N-[1- 522.3 dioxyaniline (3(S)-carbamoyl-2(R)-isobutyl- hexanoyl)-piperidin-4-yl]- benzamide. 119 Aniline N-[1-(3(S)-Carbamoyl-2(R)- 478.3 isobutyl-hexanoyl)-piperidin-4-yl]- N-phenyl-benzamide. 120 m-Anisidine N-[1-(3(S)-Carbamoyl-2(R)- 508.4 isobutyl-hexanoyl)-piperidin-4-yl]- N-(3-methoxy-phenyl)-benzamide. 121 Isopropylamine N-[1-(3(S)-Carbamoyl-2(R)- 444.4 isobutyl-hexanoyl)-piperidin-4-yl]- N-isopropyl-benzamide. 122 3-Fluoro-5- N-[1-(3(S)-Carbamoyl-2(R)- 578.4 (trifluoromethyl) isobutyl-hexanoyl)-piperidin-4-yl]- benzylamine N-(3-fluoro-5-trifluoromethyl- benzyl)-benzamide.
[0652] [0652]
Example 123
5-Methyl-3(R)-{3-[(naphthalen-1-ylmethyl)-amino]-piperidine-1-carbonyl}-2(S)-propyl-hexanoic acid amide
[0653] 3-benzylpiperidine HC 1 hydrate 10 g, 41 mmol) was dissolved in 100 mL of methanol and placed in a Parr flask. A 0.5 g portion of 10% palladium on carbon was added and the reaction solution was shaken under 50 p.s.i. of dihydrogen for 16 h. The catalyst was removed by filtration and the solvent was removed in vacuo to provide the crude 3-piperidone which was used without further purification.
[0654] The compound of example 123 was then prepared according to the preparation of the compound of example 107 but using 3-piperidone, yielding 11 mg of the desired compound. MS (M+H) + =438.4.
Examples 124-129
[0655] For each reagent listed in Table 4, the corresponding product was prepared according to the preparation of the compound of Example 123. The compounds of Examples 128 and 129 were prepared according to the preparation of the compound of Example 117, but using 3-piperidone. The products of Examples 124-129 were verified by the presence of the desired compound in ESI MS (M+H) + .
TABLE 4 (M + H) + Ex # AMINE Product Structure observed 124 3-Methoxy-4- 3(R)-[3-(3-Methoxy-4-methyl- 418.4 methylaniline phenylamino)-piperidine-1- carbonyl]-5-methyl-2(S)-propyl- hexanoic acid amide. 125 Aniline 5-Methyl-3(R)-(3-phenylamino- 374.4 piperidine-1-carbonyl)-2(S)- propyl-hexanoic acid amide. 126 m-Anisidine 3(R)-[3-(3-Methoxy-phenylamino)- 404.4 piperidine-1-carbonyl]-5-methyl- 2(S)-propyl-hexanoic acid amide. 127 3-Fluoro-5- 3(R)-[3-(3-Fluoro-5- 474.4 (trifluoromethyl) trifluoromethyl-benzylamino)- benzylamine piperidine-1-carbonyl]-5-methyl- 2(S)-propyl-hexanoic acid amide. 128 1- N-[1-(3(S)-Carbamoyl-2(R)- 542.4 Naphthalene- isobutyl-hexanoyl)-piperidin-3- methylamine yl]-N-naphthalen-1-ylmethyl- benzamide. 129 3-Fluoro-5- N-[1-(3(S)-Carbamoyl-2(R)- 578.4 (trifluoromethyl) isobutyl-hexanoyl)-piperidin-3- benzylamine yl]-N-(3-fluoro-5- trifluoromethyl-benzyl)- benzamide.
Example 130
3(R)-[4-Hydroxy-4-(4′-trifluoromethyl-biphenyl-4-yl)-piperidine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide
[0656] [0656]
Example 130(a)
[0657] 2-Chlorotrityl chloride resin (Novabiochem, 0.250 g, 0.21 mmol) was washed and suspended in DCM. Then ˜2 eq (0.5 mmol, M.W.=394.5, 197 mg) of fluorenylmethyl protected succinic acid derivative was added and the resin was allowed to shake for 5 min. Then 2 eq (with respect to acid) (1.0 mmole, M.W.=129.25, d=0.742, 174 μL) of DIEA was added and the resin was allowed to shake overnight. The resin was washed thoroughly and the fluorenylmethyl group was deprotected with 50% Piperidine/DMF for 10 min and the resin was washed again.
Example 130(b)
[0658] A 120 mg portion (0.1 mmol) of the resin from example 130(a) was suspended in DMF and then treated with 5 eq (0.5 mmol, M.W.=256.14, 128 mg) of 4-(4-Bromophenyl)-4-Piperidinol, 5 eq (o.5 mmol, M.W.=520.3, 260 mg) of PyBop and 10 eq (1.0 mmol, M.W.=129.25, d=0.742, 174 μL) of DIEA. The resin was allowed to shake overnight and then washed with DMF, dichloromethane, and methanol.
Example 130(c)
[0659] The resin from example 130(b) (50 mg, 0.8 mmol/g, 0.040 μmol) was suspended in 1 mL of THF and 15 mg of tetrakis(triphenylphosphine)palladium (0), 70 mg (0.37 mmol) of 4-trifluoromethylphenyl boronic acid, and 200 μL of a 2 M sodium carbonate solution were added. The suspension was heated to 60° C. for 16 h, and the esin was isolated by filtration and washed with DMF, dichloromethane, and methanol.
[0660] Preparation of the Title Compound of Example 130
[0661] The resin from example 130(c) was suspended in 2 mL of a 1:1:8 solution of acetic acid, trifluoroethanol, and dichloromethane and the suspension was stirred for 1 h. Evaporation gave the crude acid which was dissolved in 1 mL of DMF and treated with HATU (4 mg, 0.01 mmol) and N-methylmorpholine (5 μL, 0.04 mmol). After 5 min ammonia was introduced by bubbling and the solution was allowed to stir for 16 h. The solution was then partitioned between ethyl acetate and water and the organic layer was isolated, dried and concentrated. Purification by RP-HPLC afforded 1.0 mg (10%) of the title compound of example 130. MS (M+H) + =519.4, (M+Na) + =541.4.
Example 131
3(R)-(4-Biphenyl-4-yl-4-hydroxy-piperidine-1-carbonyl)-5-methyl-2(S)-propyl-hexanoic acid amide
[0662] The compound of Example 131 was prepared in a manner analogous to the preparation of the compound of Example 130, but using phenylboronic acid. Purification by RP-HPLC afforded 1 mg (10%) of the title compound of example 131. MS (M+H) + =451.4,
Example 132
3(R)-[3-(4-Fluoro-phenyl)-3-hydroxy-piperidine-1-carbonyl]-5-methyl-2(S)-propyl-hexanoic acid amide
Example 132(a)
[0663] To a solution of 2 g (10.6 mmol) of 3-piperidione in 50 mL of THF at 0° C. is added dropwise 10 mL of a 1M solition of 4-fluorophenylmagnesium bromide in THF. After 30 min, the reaction was quenched with 1N HCl and the THF was removed by rotary evaporation. The resultant aqueous layer was extracted twice with 50 mL of CH 2 Cl 2 to provide 1.9 g (66%) of an oil which was used without further purification.
Example 132(b)
[0664] The oil from above was dissolved in 25 mL of methanol and 380 mg of 20% paddadium on carbon was added. The reaction solution was placed under 50 p.s.i. of dihydrogen and shaken at rt for 16 h. The catalyst was then removed by filtration and the resulting piperidine was used without further purification.
Example 132(c)
[0665] To a 0.2 g portion of resin from example 130(a) (0.16 mmol, 0.83 mmol/g) was added 0.83 mmol (162 mg) of the compound of example 135(b), 0.83 mmol (432 mg) of PyBop, and 1.66 mmol (289 μL) of DIEA. The suspension was stirred for 2 days and then the resin was washed thoroughly with DMF, DCM, and methanol. The resin was then suspended in 2 mL of a 1:1:8 solution of acetic acid, trifluoroethanol, and dichloromethane and the suspension was stirred for 2 h. Evaporation gave the crude acid (56 mg, 83%) which was used without further purification.
[0666] Preparation of the Title Compound of Example 132
[0667] The acid of example 132(c) (56 mg, 0.142 mmol) was dissolved in 2 mL of DMF and 70 mg (0.184 mmol) of HATU and 62 μL (0.57 mmol) of N-methylmorpholine was added. After 1 h ammonia gas was introduced by bubbling for 1 min and the reaction solution was allowed to stir for 16. The reaction solution was then partitioned between dichloromethane and water and the organic layer was separated, dried, and concentrated. Purification by RP-HPLC afforded 10 mg (18%) of the title compound of example 132 as a white powder. MS (M+H) + =393.5, (M+Na) + =415.4.
Example 134
4(S)-Benzyloxy-1-(3(S)-carbamoyl-2(R)-isobutyl-hexanoyl)-pyrrolidine-2(S)-carboxylic acid phenethyl-amide
Example 134(a)
[0668] 7.3 g of succinate 10 of scheme 2 was dissolved in 70 mL of DMF and activated with 13.3 g of HATU and 14.73 mL of N-methylmorpholine. After stirring at rt for 30 min 7.4 g of 4(S)-benzylhydroxyproline methyl ester hydrochloride was added and the reaction solution was stirred at rt for 2 h. The reaction solution was diluted with 100 mL of water and the resulting solution was extracted 3× with ethyl acetate. The combined organic layers were dried and concentrated and ther residue was purified by chromatography eluting with 10-25% ethyl acteate in hexanes to provide 8.4 g (66%) of the desired amide. MS (M+H) + =490.4
Example 134(b)
[0669] The methyl ester from example 134(a) (8.4 g, 17.1 mmol) in 30 mL of dioxane was cooled to 0° C. and 20 mL of 1 N NaOH was added. The solution was stirred for 2 h and additional portions of dioxane (15 mL) and NaOH (20 mL) were added, followed by stiring for another 2 h. The reaction solution was then acidified to pH 3 with citric acid and then extracted 3× with ethyl acetate. The combined organic layers were dried and concentrated to provide the crude acid which required no further purification. MS (M+H) + =476.3
Example 134(c)
[0670] Alkanesufonamide safety catch resin (Novabiochem, 4.5 g, 0.8 mmol/g, 3.6 mmol) was washed well and then suspended in 50 mL of DMF. The acid from example 134(b) (5.133 g, 10.8 mmol), PyBop (5.62 g, 10.8 mmol) and DIEA (5.65 mL, 32.4 mmol) were added and the suspension was shaken for 16 h. The resin was then rinsed thoroughly with DMF, dichloromethane, and methanol and dried.
Example 134(d)
[0671] A 25 mg portion of the resin from example 134(c) (0.02 mmol) was suspended in a 1:1 solution of dichloromethane and tricluoroacetic acid (0.5 mL) and allowed to shake for 2 h at rt. The resin was then washed thoroughly, and resuspended in 0.5 mL of DMF.and treated with HATU (38 mg, 0.1 mmol) and 150 mL of a saturated solution of ammonia in THF. The reaction suspension was allowed to stir at rt for 1.5 h and then the resin was washed thoroughly.
[0672] Preparation of the Title Compound of Example 134
[0673] The resin from example 138(d) was suspended in 0.5 mL of NMP and activated with 0.1 mmol of DIEA (18 μL) and 0.25 mmol (30 μL) of bromoacetonitrile at rt for 16 h. The resin was then washed thoroughly and suspended in 300 uL of THF to which 0.008 mmol of phenethylamine (40 uL of a 0.2M solution) was added. The reaction solution was stirred at rt for 2 days and then concentrated to provide 2.6 mg of the title compound of example 134 (63%). MS (M+H) + =522.3, MS ESI − , (M−H) − =520.2.
[0674] Tables 5a-5g below provide representative Examples of the compounds of Formula (I) of the present invention.
TABLE 5a Molecular Weight Ex # L Z R 11 of Product 1 —CH 2 — 4-benzo[1,3]dioxol-5-yl H 417.54 2 — H H 283.407 3 — phenyl H 359.505 4 — 2-MeO-phenyl H 389.53 5 — 3-CF 3 -phenyl H 427.502 6 — 4-F-phenyl H 377.495 7 — 4-NO 2 -phenyl H 404.502 8 —CH 2 — H H 297.434 9 —CH 2 — phenyl H 373.531 10 —CH 2 CH 2 O— H H 327.46 11 — 2-pyridyl H 360.493 12 — 2-Cl-phenyl H 394 13 — phenyl Me 373.531 14 — 4-MeO-phenyl Me 403.557 15 — 4-Me-phenyl H 373.5 16 — 3-MeO-phenyl H 389.5 18 — 3-Me-phenyl Me 387.558 20 —CH 2 CH 2 — H H 311.461 21 —CH 2 CH═CH 2 — phenyl H 399.569 22 —(CH 2 ) 2 —O—(CH 2 ) 2 — H H 371.512 23 —(CH 2 ) 2 —NH—CH 2 — 2-pyridyl H 417.588 24 — 2-Me-5-Cl-phenyl H 407.976 65 — 4-Cl-phenyl H 394 66 — 2-EtO-phenyl H 403.6 67 — 4-F-phenyl H 377.5 68 — 2,4-diMe-phenyl H 387.561 69 — 4-Cl-phenyl Me 407.979 70 — 3,4-diCl-phenyl H 428.397 71 — 3,4-diMe-phenyl H 387.561 72 — 2,6-diMe-phenyl H 387.561 73 — 3-Cl-phenyl H 394 74 — 2-F-phenyl H 377.497 75 — 2-Cl-phenyl H 393.952 76 — 2-NO 2 -phenyl H 404.504 77 — 2-Me-phenyl H 373.534 78 — 2-Et-phenyl H 387.561 79 — 3-Me-phenyl H 373.534 80 — 3-CF 3 -4-Cl-phenyl H 461.95 81 — 4-Me-phenyl H 373.534 82 — 2-pyrimidyl H 361.482 83 — 2,3-diMe-phenyl H 387.561 84 — 4-pyridyl H 360.494 85 — 3,5-diCl-phenyl H 428.397 86 — 4-CF 3 -phenyl H 427.505 87 — 2-pyrazinyl H 361.482 88 — 2-CN-phenyl H 384.516 89 — 2,4-diMeO-phenyl H 419.559 90 — 4-benzo[1,3]dioxol-5-yl H 403.5 91 — 4-Me-phenyl Me 387.561 92 — 3-MeO-phenyl H 389.5 96 — 4-chlorobenzhydryl H 485.1 98 — 5-CF 3 -pyrid-2-yl H 428.492 99 — 3-CF 3 -pyrid-2-yl H 428.492 105 —(CH 2 ) 3 —O— H H 341.486 106 — 3-Cl-phenyl H 393.95
[0675] [0675] TABLE 5a″ Molecular Weight Ex # R 10 R 11 of Product 17 —CH 2 C(═O)OEt H 369.496 19 —C(═O)Me H 325.444 96 4-Cl-benzhydryl H 484.077
[0676] [0676] TABLE 5b Ex # L Z Mol Wt 26 — 2-keto-1-benzimidazolinyl 414.54 36 O H 298.418 38 —CH 2 — H 296.446 39 —CH 2 — phenyl 372.543 40 —CH 2 —NH— H 311.461 41 —(CH 2 ) 2 —O— H 326.472 42 — N-piperidyl 365.552 44 —CH 2 CH 2 — 4-piperidyl 393.6 49 —(CH 2 ) 3 — phenyl 400.597 50 —(CH 2 ) 3 — H 324.499 58 —CH 2 —NH—(CH 2 ) 2 — NH 2 354.529 102 — 1-pyrrolidinyl 351.527 107 —NH—CH 2 — 3-CF 3 -phenyl 456.6 108 —NH—CH 2 — naphthalen-1-yl 438.4 109 —NH— 3,4-(methylendioxy)-phenyl 418.4 110 —NH— phenyl 374.4 111 —NH— 3-MeO-phenyl 404.4 112 —NH— i-propyl 340.4 113 —NH— 3-MeO-4-Me-phenyl 418.4 114 —NH— benzhydryl 464.4 115 —NH—CH 2 — 3-CF 3 -5-F-phenyl 474.4 116 —NH— 4-CF 3 -phenyl 442.4 117 —N(benzoyl)-CH 2 — naphthalen-1-yl 542.4 118 —N(benzoyl)- 3,4-(methylendioxy)-phenyl 522.33 119 —N(benzoyl)- phenyl 478.3 120 —N(benzoyl)- 3-MeO-phenyl 508.4 121 —N(benzoyl)- i-propyl 444.4 122 —N(benzoyl)-CH 2 — 3-CF 3 -5-F-phenyl 578.4
[0677] [0677] TABLE 5c Ex # L Z Mol Wt 123 —NH—CH 2 — naphthalen-1-yl 438.4 124 —NH— 3-MeO-4-Me-phenyl 418.4 125 —NH— phenyl 374.4 126 —NH— 3-MeO-phenyl 404.4 127 —NH—CH 2 — 3-CF 3 -5-F-phenyl 474.4 128 —N(benzoyl)-CH 2 — naphthalen-1-yl 542.4 129 —N(benzoyl)-CH 2 — 3-CF 3 -5-F-phenyl 578.4
[0678] [0678] TABLE 5d Ex # L Z R 11 Mol Wt 30 — H —C(═O)NH 2 325.444 31 — H —C(═O)OH 326.428 32 — H —C(═O)OEt 354.482 33 — H —C(═O)N(Et) 2 381.551 35 — H —CH 2 OH 312.445 45 — H —OH 298.418 62 — 3-CF 3 -phenyl —OH 442.5 64 — H —OH 298.4 133 — 3-CF 3 -phenyl —OH
[0679] [0679] TABLE 5e Molecular Weight Ex # L Z of Product 27 — methyl 296.446 28 — —C(═O)OEt 354.482 29 — —CH 2 OH 312.445 46 —CH 2 CH 2 NH— 3,5-bis-CF 3 -phenyl 537.579 47 —CH 2 CH 2 NH— 4-iPr-phenyl 443.665 55 — —C(═O)OH 326.428 56 —CH 2 — N-piperidino 379.579 97 —CH 2 — 1-Me-pyrrolidin-2-yl 379.581
[0680] [0680] TABLE 5f Molecular Weight Ex # L Z R 11 of Product 34 — H Me 310.472
[0681] [0681] TABLE 5g Ex # L Z R 11 Mol Wt 37 — H —C(═O)OEt 354.482 48 — H —N(Me) 2 325.487 51 — phenyl —C(═O)Et 414.6 52 —N(Me)— Me —C(═O)NH 2 368.5 53 — H 1-pyrrolidinyl 351.525 54 — H —C(═O)NH 2 325.444 57 —NH— phenyl —C(═O)NH 2 416.556 59 —NH— cyclohexyl —C(═O)NH 2 422.604 60 —NH— Et —C(═O)NH 2 368.512 61 — phenyl Me 372.543 94 — 4-Cl-3-CF 3 -phenyl —OH 476.962 100 — phenyl —CN 383.5 101 — phenyl —OH 374.518 103 — phenyl —C(═O)Me 400.6 104 — 4-Cl-phenyl —OH 391 130 — 4-(4-CF 3 -phenyl)-phenyl —OH 519.4 131 — 4-(phenyl)-phenyl —OH 451.4 132 — 4-F-phenyl —OH 393.5
UTILITY
[0682] Aβ production has been implicated in the pathology of Alzheimer's Disease (Aβ). The compounds of the present invention have utility for the prevention and treatment of AD by inhibiting Aβ production. Methods of treatment target formation of Aβ production through the enzymes involved in the proteolytic processing of β-amyloid precursor protein. Compounds that inhibit β or γ secretase activity, either directly or indirectly, control the production of Aβ. Such inhibition of β or γ secretases reduces production of Aβ, and is expected to reduce or prevent the neurological disorders associated with Aβ protein, such as Alzheimer's Disease.
[0683] Cellular screening methods for inhibitors of Aβ production, testing methods for the in vivo suppression of Aβ production, and assays for the detection of secretase activity are known in the art and have been disclosed in numerous publications, including J.Med.Chem. 1999, 42, 3889-3898, PCT publication number WO 98/22493, EPO publication number 0652009, U.S. Pat. Nos. 5,703,129 and 5,593,846; all hereby incorporated by reference.
[0684] The compounds of the present invention have utility for the prevention and treatment of disorders involving Aβ production, such as cerebrovascular disorders.
[0685] Compounds of Formula (I) are expected to possess γ-secretase inhibitory activity. The γ-secretase inhibitory activity of the compounds of the present invention is demonstrated using assays for such activity, for Example, using the assay described below. Compounds of the present invention have been shown to inhibit the activity of γ-secretase, as determined by the Aβ immunoprecipitation assay.
[0686] Compounds provided by this invention should also be useful as standards and reagents in determining the ability of a potential pharmaceutical to inhibit Aβ production. These would be provided in commercial kits comprising a compound of this invention.
[0687] As used herein “μg” denotes microgram, “mg” denotes milligram, “g” denotes gram, “μL” denotes microliter, “mL” denotes milliliter, “L” denotes liter, “mM” denotes nanomolar, “μM” denotes micromolar, “mM” denotes millimolar, “M” denotes molar, “nm” denotes nanometer, “SDS” denotes sodium dodecyl sulfate, and “DMSO” denotes dimethyl sulfoxide, and “EDTA” denotes ethylenediaminetetraacetato.
[0688] A compound is considered to be active if it has an IC 50 or K i value of less than about 100 μM for the inhibition of Aβ production. Preferrably the IC 50 or K i value is less than about 10 μM; more preferrably the IC 50 or K i value is less than about 0.1 μM. The present invention has been shown to inhibit Aβ protein production with an IC 50 or K i value of less than 100 μM.
[0689] β Amyloid Precursor Protein Accumulation Assay (βAPPA Assay)
[0690] An assay to evaluate the accumulation of Aβ protein was developed to detect potential inhibitors of secretases. The assay uses the N 9 cell line, characterized for expression of exogenous APP by immunoblotting and immunoprecipitation.
[0691] The effect of test compounds on the accumulation of Aβ in the conditioned medium is tested by immunoprecipitation. N 9 cells are grown to confluency in 6-well plates and washed twice with 1×Hank's buffered salt solution. The cells are starved in methionine/cysteine deficient media for 30 min., followed by replacement with fresh deficient media containing 150 uCi Tran35S-LABEL™ (ICN). Test compounds dissolved in DMSO (final concentration 1%) are added, over a range of 1 picomolar to 100 micromolar, together with the addition of the fresh media containing Tran35S-LABEL™. The cells are incubated for 4 h at 37° C. in a tissue culture incubator.
[0692] At the end of the incubation period, the conditioned medium is harvested and pre-cleared by the addition of 5 μl normal mouse serum and 50 ul of protein A Sepharose (Pharmacia), mixed by end-over-end rotation for 30 minutes at 4° C., followed by a brief centrifugation in a microfuge. The supernatant is then harvested and transferred to fresh tubes containing 5 ug of a monoclonal antibody (examples of antibodies include but are not limited by, clone 1101.1, directed against an internal peptide sequence in Aβ; or 6E10 from Senetek; or 4G8 from Senetek; additionally polyclonals from rabbit antihuman Aβ from Boehringer Mannheim) and 50 ul protein A Sepharose. After incubation overnight at 4° C., the samples are washed three times with high salt washing buffer (50 mM Tris, pH 7.5, 500 mM NaCl, 5 mM EDTA, 0.5% Nonidet P-40), three times with low salt wash buffer (50 mM Tris, pH 7.5, 150 mM NaCl, 5 mM EDTA, 0.5% Nonidet P-40), and three times with 10 mM Tris, pH 7.5. The pellet after the last wash is resuspended in SDS sample buffer (Laemmli U. K. Cleavage of structural proteins during the assembly of the head of bacteriphage T4. Nature 227, 680-5, 1970.) and boiled for 3 minutes. The supernatant is then fractionated on either 10-20% Tris/Tricine SDS gels or on 16.5% Tris/Tricine SDS gels. The gels are dried and exposed to X-ray film or analyzed by phosphorimaging. The resulting image is analyzed for the presence of Aβ polypeptides. The steady-state level of Aβ in the presence of a test compound is compared to wells treated with DMSO (1%) alone. A typical test compound in this assay blocks Aβ accumulation in the conditioned medium, and is considered active with an IC 50 less than 100 μM.
[0693] C-Terminus β-Amyloid Precursor Protein Accumulation Assay (CTF Assay)
[0694] The effect of test compounds on the accumulation of C-terminal fragments is determined by immunoprecipitation of APP and fragments thereof from cell lysates. N 9 cells are metabolically labeled, as above, with media containing Tran35S-LABEL™, in the presence or absence of test compounds. At the end of the incubation period, the conditioned medium are harvested and cells lysed in RIPA buffer (10 mM Tris, pH 8.0 containing 1% Triton X-100, 1% deoxycholate, 0.1% SDS, 150 mM NaCl, 0.125% NaN 3 ). Again, lysates are precleared with 5 ul normal rabbit serum/50 ul protein A Sepharose, followed by the addition of BC-1 antiserum (15 μl;) and 50 μl protein A Sepharose for 16 hours at 4° C. The immunoprecipitates are washed as above, bound proteins eluted by boiling in SDS sample buffer and fractionated by Tris/Tricine SDS-PAGE. After exposure to X-ray film or phosphorimager, the resulting images are analyzed for the presence of C-terminal APP fragments. The steady-state level of C-terminal APP fragments is compared to wells treated with DMSO (1%) alone. A typical test compound in this assay stimulates C-terminal fragment accumulation in the cell lysates, and is considered active with an IC 50 less than 100 μM.
[0695] Accumulation-release Assay
[0696] This immunoprecipitation assay is specific for g secretase activity (i.e., proteolytic activity required to generate the C-terminal end of Aβ either by direct cleavage or generating a C-terminal extended species which is subsequently further proteolyzed). N 9 cells are pulse labeled with media containing Tran35S-LABEL™ in the presence of a reported g secretase inhibitor (MDL 28170; Higaki J, Quon D, Zhong Z, Cordell B. Inhibition of beta-amyloid formation identifies proteolytic precursors and subcellular site of catabolism. Neuron 14, 651-659, 1995) for 1 h, followed by washing to remove 35 S radiolabel and MDL 28170. The media is replaced and test compounds are added over a dose range (for example 0.1 nM to 100 μM). The cells are chased for increasing periods of times and Aβ is isolated from the conditioned medium and C-terminal fragments from cell lysates (see accumulation assay above). The activity of test compounds are characterized by whether a stabilization of C-terminal fragments is observed and whether Aβ is generated from these accumulated precursor. A typical test compound in this assay prevents the generation of Aβ out of accumulated C-terminal fragments and is considered active with an IC 50 less than 100 μM.
Dosage and Formulation
[0697] The compounds determined from the present invention can be administered orally using any pharmaceutically acceptable dosage form known in the art for such administration. The active ingredient can be supplied in solid dosage forms such as dry powders, granules, tablets or capsules, or in liquid dosage forms, such as syrups or aqueous suspensions. The active ingredient can be administered alone, but is generally administered with a pharmaceutical carrier. A valuable treatise with respect to pharmaceutical dosage forms is Remington's Pharmaceutical Sciences, Mack Publishing.
[0698] The compounds determined from the present invention can be administered in such oral dosage forms as tablets, capsules (each of which includes sustained release or timed release formulations), pills, powders, granules, elixirs, tinctures, suspensions, syrups, and emulsions. Likewise, they may also be administered in intravenous (bolus or infusion), intraperitoneal, subcutaneous, or intramuscular form, all using dosage forms well known to those of ordinary skill in the pharmaceutical arts. An effective but non-toxic amount of the compound desired can be employed to prevent or treat neurological disorders related to β-amyloid production or accumulation, such as Alzheimer's disease and Down's Syndrome.
[0699] The compounds of this invention can be administered by any means that produces contact of the active agent with the agent's site of action in the body of a host, such as a human or a mammal. They can be administered by any conventional means available for use in conjunction with pharmaceuticals, either as individual therapeutic agents or in a combination of therapeutic agents. They can be administered alone, but generally administered with a pharmaceutical carrier selected on the basis of the chosen route of administration and standard pharmaceutical practice.
[0700] The dosage regimen for the compounds determined from the present invention will, of course, vary depending upon known factors, such as the pharmacodynamic characteristics of the particular agent and its mode and route of administration; the species, age, sex, health, medical condition, and weight of the recipient; the nature and extent of the symptoms; the kind of concurrent treatment; the frequency of treatment; the route of administration, the renal and hepatic function of the patient,and the effect desired. An ordinarily skilled physician or veterinarian can readily determine and prescribe the effective amount of the drug required to prevent, counter, or arrest the progress of the condition.
[0701] Advantageously, compounds determined from the present invention may be administered in a single daily dose, or the total daily dosage may be administered in divided doses of two, three, or four times daily.
[0702] The compounds identified using the present invention can be administered in intranasal form via topical use of suitable intranasal vehicles, or via transdermal routes, using those forms of transdermal skin patches wall known to those of ordinary skill in that art. To be administered in the form of a transdermal delivery system, the dosage administration will, of course, be continuous rather than intermittent throughout the dosage regimen.
[0703] In the methods of the present invention, the compounds herein described in detail can form the active ingredient, and are typically administered in admixture with suitable pharmaceutical diluents, excipients, or carriers (collectively referred to herein as carrier materials) suitably selected with respect to the intended form of administration, that is, oral tablets, capsules, elixirs, syrups and the like, and consistent with conventional pharmaceutical practices.
[0704] For instance, for oral administration in the form of a tablet or capsule, the active drug component can be combined with an oral, non-toxic, pharmaceutically acceptable, inert carrier such as lactose, starch, sucrose, glucose, methyl callulose, magnesium stearate, dicalcium phosphate, calcium sulfate, mannitol, sorbitol and the like; for oral administration in liquid form, the oral drug components can be combined with any oral, non-toxic, pharmaceutically acceptable inert carrier such as ethanol, glycerol, water, and the like. Moreover, when desired or necessary, suitable binders, lubricants, disintegrating agents, and coloring agents can also be incorporated into the mixture. Suitable binders include starch, gelatin, natural sugars such as glucose or β-lactose, corn sweeteners, natural and synthetic gums such as acacia, tragacanth, or sodium alginate, carboxymethylcellulose, polyethylene glycol, waxes, and the like. Lubricants used in these dosage forms include sodium oleate, sodium stearate, magnesium stearate, sodium benzoate, sodium acetate, sodium chloride, and the like. Disintegrators include, without limitation, starch, methyl cellulose, agar, bentonite, xanthan gum, and the like.
[0705] The compounds determined from the present invention can also be administered in the form of liposome delivery systems, such as small unilamellar vesicles, large unilamallar vesicles, and multilamellar vesicles. Liposomes can be formed from a variety of phospholipids, such as cholesterol, stearylamine, or phosphatidylcholines.
[0706] Compounds of the present invention may also be coupled with soluble polymers as targetable drug carriers. Such polymers can include polyvinylpyrrolidone, pyran copolymer, polyhydroxypropylmethacrylamide-phenol, polyhydroxyethylaspartamidephenol, or polyethyleneoxide-polylysine substituted with palmitoyl residues. Furthermore, the compounds determined from the present invention may be coupled to a class of biodegradable polymers useful in achieving controlled release of a drug, for example, polylactic acid, polyglycolic acid, copolymers of polylactic and polyglycolic acid, polyepsilon caprolactone, polyhydroxy butyric acid, polyorthoesters, polyacetals, polydihydropyrans, polycyanoacylates, and crosslinked or amphipathic block copolymers of hydrogels.
[0707] Gelatin capsules may contain the active ingredient and powdered carriers, such as lactose, starch, cellulose derivatives, magnesium stearate, stearic acid, and the like. Similar diluents can be used to make compressed tablets. Both tablets and capsules can be manufactured as sustained release products to provide for continuous release of medication over a period of hours. Compressed tablets can be sugar coated or film coated to mask any unpleasant taste and protect the tablet from the atmosphere, or enteric coated for selective disintegration in the gastrointestinal tract.
[0708] Liquid dosage forms for oral administration can contain coloring and flavoring to increase patient acceptance. In general, water, a suitable oil, saline, aqueous dextrose (glucose), and related sugar solutions and glycols such as propylene glycol or polyethylene glycols are suitable carriers for parenteral solutions. Solutions for parenteral administration preferably contain a water soluble salt of the active ingredient, suitable stabilizing agents, and if necessary, buffer substances. Antioxidizing agents such as sodium bisulfite, sodium sulfite, or ascorbic acid, either alone or combined, are suitable stabilizing agents. Also used are citric acid and its salts and sodium EDTA. In addition, parenteral solutions can contain preservatives, such as benzalkonium chloride, methyl- or propyl-paraben, and chlorobutanol.
[0709] Suitable pharmaceutical carriers are described in Remington's Pharmaceutical Sciences, Mack Publishing Company, a standard reference text in this field.
[0710] Table 6 demonstrates representative substituents on the left end, or succinate end, of the compound of Formula (I), showing compounds envisaged within the scope of the present invention. Each of the fragments a through bt is attached to A, below.
TABLE 6 A | This invention relates to novel succinoylamino heterocycles having drug and bio-affecting properties, their pharmaceutical compositions and methods of use. These novel compounds inhibit the processing of amyloid precursor protein and, more specifically, inhibit the production of Aβ-peptide, thereby acting to prevent the formation of neurological deposits of amyloid protein. More particularly, the present invention relates to the treatment of neurological disorders related to β-amyloid production such as Alzheimer's disease and Down's Syndrome. | 2 |
BACKGROUND OF THE INVENTION
For instrument applications such as universal counters and oscilloscopes, a peak detector for repetitive waveforms is a valuable addition to the various input channels. It can provide a means for automatic triggering, signal amplitude measurement, and other waveform parameter measurements such as risetime. To be adequate for this application, the peak detector must exhibit good accuracy over a wide input dynamic range and over the instrument's entire operational frequency range. Furthermore, it must also exhibit good accuracy with any arbitrary input waveshape. Good accuracy in this case means the output detected voltage must be a DC level within a few millivolts of the input peak level.
Peak detectors in the prior art cover a variety of circuits with different operational characteristics. For example, there are detectors for amplitude modulation (AM), that is, envelope detectors, and detectors for detecting and holding the amplitude of a single pulse indefinitely. Input waveforms and the corresponding detected output waveforms for these prior art detectors are illustrated in FIGS. 1A and 1B.
The AM detector for the waveform in FIG. 1A is common and simple; it typically comprises only three elements: a diode for a unidirectional flow of current; a capacitor for storing the peak amplitude; and a resistor for discharging the capacitor. This circuit is shown in FIG. 1D. This type of detector is normally designed for use only with one carrier frequency where its output must decay fast enough to follow the lower modulating frequency to develop the modulating envelope. Further, the input waveshape for this type of detector is known and is usually a sinusoid of fixed frequency. Because of the diode in series with the input, there is always a difference of approximately 0.6 volt between the input and output voltages caused by the forward voltage drop of the diode. But, since only the envelope information is desired, the fact that at the peaks the input differs from the output by this forward voltage drop of the diode ([V F ] pk ) has no significance. This would not be the case if this type of detector is used for wideband applications. There, the presence of the forward voltage drop of the diode, the fast decay for the circuit to function properly at low frequencies, and the dependence on input waveshape would make this type of detector unsuitable for wideband applications.
The detector used for short pulses is generally designed to achieve an accurate peak output voltage reflecting the peak input voltage. Further, it is designed to hold the peak voltage for a relatively long time. A typical circuit of this type of detector is shown in FIG. 1C. This type of circuit generally has no inherent output decay to allow the output to follow a slowly decreasing input amplitude. This can be seen in the input and output waveforms in FIG. 1B. Although nominally wideband in nature, because it detects pulses, the upper frequency limit to these circuits is only a few megahertz. Therefore, this type of detector is also not suitable for wideband, repetitive waveform detection. It does, however, have the accuracy lacking in the detectors, because of the typical inclusion of the diode in the voltage follower feedback loop. One can take advantage of this fact and add an element, e.g., a resistor or a current sink, to slowly discharge the storage capacitor to provide the desirable output decay. To extend the circuit to high frequency performance beyond a few megahertz, however, requires a high gain feedback amplifier with extreme bandwidth and stability beyond the input frequency range. This is extremely difficult and costly to achieve.
SUMMARY OF THE INVENTION
That the output differs from the input by one forward diode voltage drop at peak amplitude is a fundamental disadvantage of the AM detector for accurate wideband application. That is,
V.sub.OUT =[V.sub.IN -V.sub.F ].sub.pk
If the forward drop is precisely know, then by adding it to V OUT , one can obtain the peak value of V IN , or [V IN ] pk . To find the peak value for the diode forward voltage [V F ] pk , however, is not trivial. It varies with the peak diode current, which, in turn, depends on the input waveshape. For instance, low duty cycle pulses and triangle waveforms result in a high forward voltage V F due to the peak occurring for a brief portion of the input period. In contrast, square waves result in low forward voltage V F , because half of the input is at the peak voltage level. However, the peak detector according to the present invention generates two DC voltages that differ by [V F ] pk ; it then takes the difference between these voltages and recombines them with an operational amplifier to arrive at an accurate peak voltage output independent of the diode forward drop. In the preferred embodiment, two diode detector circuits are used to provide the two DC voltages. By making the diodes substantially identical in the two circuits, the peak DC levels derived from each of the two circuits can be made to have a related dependence on the diode forward voltage parameter. The two DC levels, then, can cancel out the related diode forward voltage parameter to provide the accurate peak voltage output required.
DESCRIPTION OF THE DRAWINGS
FIG. 1A shows the relationship between the input and output waveforms to the amplitude modulation (AM) detector in the prior art.
FIG. 1B shows the relationship between the input and output waveforms to a detector circuit having an infinite hold capacity in the prior art.
FIG. 1C shows a circuit for the detector having the input-output relationship of FIG. 1B.
FIG. 1D shows a circuit for the detector having the input-output relationship of FIG. 1A.
FIG. 2 shows a circuit having two peak detectors to provide two DC levels in accordance with the present invention.
FIG. 3 shows the preferred embodiment of the peak detector in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The technique in accordance with the present invention measures the forward voltage drop of the diode (V F ) at the peak and uses it to calculate the correct peak voltage as the output. Two AM-type detectors 2 and 4 are employed, one 2 being of the conventional three-element design comprising one diode 14 in series with a capacitor 16 and a resistor 18 in parallel and the other 4 having two diodes 6 and 8 instead of one in series with a capacitor 20 and a resistor 22 in parallel, the capacitors 16, 20 and resistors 18, 22 both being tied to some voltage level, ground and -V respectively in the present example. As shown in FIG. 2, both detector inputs 10 and 12 are connected together to an input port 15 where an input waveform is applied. If the values of the capacitors 16 and 20 and resistors 18 and 22 are large enough, a slow decay rate results. The outputs 24 and 26 to the circuit in FIG. 2 then are:
V.sub.OUT1 =[V.sub.IN ].sub.pk -[V.sub.FD1 ].sub.pk -[V.sub.FD2 ].sub.pk, and
V.sub.OUT2 =[V.sub.IN ].sub.pk -[V.sub.FD3 ].sub.pk,
where the brackets [ ] pk indicate the peak value of the enclosed quantity, that is, [V FD1 ] pk , [V FD2 ] pk , and [V FD3 ] pk are the peak forward voltages of diodes 6, 8, and 14, respectively, and [V IN ] pk is the peak input amplitude. With these two outputs 24 and 26 being essentially DC levels, their difference is -[V FD1 ] pk -[V FD2 ] pk +[V FD3 ] pk . Using diodes with matched forward voltages, this difference becomes [V FD3 ] pk . Now, if this difference is added to V OUT2 , the value for [V IN ] pk results. This can be accomplished with the preferred embodiment shown in FIG. 3. For accuracy and simplicity, a single operational amplifier 30 is used to achieve this result. An operational amplifier 32 operates as a voltage follower (unity gain) to buffer current through a resistor 34 to amplifier 30 away from resistor 22. Amplifier 30, in addition to subtracting output 26 from output 24, also buffers the output current and the currents through output resistors 34 and 36 away from resistor 18. It also provides a gain of two to its input 26, thus providing essentially a multiple of two of its input 26 less the diode forward drop. If resistors 34 and 36 are made equal, it performs the arithmetic operation of V OUT =2V OUT2 -V OUT1 . Hence, from the circuit of FIG. 3, it follows that ##EQU1##
Since only the diodes 6, 8, and 14 experience the input frequency range, the frequency response of the peak detector is limited predominantly by diode switching performance, which incidentally is very good for Schottky diodes. This technique may be implemented with discrete components, or with components integrated on a chip. Matched components are necessary for good accuracy. Capacitors 16 and 20 are made to match so that the computed value for [V F ] pk is accurate. Input loading is small; it is the diode capacitances in parallel with the low value capacitor that discharge currents into resistors 34 and 36. The output voltage at the output port 38 may require a number of input cycles to reach full peak value, but this is of little consequence for repetitive input waveforms. Furthermore, power required of the input signal at input port 15 can be negligibly small since it is only that drawn by the two discharge resistors 18 and 22.
By making the discharge resistors 18 and 22 different values, two further benefits result. Owing to the action of the subtracting operational amplifier 30, the output decay rate equals
2d(V.sub.OUT2)/dt-d(V.sub.OUT1)/dt.
Hence, the output decay can be made slower than the capacitive decays. This means a smaller capacitor value may be used to arrive at a suitable output decay. This results in a desirable initial slow drop which extends operation to low frequencies, and then a fast decay a short time later, thus allowing the detector to adapt quickly to a new lower peak amplitude input signal. | A peak detector is comprised of two related circuits having similar circuit parameters, each providing an output in response to a repetitive waveform applied to the detector. The two outputs are combined to eliminate the dependence on the circuit parameters to provide as an output of the detector an accurate, wideband peak voltage of the applied waveform. | 6 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This is a continuation of application Ser. No. 07/832,350 filed Feb. 7, 1992 now issued as U.S. Pat. No. 5,183,081.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to a shed format ion device for use in weaving. More particularly, the present invention relates to a shed formation device which is particularly useful in weaving narrow strips of fabric. Most particularly, the present invention relates to a shed forming device which is useful in an automatic seaming apparatus which is used to join the fabric ends to render the fabric endless.
2. Description of Prior Art
It is known to join woven fabrics in order to render them endless. Likewise, it is known to join the ends of a woven fabric through a process of reweaving. In the known processes, the ends of the fabric to be joined are processed so as to produce a yarn fringe which is comprised of yarns from the fabric body. The fringe yarns from each end are then interwoven, generally in the same repeat pattern as the remainder of the fabric, with a system of yarns selected in accordance with the original yarns that were interwoven with the fringe. Through this reweaving process, the resulting fabric is endless and has the same general construction throughout its length.
In the prior art, it is been known to join the fabrics through manual procedures , semiautomatic procedures and automatic procedures. In connection with forming the weaving shed, standard loom harnesses, dobby movements and a Jacquard movement have been utilized to form the shed. Although the semiautomatic and automatic devices of the prior art have produced some improvement over the manual procedure, the prior art devices exhibit three principal flaws . One, the shed formation devices do not easily accommodate changes in the weave pattern. Two, the join speed of the prior art devices is limited by the speed of the shed formation. Three, the need for mechanical interconnection, generally, means that the shed formation control device and the actual shed formation apparatus must be positioned close to each other.
It is the object of the present invention to provide a shed formation apparatus that can easily accommodate a change of weave patterns and can achieve shed formation speeds not available with the prior art devices.
SUMMARY OF THE INVENTION
The present invention provides a shed formation apparatus having increased flexibility and speed. The shed formation apparatus is comprised of a plurality of movable heddles which are connected to a plurality of moveable heddle selectors by a first plurality of control leads. Heddle selector controllers, which include stopper means to retard the movement of the heddle selectors, are connected to the selector. A second plurality of control leads are attached to the heddle selectors opposite the first plurality. Repeat pattern output means determines the movement of the control leads and the attached heddle selectors, and selectively activates the stopper means.
In order to provide sufficient space for the controllers, the control leads may be passed through a first harness means to increase the spacing therebetween and then passed through a second harness means to reduce the spacing therebetween.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a shed formation apparatus in accordance with the present invention retrofitted to a known automatic seaming apparatus.
FIG. 2 is a fragmentary section of a typical plate which illustrates a yarn guide in accordance with the present invention.
FIG. 3 illustrates a yarn heddle in accordance with the present invention.
FIG. 4 illustrates, in section, the assembly of a controller, including the guide, a heddle selector and a stopper mechanism, in accordance with the present invention.
FIG. 5 illustrates a heddle selector in accordance with the present invention.
FIG. 6 illustrates a section of the guide in accordance with the present invention.
FIG. 7 illustrates one arrangement for a plurality of controllers in accordance with the present invention.
FIG. 8 illustrates a shed formation plate in accordance with the invention.
FIG. 9 illustrates a shed formation plate and varied lead positions in accordance with the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The preferred embodiment will be described with reference to the drawing figures.
With reference with FIG. 1, the shed formation apparatus 10 will be described in more detail. It will be recognized by those skilled in the art that the apparatus 10 in FIG. 1 is shown without any means of securement. It is shown in this manner for the purpose of illustration and it is expected that the fixed elements of the apparatus will be secured in accordance with the configuration of the weaving device into which it is incorporated. The weaving apparatus shown in FIG. 1 is described in U.S. Pat. No. 5,027,483 which is commonly assigned and incorporated herein as if fully set forth.
For the purpose of a general understanding of the process, the process is briefly described. The ends of the fabric are presented on either side of auxiliary yarns 12 with the prepared fringe 14 comprised of a plurality of yarns which are retained in their relative positions by the ribbon 16. As a result of manipulation of the ribbon 16, individual fringe yarns 14 are released and presented to a transfer arm 18. The transfer arm 18 will position the yarn 14 below the surface of the fabric. As a result of the shedding apparatus, the yarns 12 will be manipulated to form a shed in accordance with the fabric repeat pattern. Since the weaving takes place beneath the plane of the yarns, the shed is formed downwardly. The interlacing arm 20 will accept the yarn 14 from the transfer arm 18 and will interweave it with the yarns 18. After the transfer arm 12 has traversed the shed and is against the fell of the cloth, an extractor arm 22 will grip the yarn and pull it against the fell and through to one side of the fabric so that it may be ultimately trimmed. In the complete operation, a beat up mechanism is provided, however, it is not shown here for the sake of clarity. As this process continues, the joint area 24 will be completed and the resultant endless fabric will have a common weave structure throughout.
Still with reference to FIG. 1, the shed formation apparatus 10 will be further described. Apparatus 10 has a plurality of fixed plates 30, 32 , 34 , 36 and 38 and a moveable shed formation plate 40. All of the fixed plates are at fixed distances from each other. As noted previously, the specific arrangement for fixing the plates relative to each other will depend on the weaving apparatus. In some instances, it is expected that the illustrated arrangement will be inverted. In order to facilitate an understanding of the invention, it will be beneficial to discuss the purpose of the plates prior to discussing operation of the shedding apparatus.
Plates 30 and 32 are set at a fixed distance from each other and are positioned so that the heddles 42 will depend from the fixed plate 30 with the mail 48 positioned in plane of the yarns 12. In the preferred embodiment, each of the heddles 42 is of the type commonly associated with a Jacquard mechanism. The heddles 42 will be described in more detail with respect to FIG. 3. In general, the end 44 of the heddle is spring loaded and secured to the underside of plate 30 by a first lead 46. Each second lead 50 passes through one of the apertures 52 in plate 32. Each lead 50 continues through a respective aperture 54 in plate 34. As can be seen from the illustration, the plate 34 has a substantially larger area than the plate 32 and the apertures 54 are spaced further apart than the apertures 52 and plate 32. As a result, the leads 50 are defused over a larger area as they pass through plate 34.
Still with reference to FIG. 1, the plates 34 and 36 are at a fixed distance with respect to each other. At present, it is preferred that the plates 34 and 36 be equal in area with the respective apertures 54 and 56 on centerline with each other. The second lead 50 terminates at one end of the selector 80, and a third lead 84 is attached to the other end of the selector 80, see FIGS. 4 and 5. Each third lead 84 passes through its respective aperture 56, through the respective aperture 58 in plate 38 and is terminated at shed formation plate 40. As can been seen from FIG. 1, plate 38 has an area which is substantially equal to that of plate 32. The spacing of the apertures 58 corresponds generally to the spacing of apertures 52. Since the plate 38 has a smaller area than the plate 36, the leads 84 will be concentrated as they pass through the apertures 58. Accordingly, plate 34 will cause a diffusion of the second leads 50 and plate 38 will cause a concentration of third leads 84.
Before turning to a detailed description of additional elements of the invention, it is believed that a description of shed formation with this apparatus will benefit an understanding of the invention. Still with reference to FIG. 1, the movable plate 40 is moved in response to the repeat pattern which is required by the weave. Since the interweaving arms of the present weaving apparatus are generally below the plane of the fabric being joined, the shed will be formed beneath the plane of the yarns 12. As is known to those skilled in the art, each yarn 12 will be threaded through the respective mail 48 of a given heddle. Movement of the heddle will position the yarns 12 in the proper shed position.
If we assume an initial position with all of the auxiliary yarns 12 in a common plane, all of the mails 48 will also be in a common plane. In order to form a shed, the moveable shed formation plate 40 will move downwardly. As a result of this movement, the third lead 84 will move downwardly and cause a resultant downward movement of the mails 48 and extension of the spring 44. After plate 40 has completed its movement, selected controllers 60 will be activated. The selected controllers will be determined in accordance with the weave pattern as will be explained hereinafter. As soon as the selected controllers 60 have been activated, the moveable plate 40 will be permitted to return to its initial position. As a result of this movement, each yarn which is not associated with an activated controller will return to the original plane of the auxiliary yarns by the contraction of spring 44. Those yarns which have been selected will remain in a down position. After interweaving of the selected yarn has been completed, the moveable plate 40 will be activated and the selection process will be repeated. In the event that the repeat pattern does not require any change in the position of a previously selected yarn, no further activity will take place with respect to that yarn. In the event that a previously non-selected yarn is now a selected yarn, the weave pattern information will cause actuation of the associated controller 60. Accordingly, the moveable plate 40 will act upon each of the third leads 84 at each and every shedding, however, the controllers 60 will only be activated as needed. The information regarding the weave pattern must include a repeat pattern output means for selectively activating the controllers 60. However, the specific weave pattern output means is not critical to the invention. Those familiar with Jacquard movements will recognize that such a shed formation apparatus may be controlled by punch cards, tape or a computerized information source. Any of these weave patterns information output means will work with the present invention so long as the weave pattern information is presented in a form which will cause switching of the controllers 60. If one considers a standard Jacquard device, the yarn control information would not pass directly to the heddle, instead, the selected heddle information would be passed directly to a switching mechanism which will activate the selected controllers 60. The moveable plate 40 will be activated on each shedding pass and does not require specific control other than sequential timing in coordination with the selector operation.
With reference to FIG. 2, there is shown a typical aperture through one of the plates 30 through 40. It is expected that each of the plates will be formed of steel or some other metal. Since all of the leads will be subject to abrasion, it is preferred that each of the apertures be provided with a ceramic eyelet 41. Such eyelets are well known in the art and are frequently used as thread guides.
With respect to FIG. 3 , there is shown a typical heddle 42. Heddle 42 is very similar to those which are generally associated with Jacquard movements, however, in the presently preferred embodiment, the second lead 50 is longer than that normally associated with the Jacquard heddle. Typically, such a heddle has a sleeve encased spring 44 at one end thereof. Generally, the spring terminates at one end in a mounting loop 45 and at the other end in a first lead 46. The loop 45 is dimensioned so as to abut the sleeve 43 and permit elongation of the spring 44 as a result of movement of the first lead 46. The first lead 46 is attached to one end of the mail 48. The second lead 50 is attached to the other end of the mail 48. As is common in the art, mail 48 includes an aperture 49 through which the yarn is threaded.
With respect to FIG. 4, there is illustrated a controller 60 in accordance with the presently preferred embodiment. The controller 60 is comprised of a guide 62 which is further comprised of guide halves 64 and 66. At least one guide half, includes an aperture 76 which extends into the slot 78. In the present embodiment, the aperture 76 is illustrated in the guide half 66. The controller also includes a stopper mechanism 68. Stopper mechanism 68 is comprised of a solenoid 70 which activates the plunger 72. Plunger 72 includes a projection 74 which is dimensioned to pass through the aperture 76 and to impede the movement of the selector 80 within the slot 78 in guide 62. In the presently preferred embodiment, the projection 74 dimensioned to engage an aperture 82 in the selector 80. This provides a positive mechanical stop against further movement of the selector 80. Alternatively, the plunger 72 could merely move into an interfering contact to halt movement of the selector 80. Actuation of the solenoid 70 is accomplished through the electorial lead 71. As noted previously, the passage of electorial current to the lead 71 will be made in accordance with the weave pattern selection process. When it is determined by the weave pattern that a particular heddle should remain in the down position, the solenoid will be activated and the projection 74 will impede movement of the selector 80. As a result, the associated heddle will remain at a down position.
With reference to FIG. 5, the selector 80 will be described in more detail . The selector 80 will have a configuration very similar to that associated with the heddle 42. However, the selector 80 will have sufficient length so that it will move within the guide 62 without causing abrasion or other alignment problems. Since one end of the selector 80 is connected to the primary lead 50, it will be appreciated that the lengths of the primary lead 50 and the selector 80 must be selected in accordance with the movement necessary to produce the shed opening. In the preferred embodiment, the selector 80 includes an aperture 82 which is dimensioned to receive projection 74. The third lead 84 is affixed to the other end of the selector 82 and is routed as discussed previously.
With respect to FIG. 6, guide half 66 is shown in more detail. From FIG. 6, it can be seen that the aperture 76 is positioned in one wall of the guide. The dimensions of slot 78 will be determined by selector 82 . At present, it is preferred that guide halves 64 and 66 be used to fully encase the selector 80 . However, it is contemplated that the selector 80 could be captured within a single slot as indicated by the phantom lines in FIG. 6.
With reference to FIG. 7 , there is illustrated a plurality of controller 70 as they may be positioned on the plate 36. The specific arrangement of the controller 60 is not critical to the present invention. It is intended by FIG. 7 to illustrate the flexibility in special arrangements. In the presently preferred embodiment each controller 60 includes a miniature solenoid which is available from Autotronics, Inc. of Joplin, Miss. Each controller 60, including the guide 62 and the stopper mechanism 68, requires approximately 121 square millimeters on plate 36.
In FIGS. 1, 4 and 7, the controllers have not been depicted as affixed to the plate 36 and the controller has not been shown with the stopper mechanism 68 affixed to the guide 62. Since it is believed such attachments are well within the skill of the art, the specific means of attachment do not require description herein. However, it must be recognized that attachment of the controller 60 to the plate 36 must permit movement of the third lead 84 and the selector 80. For example, each controller 60 may be secured to a generally "L" shaped mount of the type which shown in phantom at 63 on FIG. 4. The mount is removably secured to the guide 62 to permit quick interchange of the elements when necessary.
With reference to FIGS. 8 and 9, the shed formation plate 40 will be described in more detail. Plate 40 is secured to the roller 100 which is mounted for rotation at its ends in the mounts 102. The mounts 102 may be affixed to the floor, a cross member or some other portion of the weaving apparatus to fix them against movement. The free end of plate 40 is secured to a solenoid 104. Solenoid 104 will move through an arc, as indicated by the arrows in FIG. 8, which will generally translate into vertical movement of the secondary leads 84. In view of the fact that the roller 100 must rotate, it will be understood by those skilled in the art that either the attachment of plunger 106 to plate 40 or the attachment of solenoid 104 to the base 110 must be a moving attachment to accommodate the arcuate movement of plate 40. As noted previously, the solenoid 104 will be activated on each pass of the shed formation apparatus. The actuation of the solenoid 104 is accomplished through the cad 108. As will be recognized by those skilled in the art, mechanical, pneumatic, hydraulic or other electrical--electronic means may be used in place of the solenoids described herein.
With reference to FIG. 9, there is shown a side view of the plate 40 which illustrates the position of representative third leads 84 during a weaving operation. In the preferred embodiment, each third lead 84 passes through an aperture 86. The end of the lead 84 is terminated and a small weight 88 is affixed thereto. Thus, the weight 88 also serves as the termination of the lead 84. The principle purpose of the weight 88 is to retain the lead 84 in a generally vertical condition. As noted previously, a selected heddle will not return to the original plane of the yarns 12. Since the projection 74 retards movement of the heddle selector 80, the lead 84 is unloaded. In order to avoid entanglement and to retain the generally vertical position of the lead 84, the weight 88 is attached. As will be understood by those skilled in the art, the weight 88 does not need to be substantial, however, the attachment to lead 84 must be secure in order to maintain control during movement of the plate 40. Still with reference to FIG. 9, it will be understood by those skilled in the art that the plate 40 will traverse an arcuate path and the stroke length of the plunger 106 must be considered in positioning the selector 80 with respect to the respective stopper mechanism 68.
At present, it is preferred to use electrically operated solenoids in connection with the present invention. Since each solenoid does not have to be activated on each pass, the electrical load of the present invention is greatly reduced. In addition, electrical switching devices which are controlled by punch cards or computer information are relatively common. Accordingly, the use of solenoids eliminates the need for conversion of data from an electrical format to some other format.
It will be understood by those skilled in the art that variations in the preferred embodiment will still come within the scope of the claimed invention. | A shed formation apparatus having increased flexibility and speed. The shed formation apparatus is comprised of a plurality of movable heddles which are connected to a plurality of heddle selectors by a first plurality of control leads. The heddle selectors are movably connected to a plurality of heddle selector controllers which include stoppers to retard the movement of the heddle selectors. A second plurality of control leads are attached to the heddle selectors. A repeat pattern output apparatus determines the movement of the second plurality of control leads and the attached heddle selectors, and selectively activates the stoppers. | 3 |
This application is a continuation of application Ser. No. 003,582, filed Jan. 15, 1987, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to radiation detectors and, more specifically, to such detectors which are based on semiconductor principles.
2. Prior Art
Semiconductor-based radiation detectors generally have a single-crystal substrate with a p-n junction or a Schottky junction with an inverse bias applied to the depletion layer which occurs at the junction. When radiation strikes the depletion layer such radiation is detected by detecting the increase in electron-hole pairs which occurs in the region where the radiation is incident. This technique is effective in detecting radiation of the α, β, γ, and/or x-ray types.
When it comes to detecting neutrons, which by definition have no charge, there is no electrostatic influence on the Coulomb fields of the orbital electrons and atomic nuclei so the electron-hole pairs relied upon in the conventional semiconductor-based radiation detector do not appear as a result of incident neutron bombardment. Thus, the conventional semiconductor-based radiation detector cannot be used to detect neutrons. With this problem in mind, neutron detection has been approached from the standpoint of detecting charged particles produced by the reaction between the incident neutrons and the atomic nuclei. Such reaction produces free protons as a result of elastic scattering and nuclear fission. A prior art neutron detector based on this principle is shown in FIG. 1. In FIG. 1, a single-crystal silicon substrate detector-element 10 is housed in a sealing vessel 12 comprising a vessel body 14 and a cover 16, the purpose of which is to produce an hermetic seal of the vessel. Lead wire 18 is led out from one surface of semiconductor-based detector element 10 and through hermetic packing element 20. In the embodiment of FIG. 1, showing the prior art, the remaining lead wire 22 is grounded to the vessel body 14 which is metallic and, therefore, electrically conductive in character. The lead wire 18 is coupled to an indicating device, not shown, for indicating the presence and level of neutron incidence. A pipe 24 is hermetically sealed in cover 16. In operation, 3 He is introduced into vessel 12 by way of pipe 24 from a source of such gas, not shown. This type of semiconductor-based neutron detector relies upon the reaction and the elastic scattering which result with respect to 3 He and the incident neutrons, according to the following equation
.sup.3 He+n→.sup.3 He+P+765 KeV (1)
where P is protons. It can be seen from that equation that the incidence of neutrons on the 3 He produces 3 He+protons and a nuclear energy of 765 KeV. More specifically equation (1) shows that the incidence of neutrons on a 3 He produces 3 He and the following components: (1) reaction-generated nuclear energy to which an electron kinetic energy of 765 KeV is ascribed when the neutrons are reactive, (2) the reaction generated nuclear energy caused by the thermoneutron background, and, (3) protons produced by the elastic scattering caused by the incidence of neutrons upon 3 He.
In the detector of FIG. 1, however, charged particles generated in the 3 He gas must pass through the gas in order to reach the detecting element and, hence, the detection efficiency is decreased. The resolving power of the detector and and its associated indicating equipment is consequently limited. Further, the vessel 12 must be very strong because the 3 He gas is introduced into the vessel at a pressure of 1 to 5 atmospheres. Further, the detector of FIG. 1 requires various ancillary equipment, such as pipes for introducing the 3 He gas into vessel 12. It is also necessary to have a gas flow rate regulator. Thus the equipment of FIG. 1 is not portable nor is it easy to utilize other than in a laboratory.
Therefore, it is a primary object of the present invention to provide a compact, lightweight semiconductor-based radiation detector which is highly portable and still also highly effective in detecting neutrons.
SUMMARY OF THE INVENTION
There is provided by this invention a semiconductor-based radiation detector (more specifically a neutron detector) in which 3 He is diffused into the semiconductor substrate, in advance, by a plasma doping method with the resulting semiconductor substrate producing electron-hole pairs upon the incidence of neutrons on the surface of the semiconductor substrate. The p-n junction of a single-crystal semiconductor substrate (basically a p-n junction diode structure) having an inverse bias applied to the junction to expand the depletion layer results in a semiconductor-based radiation detector that is capable of detecting neutrons relying upon the 3 He (n, p) reaction.
BRIEF DESCRIPTION OF THE DRAWINGS
This invention can best be understood by reviewing the description which follows in conjunction with the drawings herein, in which:
FIG. 1 is a mechanical schematic diagram, partially in cross-section showing a semiconductor-based radiation detector, according to the prior art;
FIG. 2 is a schematic diagram of apparatus for diffusing 3 He gas into a single-crystal silicon substrate;
FIG. 3 is a graphical representation of the results produced by the apparatus of FIG. 2;
FIG. 4 is a schematic mechanical diagram, partially in section, of a Schottky-junction, semiconductor-based radiation detector element incorporating the present invention in its elemental form;
FIG. 5 shows an additional embodiment of the structure of FIG. 4, according to the present invention;
FIG. 6 shows an additional embodiment of the structure of FIG. 4, incorporating the present invention;
FIG. 7 is a schematic mechanical diagram, partially sectioned, showing an additional embodiment of the present invention; and,
FIG. 8 is a schematic mechanical diagram, partially in section, of an additional embodiment of the structure of FIG. 7 utilizing the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 has been discussed in connection with the prior art and needs not to be discussed further herein.
As has been indicated in the Summary of the Invention, the radiation detecting element contemplated by this invention includes a single-crystal silicon substrate which has at least one layer of diffused 3 He. To effect the diffusion of the 3 He into the single-crystal silicon substrate, apparatus of the type shown in FIG. 2 may be used. This apparatus is more or less conventional plasma diffusion apparatus. In FIG. 2, reaction chamber 26, which is hermetically sealed, carries in its walls an upper electrode plate 28 and a lower electrode plate 30 which are opposed to each other. Appropriate potentials are applied to electrodes 28 and 30 from voltage source 32 by way of connectors 34 and 36 which pass through the walls of chamber 26 in a fashion so as to keep the hermetic sealing of chamber 26 intact. Electrodes 28 and 30 are supported from the walls of chamber 26. The internal pressure in chamber 26 is reduced by means of vacuum pump 38 which is coupled into chamber 26 by way of pipe 40, the passage of pipe 40 through the walls of chamber 26 being sealed, hermetically, to maintain the integrity of the chamber. The reduction in pressure within chamber 26 is measured by means of vacuum gage 42 which is intercoupled with the inner portion of chamber 26 by means of pipe 44, again hermetically sealed in the walls of chamber 26. A lower electrode 30 is heated by heater element 46 which is connected to a source of electricity, not shown. Tank or bottle 48 contains 3 He gas which is coupled into reaction chamber 26 by way of pipes 50 and 54 and regulator 52.
A P-type single-crystal substrate 56, having a specific resistance of, for example, 10KΩ cm or more is placed on lower electrode 30 and is heated to a temperature of, for example, 200 degrees C by means of heater 46. At the same time, 3 He gas is introduced from tank or bottle 48 into chamber 26 so that the pressure within reaction chamber 26, which had been previously reduced by exhaust system 38, arrives at, for instance, 4 Torr. A voltage, for example 550 volts DC, is applied between upper electrode plate 28 and lower electrode plate 30 from direct current source 32, thereby generating a plasma between the electrode plates 28 and 30. As a consequence, a significant amount of 3 He is diffused into the surface of the single-crystal substrate 56 which rests on lower electrode 30. Such a low-temperature plasma doping method is fully disclosed in the Specification of Japanese patent laid-open publication Nos. 218727, 218728/1984 in which the inventors are the same as the inventors of this invention.
Turning to FIG. 3 there are shown the results which are obtained by the diffusion apparatus of FIG. 2. The data in FIG. 3 were obtained with the aid of a secondary ion mass analyzer (SIMS). The abscissa of the graph of FIG. 3 indicates the depth of diffusion into substrate 56 by the 3 He atoms. The ordinate axis shows the concentration of 3 He within substrate 56. It is clear from the curve of FIG. 3 that 3 He of 1×10 atom/cm 3 diffuses into the surface of single-crystal silicon substrate 56 and that 3 He atoms continue to diffuse into the body of substrate 56. Thus 3 He may be said to be interstitially disposed in substrate 56. It is this diffusion of 3 He into the substrate 56 that is relied upon to make the semiconductor-based radiation detector which is the subject of this invention. Specific embodiments of the semiconductor-based detector are shown in FIGS. 4 thru 8.
In FIG. 4, substrate 60 has a 3 He-diffused region 62 adjacent to one of its surfaces. A metallic electrode 64 is deposited on the diffused region of substrate 60. An ohmic-contact electrode 66 is deposited on the opposite surface of substrate 60. When an inverse bias is applied between electrodes 64 and 66 a depletion layer forms in the region of the interface between electrode 64 and substrate 60. Any neutrons in radiant energy falling on the depletion layer react with the 3 He of the diffused region 62 and produce the reaction set forth in equation (1). Tritons ( 3 H) and protons which are derived from the reaction cause electron-hole pairs to be produced in the depletion layer and these pairs are detected as pulses corresponding to incident neutrons. The embodiment of FIG. 4 is the simplest approach to the semiconductor-based radiation detector which is the subject of this invention.
In FIG. 5, substrate 60 has 3 He-diffused regions on both the upper and lower faces of substrate 60. These are regions 68 and 70. The technique for forming these diffused regions utilizes the apparatus of FIG. 2. Electrodes 64 and 66 are then applied to the opposite surfaces of substrate 60, as before, only in this case there are diffused regions on both sides of substrate 60. The use of the two diffused regions, one on each side including the side carrying the ohmic contact, permits the enhanced operation of this detector because additional tritons and protons can be generated with the larger diffused surface area.
In FIG. 6 substrate 60 has a p + layer 72 in contact with ohmic contact 66. The p + region is produced by doping region 72 heavily with boron, utilizing the plasma doping equipment of FIG. 2. In FIG. 6 the lower 3 He-diffused region 70 of FIG. 5 does not exist. The purpose of the structure of FIG. 6 is to get a very good ohmic contact with substrate 60 from ohmic contact 66. The other elements of FIG. 6 are the same as those shown in FIGS. 4 and 5.
In FIG. 7 substrate 60 has an amorphous silicon layer 74 formed thereon by means of the plasma CVD method utilizing monosilane gas. This amorphous silicon layer is laminated on top of 3 He-diffused region 62. The substrate 60 is of the P-type having a specific resistance of more than 10KΩ cm, thereby forming a hetero-junction between the single-crystal silicon substrate 60 and the amorphous silicon layer 74. After the formation of the amorphous silicon region on the diffused region 62, ohmic electrodes 76 and 78 are applied to the combination. This may be achieved by the vacuum vapor-deposition method, an electron beam method or a sputtering method.
The requirements for achieving the plasma CVD deposition of the amorphous silicon layer 74 on the substrate 60 are as follows:
Gas for use: Hydrogen with 10% monosilane (SiH 4 )
Pressure: 10 Torr
Applied voltage: DC 800 volts
Temperature of lower electrode plate: 200 degrees C.
Under these conditions an amorphous silicon layer 74 is formed having a thickness of approximately 1 μm.
In FIG. 8, radiation detecting element 80 has a p + region 72 formed therein by doping the region with boron so as to assure a better ohmic contact to terminal 76. It is to be noted that, as in FIG. 6, there is no 3 He-diffused region between substrate 60 and contact or terminal 76. There is a 3 He-diffused region 62 formed on the opposite side of substrate 60 from p + region 72. That region 62 and the amorphous silicon layer 82, as well as ohmic contact or terminal 84, may be formed by the techniques and in the manner set forth in connection with the structure of FIG. 7. The detecting element of FIG. 8 exhibits a lower noise level than the structure of FIG. 7 and the temperature characteristics of the structure of FIG. 8 are superior to those of the structure of FIG. 7.
It is essential in connection with the doping of substrate 60, in all cases, that the plasma method described hereinbefore be used because it requires raising the temperature of the substrate minimally. If conventional techniques (which are applied in the manufacture of integrated circuits) are applied here, there may be a destruction of the single-crystal structure which is so essential to the proper performance of the radiation detector described herein. With the low temperature plasma diffusion technique described herein the temperature of the single-crystal substrate need not be raised beyond 200 degrees C. At such temperatures there is no degradation of the single-crystal nature of substrate 60.
It should be understood that while reference has been made repeatedly to single-crystal silicon as the substrate 60, the present invention is not confined to silicon but may involve crystal or compound semiconductors such as cadmium telluride and gallium arsenide. In the formation of the 3 He-diffused region an ion implanting method may be used instead of the previously described plasma CVD method, with identical results being obtained. This latter method has the disadvantages of being expensive and time consuming.
The essence of the structure comprising the invention disclosed herein is the resident nature of the 3 He gas in the semiconductor substrate and the method of getting it there. As a result of the resident nature of the 3 He gas, external sources of gas are not required during the operation of the detector. Previous neutron detectors have required complex and heavy external equipment to support the operation of the detecting element itself. The detecting element according to this invention is stable and sensitive over a long period of time. Since the 3 He-diffused region has a gas concentration of 10 21 atoms/cm 3 , on the average, the level of sensitivity of the detector is very high, which is important when it is being used as a neutron detector for protection of the human body. Experience indicates a lifespan of more than 10 years can be realized for the device according to the present invention.
While particular embodiments of the present invention have been shown and described, it will be apparent to those ordinarily skilled in the art that variations and modifications may be made therein without departing from the true spirit and scope of the invention. | A semiconductor-based radiation-detector element particularly adapted to neutron detection, and the method for making the same, in which a high sensitivity single-crystal semiconductor substrate has diffused therein at-least-one region of 3 He gas, which remains resident therein, whereby, upon application of an inverse bias to the junction in the semiconductor substrate, the colliding of incident neutrons with the resident 3 He gas results in a reaction which produces hole-electron pairs in the depletion layer within the semiconductor, those hole-electron pairs producing output electrical pulses which appear at the output terminals of the detector for utilization by detection and measuring apparatus connected to the semiconductor-based radiation-detector element. | 8 |
This application is a continuation of U.S. patent application Ser. No. 07/730,164, filed Jul. 16, 1991 now U.S. Pat. No. 5,330,967.
BACKGROUND OF THE INVENTION
The present invention relates to superconducting bearing devices having incorporated therein a superconductor permitting penetration of a magnetic flux thereinto.
Superconducting bearing devices heretofore known include, for example, the one disclosed in Unexamined Japanese Patent Publication SHO 63-243523.
The superconducting bearing device disclosed includes a Type I superconductor, i.e., a superconductor preventing the penetration of magnetic flux perfectly to utilize the perfect diamagnetism of the superconductor. The device comprises a rotary shaft made of the superconductor and having its opposite ends fitted in a pair of recesses each of which is formed in a support member of magnetic material magnetized to one of the polarities, the rotary shaft being supported in a non-contacting position axially thereof.
With the known superconducting bearing device, the rotaty shaft is supported in a non-contacting position utilizing perfect diamagnetism as stated above and is therefore instable with respect to a direction orthogonal to the direction of repulsion, so that the support member for supporting each end of the rotary shaft must be machined to a shape surrounding the shaft end. Furthermore,between the shaft end and the support member, the portion opposed to the shaft end axially and radially of the shaft needs to be magnetized. Accordingly, the device is cumbersome to design and make.
SUMMARY OF THE INVENTION
The main object of the present invention is to provide a superconducting bearing device adapted to support a rotatable member by a simple construction.
The present invention provides a superconducting bearing device which comprises, in a temperature environment for realizing a Type II superconducting state, a permanent magnet portion provided on a rotatable member, and a Type II superconductor disposed as opposed to the permanent magnet portion, the permanent magnet portion being so mounted on the rotatable member that the rotation of the rotatable member does not alter the magnetic flux distribution around the axis of rotation of the rotatable member, the Type II superconductor permitting penetration of the magnetic flux of the permanent magnet portion thereinto and being spaced apart from the permanent magnet portion by a distance permitting a predetermined quantity of magnetic flux thereof to penetrate thereinto, the superconductor being disposed at a position not permitting the rotation of the rotatable member to alter the distribution of penetrating magnetic flux.
According to an embodiment, the permanent magnet portion is in the form of a disk and mounted on the rotatable member concentrically therewith, and the superconductor is opposed to an end face of the magnet portion and spaced apart therefrom .axially of the rotatable member.
According to another embodiment, the permanent magnet portion is in the form of a disk and mounted on the rotatable member concentrically therewith, and the super conductor is opposed to the outer periphery of the magnet portion and spaced apart therefrom radially of the rotatable member.
The restraining action of the magnetic flux of the permanent magent portion penetrating into the superconductor stably holds the magnet portion and the superconductor opposed to each other and spaced apart by a predetermined distance. In this state, the rotatable member carrying the magnet portion can be rotated about the axis of the member. At this time, the external magnetic field acting on the superconductor offers no resistance to the rotation insofar as the magnetic flux distribution is uniform with respect to the axis of rotation and remains unchanged. Accordingly, the rotatable member can be supported by the superconductor in a non-contacting position radially and axially thereof when the magnet portion mounted on the rotatably member is merely position in place relative to the superconductor without the necessity of machining the superconductor to a shape surrounding the end of the member to support the member.
Thus, the device of the invention is adapted to rotatably support the rotatable member with good stability by a very simple construction.
According to another embodiment of the invention, the permanent magnet portion comprises a plurality of annular permanent magnets arranged at a spacing radially of the rotatable member and a nonmagnetic material interposed therebetween, and the ends of each permanent magnet which are opposite axially of the rotatable member are mangnetized to polarities opposite to each other, all the permanent magnets being magnetized to the same polarity at their ends which are positioned toward the same direction with respect to the axis of rotation.
At each end of the permanent magnet portion thus constructed, the magnetism of one of the magnets repels that of another magnet of the same polarity, causing the magnetic flux to extend axially of the rotatable member and permitting an increased quantity of flux to penetrate into the superconductor which is disposed as opposed to the end face of the permanent magnet portion. Consequently, the superconductor traps the increased amount of flux to give the device an increased load capacity and enhanced rigidity.
According to another embodiment of the invention, the permanent magnet portion comprises a plurality of annular permanent magnets arranged at a spacing radially of the rotatable member and a nonmagnetic material interposed therebetween, and the side portions of each permanent magnet which are opposite radially of the member are magnetized to polarities opposite to each other, the opposed side portions of the adjacent magnets being magnetized to the same polarity.
At the opposed side portions of the adjacent magnets in this arrangement, the magnetism of one portion repels that of the other portion having the same polarity, with the result that the magnetic flux expands both axially and radially of the rotatable member. This permits an increased quantity of flux to penetrate into the superconductor which is opposed to the end faces of the permanent magnet portion and to the outer periphery thereof, consequently giving an increased load capacity and enhanced rigidity as in the above embodiment.
According to another embodiment of the invention, the permanent magnet portion comprises a plurality of annular permanent magnets arranged at a spacing axially of the rotatable member and a nonmagnetic material interposed therebetween, and the ends of each permanent magnet which are opposite axially of the rotatable member are magnetized to polarities opposite to each other, the opposed ends of the adjacent magnets being magnetized to the same polarity.
At the opposed ends of the adjacent magnets in this arrangement, the magnetism of one end repels that of the other end having the same polarity, with the result that the magnetic flux expands both axially and radially of the rotatable member. This permits an increased quantity of flux to penetrate into the superconductor which is opposed to the end faces of the permanent magnet portion and to the outer periphery thereof, consequently giving a greater load capacity and higher rigidity as in the above embodiment.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevation schematically showing a first embodiment of superconducting bearing device of the invention;
FIG. 2 is a side elevation schematically showing a second embodiment of superconducting bearing device of the invention;
FIG. 3 is a view in vertical section schematically showing a third embodiment of superconducting bearing device of the invention;
FIG. 4 is a view in vertical section schematically showing a fourth embodiment of superconducting bearing device of the invention;
FIG. 5 is a view in vertical section schematically showing a fifth embodiment of superconducting bearing device of the invention;
FIG. 6 is a view in vertical section schematically showing a sixth embodiment of superconducting bearing device of the invention;
FIG. 7 is a view in vertical section schematically showing a seventh embodiment of superconducting bearing device of the invention; and
FIG. 8 is a view in vertical section schematically showing an eighth embodiment of superconducting bearing device of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Several embodiments of the present invention will be described below with reference to the drawings. Throughout the drawings, like parts are designated by like reference numerals.
FIG. 1 schematically shows the main arrangement providing a first embodiment.
This embodiment, i.e., a superconducting bearing device, comprises a solid cylindrical rotatable member 1, and a superconductor 2 in the form of a flat plate.
The rotatable member 1 in its entirety is a permanent magnet portion in the form of a single permanent magnet. The rotatable member 1 has one end magnetized to an N pole, and the other end magnetized to an S pole.
The superconductor 2 comprises a base plate which is prepared from a high-temperature superconducting material of the yttrium type of great pinning force, for example, YBa 2 Cu 3 O x , and which contains normally conductive particles (Y 2 Ba 1 Cu 1 ) as uniformly mixed with the superconducting material. The superconductor 2 has properties to trap the magnetic flux released from the rotatable member 1 and penetrating thereinto.
The rotatable member 1 is disposed with its axis positioned horizontally and is rotatable about the axis without permitting alteration of the magnetic flux distribution around the axis despite the rotation.
The superconductor 2 is opposed to the rotatable member 1 and disposed at a position spaced apart from the member 1 by a distance permitting a predetermined quantity of magnetic flux of the member 1 to penetrate into the superconductor, the superconductor 2 further being so positioned that the rotation of the member 1 will not alter the distribution of penetrating magnetic flux. With the present embodiment, the superconductor 2 has its upper surface opposed to the outer peripheral surface of the rotatable member 1 and is positioned horizontally below the rotatable member 1 in parallel thereto.
When the bearing device is to be operated, the superconductor 2 is cooled by suitable cooling means and maintained in a superconducting state.
If the rotatable member 1 is merely disposed horizontally above the superconductor 2 as positioned horizontally in a superconducting state, only a small quantity of magnetic flux of the member 1 penetrates into the superconductor 2, so that the member 1 is merely levitated by a repulsive force due to the Meissner effect of the superconductor 2 and is not supported stably.
However, when the rotatable member 1 is disposed above the superconductor 2 in the vicinity thereof first and the superconductor 2 is thereafter cooled to the superconducting state, a large quantity of magnetic flux released from the rotatable member 1 penetrates into the superconductor 2 and is trapped in this state. Since the superconductor 2 contains pinning centers (e.g., normally conductive particles) as uniformly mixed with the superconducting material, the magnetic flux penetrating into the superconductor 2 becomes distrubuted also uniformly and is held trapped. Consequently, the rotatable member 1 is held levitated above the superconductor 2 and supported axially and radially with high stability.
When the rotatable member 1 as thus supported in a non-contacting position is rotated about its axis, the magnetic flux penetrating into the superconductor 2 offers no resistance to the rotation because the magnetic flux distribution around the axis remains unchanged despite the rotation. Further because the rotation involves no frictional resistance unlike sliding or rolling bearings, the rotatable member 1 is to rotate permanently, whereas the member is influenced by air resistance and geomagnetism in actuality and therefore comes to a halt eventually. Nevertheless, such resistance to rotation is very small for the bearing device and almost negligible.
If the rotatable member 1 as supported in the above non-contacting position is pushed in one direction with a force smaller than the pinning force, the member 1 shifts in this direction once, then shifts toward the original position, thus undergoing a swinging motion for some time, and thereafter comes to a stop at the original position. However, if the rotatable member 1 is pushed toward one direction with a force greater than the pinning force, the member 1 stops upon moving to a position to which it is forcibly shifted from the original position. Thus, the member 1 is restrained in the shifted position. This phenomenon occurs owing to the pinning force peculiar to the superconductor 2 of the foregoing structure.
If the magnetic flux of the rotatable member 1 is held pinned to the supercontactor 2 as described above, the rotatable member 1 will always be supported with good stability by a restraining action.
FIG. 2 schematically shows the main portion of another superconducting bearing device as a second embodiment.
This embodiment is the same as the first embodiment with respect to the structure and arrangement of the superconductor 2. The rotatable member 1, although the same as the one included in the first embodiment, is disposed above the superconductor 2 with its axis of rotation positioned vertically. The upper surface of the superconductor 2 is opposed to the lower end face of the rotary member 1. With the exception of this feature, the second embodiment is the same as the first.
With the second embodiment, the rotatable member 1 is also supported as levitated above the superconductor 2 as in the case of the first embodiment.
In the foregoing two embodiments, the arrangement of the rotatable member 1 and the superconductor 2 may be inverted. In other words, the rotatable member 1 may be disposed below the lower surface of the superconductor 2 in proximity to the superconductor 2. The rotatable member 1 is then supported as levitated as if being suspended from the superconductor 2. Alternatively, if the rotatable member 1 is opposed, as positioned obliquely, to the superconductor 2, the member 1 is held levitated in the oblique position.
FIG. 3 schematically shows the main portion of another superconducting bearing device, i.e., a third embodiment.
This bearing device comprises a rotatable member 1 in the form of a vertical shaft, and a superconductor 2. A permanent magnet portion 3 in the form of a horizontal disk is mounted on the rotatable member 1 concentrically therewith, and the superconductor 2 is opposed to the lower end face of the magnet portion 3 and spaced apart therefrom axially of the rotatable member 1. The superconductor 2 is in the form of a disk having a bore, and the rotatable member 1 extends through the bore with a clearance formed in the bore around the member 1.
The permanent magnet portion 3 is in the form of an integral assembly and comprises a plurality of annular permanent magnets 4a, 4b, 4c arranged at a spacing radially of the member 1, and a nonmagnetic material 5 interposed therebetween. The portion 3 is secured to the rotatable member 1. The upper and lower ends of each of the magnets 4a, 4b, 4c are magnetized to polarities opposite to each other, and all the magnets 4a, 4b, 4c are magnetized to the same polarity at their same ends. For example, the upper ends of all the magnets 4a, 4b, 4c are magnetized as N poles, and the lower ends thereof as S poles. The magnetic flux distribution around the axis of rotation is free of changes despite the rotation of the member 1.
The superconductor 2 has the same properties as the one included in the first embodiment and is disposed at a position spaced apart from the magnet portion 3 by a distance permitting a predetermined quantity of magnetic flux of the portion 3 to penetrate thereinto and which will not permit the rotation of the member 1 to alter the distribution of penetrating magnetic flux.
A cooling case 22 which is cooled by a refrigerator 20 or the like via a temperature control unit 21 is fixedly provided within a housing (not shown) for the bearing device. The superconductor 2 is fixed to the cooling case 22.
When the superconducting bearing device is operated, the superconductor 2 is cooled with a suitable refrigerant circulated through the cooling case 22 and maintained in a superconducting state. As in the case of the first embodiment, the restraining action of the magnetic flux penetrating into the superconductor 2 from the permanent magnet portion 3 and trapped in the superconduct 2 holds the rotatable member 1 and the superconductor 2 opposed to each other with a predetermined spacing provided therebetween and supports the member 1 as levitated above the superconductor 2.
At each end of the permanent magnet portion 3, the magnetism of one of the permanent magnets 4a, 4b, 4c repels that of another magnet of the same polarity, with the result that the magnetic flux extends to a greater extent axially of the rotatable member 1 than in the case where the permanent magnet portion has a single permanent magnet. Consequently, an increased quantity of flux penetrates into the superconductor 2 which is disposed as opposed to the lower end face of the magnet portion 3 for the superconductor 2 to trap the increased quantity of flux. This gives the device a greater load capacity and higher rigidity.
In addition to the superconductor 2, second superconductors 6 may be provided as indicated in broken lines in FIG. 3. These second superconductors 6 are arranged radially outwardly of the periphery of the permanent magnet portion 3 at a distance from and as opposed to the periphery. These superconductors 6 also support the rotatable member 1, consequently giving further enhanced rigidity to the entire bearing device. These superconductors 6 may form a completely annular block or may be segments of an annular block.
FIG. 4 schematically shows the main portion of another superconducting bearing device, i.e. a fourth embodiment.
In this embodiment, superconductors 2, 6, 7 are provided as opposed respectively to the lower end face, outer peripheral surface and upper end face of a permanent magnet portion 3 on a rotatable member 1.
FIG. 5 schematically shows the main portion of another superconducting bearing device, i.e., a fifth embodiment.
This embodiment has a permanent magnet portion 8 which also comprises a plurality of annular permanent magnets 9a, 9b arranged at a spacing radially of the rotatable member 1 and a nonmagnetic material 10 interposed therebetween. The side portions of each permanent magnet 9a or 9b which are opposite radially of the rotatable member 1 are magnetized to polarities opposite to each other, and the opposed side portions of the adjacent magnets 9a, 9b are magnetized to the same polarity. For example, the inner side portion of the inner magnet 9a has N pole, the outer side portion thereof S pole, the inner side portion of the outer magnet 9b S pole, and the outer side portion thereof N pole. Three or more permanent magnets, when used, are also magnetized similarly.
At the opposed side portions of the adjacent magnets 9a, 9b in this embodiment, the magnetism of one side portion repels that of the other side portion having the same polarity, with the result that the magnetic flux expands both axially and radially of the rotatable member. This permits an increased quantity of flux to penetrate into the superconductor 2 which is opposed to the lower end face of the permanent magnet portion 8.
In this case, additional superconductors may also be provided as opposed to the outer peripheral surface and the upper end face of the magnet portion 8.
FIG. 6 schematically shows the main portion of another superconducting bearing device, i.e., a sixth embodiment.
This embodiment has a permanent magnet portion 11 in the form of an integral assembly and comprising a plurality of annular permanent magnets 12a, 12b arranged at a spacing axially of the rotatable member 1 and a nonmagnetic material 13 interposed therebetween. The side portions of each magnet 12a or 12b which are opposite axially of the rotatable member are magnetized to polarities opposite to each other, and the opposed ends of the adjacent magnets 12a, 12b are magnetized to the same polarity. For example, the upper end of the upper magnet 12a is magnetized as N pole, the lower end thereof as S pole, the upper end of the lower magnet 12b as S pole, and the lower end thereof as N pole. The same is true of the case wherein three or more permanent magnets are used.
At the opposed ends of the adjacnet magnets 12a, 12b of the sixth embodiment, the magnetism of one end repels that of the other end having the same polarity, with the result that the magnetic flux expands both axially and radially of the rotatable member. This permits an increased quantity of flux to penetrate into the superconductor 2 which is opposed to the lower end face of the magnet portion 11.
In this case, additional superconductors may also be provided as opposed to the outer peripheral surface and the upper end face of the permanent magnet portion 11.
FIG. 7 schematically shows the main portion of another superconducting bearing device, i.e., a seventh embodiment.
In this embodiment, the superconductor 2 of the fifth embodiment is replaced by a superconductor 6 opposed to the outer peripheral surface of the permanent magnet portion 8.
As already stated with reference to the fifth embodiment, the magnetic flux expands both axially and radially of the rotatable member also in this case, with the result that an increased quantity of flux penetrates into the superconductor 6 which is disposed as opposed to the outer peripheral surface of the magnet portion 8.
FIG. 8 schematically shows the main portion of another superconducting bearing device, i.e., an eighth embodiment.
In this embodiment, the superconductor 2 of the sixth embodiment is replaced by a superconductor 6 opposed to the outer peripheral surface of the permanent magnet portion 11.
As already described with reference to the sixth embodiment, the magnetic flux expands both axially and radially of the rotatable member also in this case, with the result that in increased quantity of flux penetrates into the superconductor 6 which is disposed as opposed to the outer peripheral surface of the magnet portion 11. | A superconducting bearing device includes a permanent magnet on a rotor, with a superconductor placed opposite the magnet. Flux trapped in the superconductor during cooling helps to stabilize the rotor. More specifically, the permanent magnet is mounted on the rotor so that, as the rotor rotates, its rotation does not alter the magnetic flux distribution around the axis of rotation of the rotor. The superconductor permits penetration of the magnetic flux from the magnet, being spaced from the magnet by a distance that permits a predetermined quantity of the magnetic flux to penetrate it, while not permitting rotation of the rotor to alter the distribution of the penetrating magnetic flux. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application Ser. No. 60/020,952 filed Jun. 19, 1996.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an environmentally safe detergent, or cleaning and sanitizing composition, for cleaning diverse surfaces. The composition is completely biodegradable and contains a mixture of nonionic surfactants, a phosphate ester anionic surfactant, a mixture of specific ethanolamines, water and a chelating agent.
2. Description of Relevant Art
In today's environmentally conscious society, it is particularly desirable to provide compositions which are useful for performing daily cleaning and sanitizing tasks and which also are biodegradable. This need has been met by many diverse types of cleaning compositions; however, each is generally suited for cleaning specific surfaces. Thus, there is a need to replace the many different kinds of cleaning agents useful for cleaning various kinds of surfaces with a single, universal cleaning composition that is effective, inexpensive, biodegradable and environmentally friendly.
Cleaning compositions comprising water, surfactants, emulsifiers, etc. for removing oily residues from surfaces are well known. British Pat. No. 1,066,407 to Unilever Limited discloses mixtures of nonionic surfactants, fatty acid and alkanolamine for use on metal surfaces. However, this disclosure does not describe a mixture of the specific nonionic surfactants of the present invention with an acid phosphate ester of an ethoxylated alcohol, an anionic surfactant.
A report by the Shell Chemical Co. describes the performance of various C 9 -C 13 alcohol ethoxylates as hard surface cleaners. The performance was measured only against non-polar, oily soil on a non-polar, hydrophobic substrate.
A patent from the former Soviet Union, SU 681134 to Urals Chem. discloses a composition f or removing ink stains comprising mixtures of monoethanolamine and triethanolamine, mixed polyglycol esters of alkyl phenols, polypropylene glycol and an anionic surfactant. However, the patent does not show the combination of an acid phosphate ester, specific ethanolamine mixtures and specific nonionic surfactant mixtures.
U.S. Pat. No. 5,124,077 to Kajihara et al. discloses a skin detergent composition comprising a phosphoric acid ester surfactant and a water soluble chitin derivative. However, the patent does not provide teachings of the use of acid phosphate esters of ethoxylated alcohol, specific nonionic surfactants and specific mixture of ethanolamines for use in cleaning diverse surfaces.
U.S. Pat. No. 5,078,991 to Birtwistle et al. discloses a composition for skin treatment comprising a phosphate salt. There is no disclosure, however, of the use of other ingredients to arrive at a multi-utility cleaning composition.
U.S. Pat. No. 4,197,197 to Abaeva et al. discloses a dispersant for removing oil from water surfaces comprising the use of esters of hydroxyethylated higher aliphatic alcohols of phosphoric acid.
U.S. Pat. No. 3,948,919 to Wilde discloses a cleaning composition for aircraft comprising a mixture of nonionic surfactants having different mole amounts of ethylene oxide units per molecule.
Japanese Pat. No. 6-107984 to Yushiro Chem. Ind. shows a cleaning composition comprising mixtures of an ethanolamine with EDTA, anionic and nonionic surfactants and an aromatic alcohol. However, the patent does not teach the use of the specific nonionic surfactants and anionic surfactants with EDTA and a specific mixture of ethanolamines for use in multi-surface cleaning.
While the prior art may show the use of the various compounds I use in my invention for a cleaning composition, none of the patents or other disclosures teach my specific composition, nor provide any motivation for making my specific composition, and none of the above inventions and patents, taken either singly or in combination, describes my invention as claimed.
OBJECTS OF THE INVENTION
Accordingly, it is a principal object of my invention to provide a cleaning composition for various kinds of surfaces which is highly effective and substantially free from deleteriously effecting our environment on earth when used in a normal manner for cleaning.
It is another object of the invention to provide a universal cleaning or detergent composition comprising a mixture of an anionic surfactant, specifically an acid phosphate ester of an ethoxylated alcohol, two nonionic surfactants, namely ethylene oxide abducts of a C 11 linear primary alcohol, triethanolamine, monoethanolamine and a chelating agent, the forgoing being mixed with water as a solvent, carrier or vehicle.
It is a further object of the invention to provide a composition having wide utility, not only as a general cleaning agent, but also for use in soil redemption, and for use as a healing promoter for cuts and burns, due to the composition's sanitizing properties.
Still another object of the invention is to provide a cleaning composition that does not contain and is free from lower alkyl alcohols, phenols, solvent esters or ester-ethers such as, for example, butyl esters or glycols, for example, ethylene glycol monobutylether, hydrocarbon solvents, ethers, ketones, inorganic phosphates, silicates, borates, potassium or sodium hydroxide, and organic and inorganic acids, but which nevertheless is an effective and efficient cleaning agent, capable of substituting for several different detergents, each having specific cleaning properties or functions, for example.
It is an object of the invention to provide an improved, universal cleaning, sanitizing and soil reclamation composition for the purposes described which is inexpensive, dependable and fully effective in accomplishing its intended purposes.
These and other objects of the present invention will become readily apparent upon further review of the following specification.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention relates to a cleaning, sanitizing, soil reclamation, waste and water treatment composition. However, the composition is intended to function primarily as a detergent or cleaner for removing from many kinds of surfaces what is generically referred to as dirt, namely: synthetic and natural oil residues, grease, fat residues, the partial thermal decomposition products thereof and other organic and inorganic residues, deposits or coatings and mixtures thereof.
A few of the surfaces upon which my composition is effective, for example, include: wood, fine fabrics, polymethyl methacrylate polymer and plastic, stainless steel, gold, silver, brass, copper aluminum and glass. Depending upon the dilution ratio with water from the concentrated formula, other applications for cleaning or removing unwanted residues, for example, include: fruits and vegetables, automobile exteriors and interiors, bowling ally lanes, carpets, showers, tubs, slot machine surfaces, cooling tower scale removal, swimming pools, tile, mirrors, clothing, canvas, leather, rust removal, white walled tires, machinery and woodwork. With respect to fine fabrics, or colored or dyed cloth, however, it is to be noted that the use of my composition at full strength, the concentrate, that is, without dilution with water, to clean these materials, may result in some of the dye or color in the fabric either being removed or chemically altered.
More specifically, my invention composition may comprise any of three different forms. In this disclosure the expression "active ingredient" means an ingredient other than water which functions as an emulsifying agent, surface active agent, wetting agent, detergent, base, chelating agent, coupling agent or water solubility or miscibility enhancing agent. The term "base" refers to compounds classified as such in the ordinary chemical sense.
One form of my invention is a composition comprising only the active ingredients, or raw mixture. Another form is a composition comprising the active ingredients, an amount of water to make a concentrate or concentrated mixture of active ingredients in solution with water, and optionally a preservative. The third form of my invention is a diluted composition, wherein the concentrated solution is further mixed with up to ten times or more of water. In the form of a diluted composition, it is particularly desirable to include a preservative in order to prevent microbial activity against the composition.
Insofar as the raw mixture of only or essentially only the active ingredients is concerned, the composition comprises the following ingredients in the weight proportions given based on the total weight of the composition:
a: from 3 to 4% of a chelating agent such as, for example, ethylene diamine tetrasodium acetate (EDTA)
b. from 21.5 to 30.5% of an anionic surfactant-coupling agent, for example, an acid phosphate ester of an ethoxylated alcohol
c. from 28.5 to 31.5% of a nonionic surfactant, for example, a C 11 linear primary alcohol ethoxylate having an average of 7 moles of ethylene oxide units
d. from 9 to 10.5% of a nonionic surfactant, for example, a C 11 linear primary alcohol ethoxylate having an average of 3 moles of ethylene oxide units
e. from 14 to 16.5% of an organic amine containing base, for example, monoethanolamine (MEA)
d. from 14 to 16.5% of an organic amine containing base, for example, triethanolamine (TEA)
Although EDTA has been provided as an example of a suitable chelating agent, other chelating agents may be substituted therefor.
The raw composition may be made by mixing the materials in a suitable container with the addition of sufficient heat to lower the viscosity of the ingredients in liquid form, and thus lower the amount of energy for the physical mixing process. Some of the raw materials or ingredients are obtained from suppliers and manufacturers in a liquid form which is quite viscous, thus heat may be applied to the container in which they are supplied to enable more efficient transfer from the supply container to mixing container. The above composition of raw ingredients, without water is used as a composition for making a cleaning composition when it is mixed with water.
The above composition may be made as a water solution concentrate. This is the second form of my invention. The water used, in order to make a composition of high quality, which possesses very reproducible results from batch to batch, should be distilled water or deionized water. If not, the water used should not contain excessive inorganic salt content, particularly salts of divalent metal ions. In this respect, the composition comprises the following ingredients in weight percent, based on total weight:
a. from 78 to 82% water
b. from 0.5 to 8.5% chelating agent
c. from 4.0 to 5.5% phosphate ester anionic surfactant
d. from 5.0 to 6.5% nonionic surfactant, ethoxylated primary alcohol having an average of 7 moles of ethylene oxide units
e. from 1.0 to 2.5% nonionic surfactant, an ethoxylated alcohol having an average of 3 moles of ethylene oxide units
f. from 2.5 to 3.5% of monoethanolamine
g. from 3.0 to 4.5% of triethanolamine
This concentrate composition may be made by mixing the ingredients in a specific order and manner into an appropriate amount of water. It is particularly important to begin the mixing operation by first mixing into water the chelating agent. A convenient container for mixing and storing the composition may be a 55 gallon drum, for example. The concentrate composition may additionally include a preservative, preferably a food grade preservative having sufficient activity as an antibacterial agent. It is particularly useful to include such a preservative in the concentrate composition if it is intended for consumer use in a diluted form, discussed hereinafter, which will be required to have a significant shelf-life.
The diluted composition may be made by the consumer or user depending upon the cleaning application under consideration. For example, to clean fruits and vegetables, a suitable dilution ratio is one-fourth teaspoon concentrate composition to one pint water. A suitable dilution ratio for cleaning showers (tile), walls, furniture, automobile exteriors and interiors, upholstery, woolens, silks, nylons or fine fabrics would be 15 parts water to 1 part concentrate composition. For glass surfaces 100 parts water to 1 part concentrate composition. For removing scale from cooling towers, use of the concentrate composition at full strength is appropriate.
My composition may also be used in ordinary washing processes for clothing. For example, one volume of normal liquid or powdered washing machine detergent may be mixed with 1/2 volume of my concentrate composition.
Regarding the method of use, it is conventional in the detergent arts insofar as the steps are concerned. For hard surfaces, the composition is applied to such surface either directly or through the agency of a solid carrier device, for example, a cloth, synthetic fabric, sponge, brush or other device capable of retaining the composition in contact therewith, the surface of which is substantially lower in hardness (MOHS) than the surface to be cleaned. Whether or not the composition is applied directly or through the agency of a carrier device, the composition in contact with the surface to be cleaned is combined with the frictional action of an applicator or carrier device. The combination of frictional forces and the chemical, surfactant and emulsifying properties possessed by the composition act to remove unwanted oily or fatty residues from surfaces.
In my compositions the most preferred embodiment comprises a composition containing ethylene diamine tetrasodium acetate (EDTA) as a chelating agent. The phosphate ester is preferably a compound such as a-hydro-w-hydroxy-mono-alkyl ether phosphate (CAS #68909-65-9), sold under the tradename Norfox PE600 and available from Norman, Fox & Co. The nonionic surfactants are preferably ethylene oxide adducts of a C 11 primary alcohol, namely a-undecyl-w-hydroxypoly(oxy-1,2-ethanediyl), one having an average of seven moles of ethylene oxide units and the other having an average of three moles of ethylene oxide units. Two exemplary surfactants are sold under the tradename Neodol 1-3 and Neodol 1-7, both of which are available from Shell Chemical Co. One example of a suitable antibacterial, food grade preservative is available under the tradename DOWICIL 75 from Van Water & Rogers, Inc., a subsidiary of Univar (Kirkland, Wash.). The ingredients of DOWICIL 75 are: 1-(3chloro-2-propenyl)-3,5,7-Triaza-1-azoniatricyclo 3.3.1.1 3 ,7 !decane chloride (CAS #004080-31-3), 69%; sodium bicarbonate (CAS #000144-55-8), 25%; and hexamethylenetetramine hydrochloride (CAS #058713-21-6), 4%. Further, I intend that my composition include minor amounts of other ingredients such as, for example, colorants, fragrances or odor enhancing agents, and other materials that function to provide my composition with resistance to degradation or decomposition resulting from oxidation or radiant energy, for example. Additionally, in respect to the monoethanolamine component, for some cleaning applications, this material may be omitted entirely and replaced with an equivalent amount of triethanolamine. However, against all types of soils for which my composition is intended, such modified compositions are not as effective as are compositions containing both monoethanolamine and triethanolamine.
The examples of preferred embodiments presented herein are for illustration and the invention is not to be construed as being limited thereto as set forth above, but it encompasses any and all embodiments within the scope of the following claims. Further, my invention includes the substitution of functionally equivalent materials for any and all of the ingredients I use in the sense that any material or ingredient capable of producing substantially identical functional properties, including cooperative synergistic properties, is usable in place of any of the materials of my invention. The effectiveness and efficiency with which the disclosed compositions function is due to the properties each of the ingredients possesses, in general, and are not necessarily due to the materials themselves.
It is to be understood that the present invention is not limited to the embodiments described above, but encompasses any and all embodiments within the scope of the following claims. | A cleaning and sanitizing composition for use essentially on surfaces, but having other related utilities. The composition comprises a mixture in certain proportions of an anionic surfactant, a mixture of ethanolamines, two nonionic surfactants and a chelating agent in a water vehicle. The composition may further comprise a food grade preservative to enhance shelf-life at higher dilutions of the composition. The composition contains no inorganic builders or salts, nor inorganic bases or acids. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to output stages for analog circuits, and more particularly, to output stages for amplifiers.
2. Description of the Related Art
Amplifiers are commonly known and used in discrete analog circuits and in monolithic integrated circuits (ICs). For details on amplifier fundamentals, see e.g., Malvino, Electronic Principles, McGraw-Hill, Inc., 1973. Often amplifiers will consist of a number of stages. These stages may, for example, include one or more amplifying stages followed by an output stage. One function served by an output stage is to provide an appropriate output impedance. It is also desirable that the output stage also provide amplification.
FIG. 1 illustrates a schematic diagram of a conventional output stage 100 of an amplifier. The output stage 100 includes a first transistor (Q 1 ) 102 and a second transistor (Q 2 ) 104. The emitters of first and second transistors 102 and 104 are connected together and receive a supply voltage (V CC ). Hence, the output stage is referred to as having a common-emitter configuration. The bases of the first and second transistors 102 and 104 are commonly connected. The collector of the first transistor 102 is connected to a signal current source (i s ) 106 as well as to the commonly connected bases of the first and second transistors 102 and 104. The signal current source (i s ) 106 is then coupled to ground (GND). The collector of the second transistor 104 is coupled to ground (GND) via a load resistor R L . The output voltage (V OUT ) is obtained from the collector of the second transistor 104.
The conventional output stage 100 is driven by the signal current source (i s ) 106, which serves as the input to the output stage 100. In producing the collector current (I c ), the output stage 100 amplifies the signal current source (i s ) 106 by a gain amount. The gain amount is determined by the ratio of the emitter areas, namely, the emitter area of the second transistor 104 divided by the emitter area of the first transistor 102 (Area Q2 /Area Q1 ). The output stage produces the output voltage (V OUT ) as the product of the collector current (I C ) and the load resistor (R L ) 108. The resulting output voltage (V OUT ) is able to swing to a maximum output of within one saturation voltage (V EC ) of the supply voltage (V CC ).
One problem with the conventional output stage 100 is that the gain it provides is rather limited in practice. Specifically, the area or size for the first transistor 102 cannot be made smaller than some predetermined minimum transistor size. Further, given that speed slows as area increases, the area or size for the second transistor 104 is also restricted by speed requirements of the device. Hence, although large gains are desired, only limited gains are practical with the convention output stage 100.
Thus, there is a need for an output stage for amplifiers that yields large gains without hindering high speed operation.
SUMMARY OF THE INVENTION
Broadly speaking, the invention relates to a high gain common-emitter output stage for an amplifier. The output stage or amplifier according to the invention is advantageous because the gain provided is exponential, yet the bias condition remains stable.
In a first embodiment, an output stage for an amplifier circuit according to the invention includes: a first transistor having a base, an emitter and a collector, the emitter being connected to a first potential through a first resistor, the collector being connected to a second potential through a series connection of a second resistor and a bias current source, the base being connected between the second resistor and the bias current; a second transistor having a base, an emitter and a collector, the emitter being connected to the first potential, the collector being connected to the second potential through a load element, the base being connected to the collector of said first transistor; and a signal current source for supplying a current signal to be amplified. The output stage according to the invention is advantageous because the gain provided is exponential, yet the bias condition remains stable. The output stage also operates efficiently from a power perspective as power consumption is low during quiescent conditions.
In a second embodiment, an amplifier for amplifying a difference voltage between first and second input voltages to produce an output voltage includes: a first buffer circuit for receiving the first and second input voltages and producing complementary current signals; and a current amplification circuit for receiving the complementary current signals and outputting an output voltage, the output voltage being an amplified version of the difference of the first and second input voltages, and the current amplification circuit including complementary circuitry. The complementary circuitry includes first and second circuits connected to the first buffer circuit. The first circuit includes: a first transistor having a base, an emitter and a collector, the emitter being connected to a first potential through a first resistor, the collector being connected to a second potential through a series connection of a second resistor and a first bias current source, the base being connected between the second resistor and the first bias current source, the collector also being connected to receive a first of the complementary current signals; and a second transistor having a base, an emitter and a collector, the emitter being connected to the first potential, the collector being connected to an output terminal from which the output voltage is obtained, the base being connected to the collector of the first transistor. The second circuit includes: a third transistor having a base, an emitter and a collector, the emitter being connected to the second potential through a third resistor, the collector being connected to the first potential through a series connection of a fourth resistor and a second bias current source, the base being connected between the fourth resistor and the second bias current source, the collector also being connected to receive a second of the complementary current signal; and a fourth transistor having a base, an emitter and a collector, the emitter being connected to the second potential, the collector being connected to the output terminal, the base being connected to the collector of the third transistor. The amplifier may further include a feedback network coupled between the output terminal and the second input voltage.
Advantages of amplifiers or output stages for amplifiers according to the invention include improved gain, while maintaining a stable bias condition, full voltage swing and low power utilization. Other aspects and advantages of the invention will become apparent from the following detailed description, taken in conjunction with the accompanying drawings, illustrating by way of example the principals of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be readily understood by the following detailed description in conjunction with the accompanying drawings, wherein like reference numerals designate like structural elements, and in which:
FIG. 1 illustrates a schematic diagram of a conventional output stage of an amplifier;
FIG. 2 illustrates a schematic diagram of an output stage of an amplifier according to a first embodiment of the invention;
FIG. 3 is a schematic diagram of complementary output stage according a second embodiment of the invention;
FIG. 4 illustrates a schematic diagram of an output stage according to a third embodiment of the invention; and
FIG. 5 illustrates a schematic diagram of an output stage according to a fourth embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
The invention relates to a high gain common-emitter output stage for an amplifier. The output stage according to the invention is advantageous because the gain provided is exponential, yet the bias condition remains stable.
Embodiments of the invention are discussed below with reference to FIGS. 2-5. However, those skilled in the art will readily appreciate that the detailed description given herein with respect to these figures is for explanatory purposes as the invention extends beyond these limited embodiments.
FIG. 2 illustrates a schematic diagram of an output stage 200 of an amplifier according to a first embodiment of the invention. The output stage 200 includes a first transistor (Q 1 ) 202 and a second transistor (Q 2 ) 204. The emitters of first and second transistors 202 and 204 are connected together to a supply voltage (V CC ). Hence, the output stage 200 is referred to as having a common-emitter configuration. However, although the second transistor 204 connects directly to the supply voltage (V CC ), the first transistor 202 connects to the supply voltage (V CC ) via a first transistor (R 1 ) 206.
The collector of the first transistor 202 is connected to ground (GND) through the series connection of a second resistor (R 2 ) 208 and a bias current source (I B ) 210. More particularly, the collector of the first transistor 202 is connected to a first side of the second resistor 208 and the bias current source (I B ) 210 is connected between a second side of the second resistor 208 and ground (GND). The connection of the bias current source (I B ) 210 and the second side of the resistor 208 occurs at a node 212. The base of the first transistor 202 is also connected to the node 212. The collector of the first transistor 202 is also connected to a signal current source (i s ) 214. That is, the signal current source (i s ) 214 is connected between the collector of the first transistor 202 and ground (GND). The signal current source (i s ) 214 includes a DC component (i s (DC)) and an AC component (i s (AC)). The DC component is present even during quiescent conditions for biasing purposes. The AC component is an input current signal that is to be amplified and output.
With respect to the second transistor 204, the base of the second transistor 204 is connected to the collector of the first transistor 202 (which is in turn connected to the signal current source (i s ) 214), and the collector of the second transistor 204 is coupled to ground (GND) via a load resistor (R L ) 216. The output voltage (V OUT ) is obtained from the collector of the second transistor 204. In particular, the output voltage (V OUT ) is determined in accordance with equation 1 below.
V.sub.OUT =I.sub.C ·R.sub.L (1)
The resulting output voltage (V OUT ) is able to swing to a maximum output of within one saturation voltage (V EC ) of the supply voltage (V CC ).
In producing a collector current (I C ) from the collector of the second transistor 204, the output stage 200 amplifies the signal current source (i s (AC)) 214 by a gain amount. The gain amount is determined by equation 2 below
i.sub.C ≅I.sub.s2 e.sup.i.sbsp.s(AC).sup.R.sbsp.1.sup./V.sbsp.T(2)
where V T is the thermal voltage and is determined by V T =kT/q, with k being the Boltzmann constant, T being temperature (Kelvin), q being electronic charge magnitude, and I s2 being the reverse saturation current of the second transistor (Q 2 ) 202.
Thus, as clear from equation (2), the output stage 200 provides a high current gain. Namely, the first resistor (R 1 ) 206 causes a high current gain in response to the signal current source (i s ) 214. The second resistor (R 2 ) 208, On the other hand, stabilizes the bias condition. It should be noted that the voltage across the first resistor (R 1 ) 206 increases the voltage impressed upon the emitter-base junction of the second transistor 204, while the voltage across the second resistor (R 2 ) 208 decreases it. Under quiescent conditions (i.e., i s (AC) =0), making the voltage drop across the first and second resistors 206 and 208 equal neutralizes the effects of the first and second resistor 206 and 208, and therefore, stabilizes the bias condition. Given that the currents running through the first and second resistors 206 and 208 are not equal, the values (e.g., ohms) of the first and second resistors 206 and 208 are typically not equal. By using monolithic IC resistors, this equal voltage condition easy to control using resistor matching. When the voltage drop across the first and second resistors 206 and 208 are essentially equal, only the emitter-base voltage of the first transistor (Q 1 ) impresses upon the emitter-base junction of the second transistor (Q 2 ) and the inherent transistor matching of monolithic processes makes the resulting bias condition highly predictable. In other words, when the voltage drop across the first and second resistors 206 and 208 are essentially equal, no significant voltage drop due to the first and second resistors 206 and 208 influences the emitter-base junction of the second transistor (Q 2 ).
Under signal drive conditions, the signal current source (i s (AC)) 214 increases the voltage drop across the first resistor (R 1 ) 206 to produce an exponentially related current change in the second transistor 204(Q 2 ). See equation 2. Note that the signal current source (i s ) 214 does not flow in the second resistor (R 2 ) 208 to produce a counteracting effect like that produced by the bias current source (I B ) 210.
Although it is preferred to have the voltage drop across the first and second resistors 206 and 208 be substantially equal, in some cases, the equal voltage condition may intentionally not be exactly met. In particular, making one of the voltages smaller or larger than the other alters the temperature coefficient of the quiescent collector current (I C ) conducted by the second transistor (Q 2 ) 204, as may be desired such as for a temperature dependent bias. In such cases, keeping the voltage drop difference small compared to the emitter-base voltage of the second transistor (Q 2 ) 204 retains an adequately predictable quiescent bias.
Another advantage of the output stage 200 according to the invention is that the fixed bias current source (I B ) 210 of the circuit is fixed and thus assures that the second transistor (Q 2 ) 204 never turns off under extreme signal swing conditions of the signal current source (i s ) 214. In other words, the bias current source (I B ) 210 ensures that the transistor (Q 2 ) 204 remains biased even when the signal current source (i s ) goes to zero. In contrast, with the conventional output stage 100 illustrated in FIG. 1, the transistor (Q 2 ) 104 turns off when the signal current source i s goes to zero. Such turn off of the transistor is undesirable because it degrades bandwidth and causes distortion.
FIG. 3 is a schematic diagram of complementary output stage 300 according a second embodiment of the invention. In this embodiment, a differential input voltage (V 1 -V 2 ) is amplified and output. The output stage 300 includes an input diamond follower circuit 302 and a current amplifier circuit 304.
The input diamond follower 302 receives the complementary input voltages V 1 and V 2 and supplies complementary current signals to the current amplifier circuit 304. The current amplifier circuit 304 receives the complementary current signals and then amplifies the complementary current signals to output an output voltage (V OUT ).
The input diamond follower 302 includes a first transistor (Q 1 ) 306 and a second transistor (Q 2 ) 310. The base of the first transistor 306 receives the input voltage V 1 , the collector of the first transistor 306 is connected to a current source (I c ) 308 that is in turn connected to a positive power supply source (V CC ), and the collector of the first transistor 306 is coupled to a negative power supply source (V EE ). The base of the second transistor 310 receives the input voltage V 1 , the collector of the second transistor 310 is connected to the positive power supply source (V CC ), and the emitter of the second transistor 310 is connected to a current source (I c ) 312 that is in turn connected to the negative power supply source (V EE ). In this embodiment, the first transistor (Q 1 ) 306 is a PNP-type transistor and the second transistor (Q 2 ) 310 is an NPN-type transistor.
The input diamond follower 302 also includes a third transistor (Q 3 ) 314 and a fourth transistor (Q 4 ) 316. The input voltage V 2 is coupled to the commonly connected emitters of the third transistor (Q 3 ) 314 and the fourth transistor (Q 4 ) 316. The base of the third transistor 314 is connected to the emitter of the first transistor 306, and the base of the fourth transistor 316 is connected to the emitter of the second transistor 310. The input diamond follower 302 provides two (complementary) outputs to the current amplifier circuit 304. The first output is from the collector of the third transistor 314, and the second output is from the collector of the fourth transistor 316. In comparison to the first embodiment illustrated in FIG. 2, the first and second output signals from the input diamond follower 302 replaced the signal current source (I s ) 214.
The current amplifier circuit 304 is coupled to the input diamond follower 302 to receive the two (complementary) outputs therefrom. Since the current amplifier circuit 304 is a complementary design, the circuitry illustrated in FIG. 2 for a non-complementary design appears essentially twice in this embodiment.
One complementary portion of the current amplifier circuit 304 includes a fifth transistor (Q 5 ) 318 and a sixth transistor (Q 6 ) 320. In this embodiment, the fifth and sixth transistors 318 and 320 are PNP-type transistors. The emitter of the fifth transistor 318 is coupled to the positive power supply source (V CC ) via a first resistor (R 1a ) 322. The bases of the fifth and sixth transistors 318 and 320 are connected together. The collector of the fifth transistor 318 receives the first output signal from the third transistor 314 of the input diamond follower 302. The collector of the fifth transistor 318 is also connected to a series connection of a second resistor (R 2a ) 324 and a bias current source (I Ba ) 326. The bias current source (I Ba ) 326 is then in turn connected to the negative power supply source (V EE ). A connection of the second resistor (R 2a ) 324 and the bias current source (I Ba ) 326 occurs at a node 328. The node 328 is also connected to the commonly connected bases of the fifth and sixth transistors 318 and 320. The emitter of the sixth transistor 320 is directly connected to the positive power supply source (V CC ), and the collector of the sixth transistor 320 is connected to an output terminal to output an output voltage V OUT .
The other complementary portion of the current amplifier circuit 304 includes a seventh transistor (Q 7 ) 330 and an eighth transistor (Q 8 ) 332. In this embodiment, the seventh and eighth transistors 330 and 332 are NPN-type transistors. The emitter of the seventh transistor 330 is coupled to the negative power supply source (V EE ) via a first resistor (R 1b ) 334. The bases of the seventh and eighth transistors 330 and 332 are connected together. The collector of the seventh transistor 330 receives the second output signal from the fourth transistor 316 of the input diamond follower 302. The collector of the seventh transistor 330 is also connected to a series connection of a resistor (R 2b ) 336 and a bias current source (I Bb ) 338. The bias current source (I Bb ) 338 is then in turn connected to the positive power supply source (V CC ). A connection of the second resistor R 2b 336 and the bias current source (I Bb ) 338 occurs at a node 340. The node 340 is also connected to the bases of the seventh and eighth transistors 330 and 332. The emitter of the eighth transistor 332 is directly connected to the negative power supply source (V EE ), and the collector of the eighth transistor 332 is connected to the output terminal to output the output voltage V OUT .
The output impedance of the output stages 200, 300 are another limitation associated with the common-emitter output stages. With the first and second embodiments described above, the high impedance of transistor collectors at the output terminal makes the output stages highly sensitive to loading effects. Hence, output stages according to the invention may further include a feedback network to reduce the output impedance at the transistor collectors. By applying feedback from the output terminal, the output stage is desensitized to the loading effects.
One example of a feedback network is a direct connection from the output terminal to the input terminal receiving the input voltage V 2 . Such a direct connection provides unity feedback to make V OUT follow V 1 . Any output loading error would then produce a difference between the input voltages V 1 and V 2 , causing corrective drive of the current amplifier circuit 304 to remove the loading error.
In practice, however, the feedback network requires a feedback factor less than unity to fully realize the output swing capability (i.e., dynamic range) of the output stage. In general, the transistors 320 and 322 (Q 6 and Q 8 ) can swing to within their saturation voltages of their respective power supplies. However, with the direct connection type of the feedback network, the voltage swing (or dynamic range) is limited by the input diamond follower 302 (which does not offer as great a voltage swing). Hence, by setting a closed-loop gain greater than unity (i.e., feedback factor less than one) allows the output to swing a larger voltage than that applied at the input to the input diamond follower 302.
FIG. 4 illustrates a schematic diagram of an output stage 400 according to a third embodiment of the invention. The output stage 400 is similar to the third embodiment illustrated in FIG. 3 in that the input diamond follower 302 and the current amplifier circuit 304 are provided. However, additionally, the output stage 400 further includes a feedback circuit 402. The feedback circuit 402 is coupled between the node 342 at the output terminal for the output voltage (V OUT ) and the second input voltage V 2 at a node 404. The feedback circuit 402 includes a voltage divider. The voltage divider includes a first feedback resistor (R f1 ) 406 connected between the node 404 and ground (GND), and a second feedback resistor (R f2 ) 408 connected between the node 404 and the node 342. The closed-loop gain is set by the values of the first and second feedback resistors 406 and 408 such that it is greater than unity.
The choice of values for the feedback resistors 406 and 408 will vary with the particular application of the output stage 400. Even still, the choosing of the values for the feedback resistors 406 and 408 involves a trade-off situation. The trade-off is that with smaller resister values, there is higher current (and thus power) utilization, whereas with larger resister values DC offset errors are problematic. More particularly, the feedback resistors 406 and 408 of the feedback circuit 402 draws a feedback current from the output terminal and power efficiency considerations preclude setting the feedback resistors 406 and 408 at small values. However, these feedback resistors 406 and 408 also act as emitter degeneration to transistors 314 and 316 (Q 3 and Q 4 ) and must supply current to those transistors 314 and 316 in order to the drive the current amplifier circuit 304. Hence, achieving high gain with these transistors 314 and 316 requires making the feedback resistors 406 and 408 (R f1 and R f2 ) resistances small.
For those cases where this trade-off cannot be resolved by an acceptable compromise for the resistance values, an additional buffer can be provided to permit independent control of the feedback current and the gain of the stage. FIG. 5 illustrates a schematic diagram of an output stage 500 according to a fourth embodiment of the invention. The fourth embodiment is substantially similar to the third embodiment illustrated in FIG. 4, except that additional buffering is provided. In the output stage 500, besides including the (first) input diamond follower 302, the output buffer 304 and the feedback circuit 402, the output stage 500 further includes a second input diamond follower 502.
The second input diamond follower 502 is connected between the first input diamond follower 502 and the feedback circuit 402. The second input diamond follower 502 includes a transistor (Q 1b ) 504 and a transistor (Q 2b ) 508. The base of the transistor 504 receives the input voltage V 2 , the emitter of the transistor 504 is connected to a current source I c 506 that is in turn connected to the positive power supply source (V CC ), and the collector is coupled to the negative power supply source (V EE ). The base of the second transistor 508 receives the input voltage V 2 , the collector of the transistor 508 is connected to the positive power supply source (V CC ), and the emitter of the transistor 508 is connected to a current source (I c ) 510 that is in turn connected to the negative power supply source (V EE ).
The second input diamond follower 502 also includes a transistor (Q 3b ) 512 and a transistor (Q 4b ) 514. The base of the third transistor 512 is connected to the emitter of the transistor 504, and the base of the transistor 514 is connected to the emitter of the transistor 508. The emitters of the transistor (Q 3b ) 512 and the transistor (Q 4b ) 514 are commonly connected together at a node 516. A resistor (R G ) 518 is also provided with the second input diamond follower 502. The resister (R G ) 518 is coupled to the first input diamond follower 302 at a node 520 that connects the emitters of the transistors 314 and 316. The first input diamond follower 302 still provides the two (complementary) outputs to the current amplifier circuit 304. Hence, in this embodiment, the feedback resistors (R f1 and R f2 ) 406 and 408 need only supply the base currents of the transistors 504 and 508 (Q 1b and Q 2b ) so large resistances can be used. Further, the resistor (R G ) 518 now serves as the emitter degeneration to the transistors of the input emitter follower 302. Here, the resistor (R G ) 518 only conducts that current needed to drive the current amplifier circuit 304 and therefore can have a small resistance value so that high gains are achievable.
The many features and advantages of the present invention are apparent from the written description, and thus, it is intended by the appended claims to cover all such features and advantages 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 as illustrated and described. Hence, all suitable modifications and equivalents may be resorted to as falling within the scope of the invention. | A high gain common-emitter output stage for an amplifier is disclosed. In one embodiment, an output stage for an amplifier circuit according to the invention includes: a first transistor having a base, an emitter and a collector, the emitter being connected to a first potential through a first resistor, the collector being connected to a second potential through a series connection of a second resistor and a bias current source, the base being connected between the second resistor and the bias current; a second transistor having a base, an emitter and a collector, the emitter being connected to the first potential, the collector being connected to the second potential through a load element, the base being connected to the collector of said first transistor; and a signal current source for supplying a current signal to be amplified. The output stage according to the invention is advantageous because the gain provided is exponential, yet the bias condition remains stable. The output stage also operates efficiently from a power perspective as power consumption is low during quiescent conditions. | 7 |
This application is a Divisional application of application Ser. No. 401,694, filed Mar. 10, 1995; now U.S. Pat. No. 5,612,150.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a method of treating a secondary battery having at least one component containing alkali metal, e.g. lithium, and to apparatus for treatment of such a battery, in order to enable safe extraction and recovery of the alkali metal and optionally other components. In batteries, alkali metal may be present as the metal or in alloy form or as an intercalation compound, and the invention is applicable to all these forms.
2. Description of the Prior Art
A high energy density battery such as a lithium battery includes an active material of its negative electrode in the form of highly reactive alkali metal and an electrolytic solution containing LiPF 6 or LiAsF 6 which are reactive with water to produce HF. The battery typically further includes a positive electrode containing metal components capable of being regenerated. However, there has been not described any method of industrially processing spent batteries such as lithium batteries or any apparatus for processing such batteries.
The demand for high energy density batteries shows a yearly increase, and problems arise in terms of effective utilisation of chemical materials used in secondary batteries and of environmental pollution caused by batteries. For example, lithium and transition metal elements (Mn, Co) used in a lithium battery are valuable materials suitable to be regenerated. Moreover, a lithium secondary battery capable of being charged and discharged has been extensively used as a power supply for back-up of a computer or a power supply of small size domestic electric equipment, and is expected to be used for power storage or as a future power supply for an electric automobile. Accordingly, there must be developed a method of processing batteries and a method regenerating battery materials for suppressing environmental pollution due to chemical materials contained in the spent batteries and for effectively recovering such components used in batteries.
European patent application 94105151.8 (now published as EP-A-618633) and pending USA patent application 08/220 220 describe a process of treating a lithium battery by contacting the lithium in the battery with a liquid alcohol, to form an insoluble reaction product, followed by supply of liquid water and alcohol to form LiOH. The solution of LiOH in water and alcohol can then be withdrawn from the battery. The present invention takes a different approach to the problem.
SUMMARY OF THE INVENTION
The object of the present invention is to provide a method of treating a battery containing an alkali metal component which is excellent in safety and efficiency, and enables recovery of chemical materials capable of being regenerated, and to provide an apparatus for processing a battery accordingly.
The present inventors have analysed the problem of treating batteries containing alkali metal and reached the following conclusions.
Since a high energy density battery using an alkali metal, such as a lithium battery, contains active materials, i.e. reactive alkali metal and electrolytic solution which is unstable in contact with water vapor, attention should be paid to controlling the atmospheric gas when destroying a battery vessel. For example, the negative electrode of a lithium battery utilises lithium metal, a lithium alloy, an intercalated lithium compound or a carbon compound electrochemically containing lithium, any of which reacts strongly with water to generate hydrogen gas. Moreover, a nonaqueous electrolytic solution containing a fluorine compound such as LiPF 6 reacts with a water content in air, possibly to generate a harmful gas such as pentafluorophosphide or hydrogen fluoride. Accordingly, to destroy the vessel of a high energy density battery using an alkali metal and to expose battery components, the humidity of the external gas is desirably controlled.
To inactivate a high energy density battery with safety, the following functions may be performed: the battery casing is opened in a dry atmosphere and then reactive battery components and electrolytic solution are decomposed in a controlled atmosphere based on an inert gas, nitrogen gas or air. Moreover, to suppress the abrupt decomposition of such active components of the battery and prevent explosion of an inflammable gas such as hydrogen, and to shorten the decomposition time as much as possible, it is desirable to use a method of controlling the decomposition rate. In the case where the concentration of valuable material contained in the waste liquid obtained after processing of the battery is low, there may be required an enriching process; accordingly, to improve the regenerating efficiency of valuable materials and to shorten the battery processing time, it is desirable to fractional-recover the battery processing liquids according to the contents of the valuable materials, that is to say to recover two or more separate liquids after contact with the battery components.
According to the invention in one aspect, there is provided a method of treating a secondary battery comprising at least one component containing alkali metal, comprising the step of introducing a gas containing at least one of water vapor and alcohol vapor into a closed chamber containing at least this component, thereby to form alkali metal hydroxide or alkoxide. The chamber or the gas introduced may contain substantially no oxygen gas, but atmospheric air may be used as a carrier gas for the water vapor.
The water content in the introduced gas is preferably in the range 0.5 to 3 g per litre of gas. The gas temperature is preferably in the range 100° to 150° C. The alcohol content is preferably in the range 0.5 to 5 g per litre of gas.
When processing a large amount of battery components, an abrupt evolution of hydrogen may occur if water is added to alkali metals contained in battery. A hydrogen explosion can take place if the hydrogen concentration is higher than 4% in air. However, the water decomposition method hardly controls the rate of hydrogen evolution, because water has an extremely high reactivity to alkali metals. On the other hand, addition of water vapor to battery components can solve this problem. Water vapor content in a gas is easily controlled, so that the evolution rate of hydrogen can be suppressed under the limit which makes hydrogen explosive.
At the initial stage of the processing of alkali metals included in batteries, the water vapor content of the gas may be lower. The alkali metal is gradually decomposed into hydrogen and alkali hydroxide. As the decomposition rate decreases, the water vapor content is made higher to continue the decomposition reaction. After most of the active materials is decomposed, then liquid water may be added to complete the decomposition processing.
Instead of water vapor, alcohol vapor such as methanol, ethanol, propanol, butanol and the like is the alternative which can be used in processing alkali metals included in batteries at the initial stage. The alcohol reacts with alkali metals yielding hydrogen and alkali metal alkoxides. As solubilities of the alkoxides in alcohols are low, they cover the surface of the active materials as the processing advances. Accordingly, water vapor or mixture of water vapor and alcohol vapor may be supplied instead of the alcohol vapor. Water in the gas can decompose the alkoxide into alkali hydroxides and alcohols, which are very soluble into water. After most of the active materials is decomposed, liquid water may be added to complete the decomposition processing.
For safety reasons, it is preferred to control the hydrogen concentration. Preferably, the method includes controlling the hydrogen gas concentration in the chamber to below 4% by volume. The hydrogen concentration may be controlled by adjusting at least one of the rate of introduction of water or alcohol vapor into the chamber, the temperature in the chamber and the temperature of the introduced gas. Suitably, at least one of the water concentration in the gas and the temperature of the gas is increased during the treatment of the battery.
The method may include the step of contacting components of the battery with an aprotic solvent to remove electrolyte therefrom, before contacting the component containing alkali metal with the introduced gas.
The invention in its method aspect can also provide a method of treating a secondary battery comprising at least one component containing alkali metal, to extract alkali metal therefrom, comprising the steps of exposing the component containing alkali metal to a gas containing at least one of water vapor and alcohol vapor so as to form alkali metal hydroxide or alkoxide, and separating the alkali metal hydroxide or alkoxide from other constituents of the battery.
The step of separating the alkali metal hydroxide may comprise adding water to form a solution thereof and separating the solution from remaining solid constituents.
Yet further, the invention provides a method of converting an alkali metal in a secondary battery into alkali metal hydroxide or alkoxide by contacting the alkali metal with water, wherein the improvement comprises contacting the alkali metal with a gas containing at least one of water vapor and alcohol vapor, and controlling the hydrogen concentration by control of the supply rate of water vapor.
The invention also provides a method of converting alkali metal present in a secondary battery to alkali metal hydroxide, comprising exposing the alkali metal to a gas containing at least one of water vapor and alcohol vapor in a closed chamber and extracting hydrogen gas evolved in said chamber by reaction of the vapor with the alkali metal, so as to maintain a concentration of hydrogen gas in said chamber below a predetermined safe concentration thereof.
Apparatus according to the invention for treatment of a battery comprising a component containing an alkali metal, comprises means for opening an outer casing of the battery, a closable chamber to receive the battery, and means for introducing to said chamber a gas containing at least one of water vapor and alcohol vapor. Preferably there are means for separating alkali metal hydroxide formed by reaction with said alkali metal from solid components of the battery.
This apparatus may have a hydrogen concentration sensor for sensing hydrogen concentration in the chamber and means for adjusting the rate of introduction of the water vapor or alcohol vapor in dependence on the sensed hydrogen concentration. Further, it may have a temperature sensor for sensing temperature in the chamber and means for adjusting the rate of introduction of the water vapor or alcohol vapor in dependence on the sensed temperature.
In another aspect, the invention provides apparatus for treatment of a battery comprising a component containing an alkali metal, comprising means for opening an outer casing Of the battery, a closable chamber to receive the battery, means for introducing to the chamber a gas containing at least one of water vapor and alcohol vapor, a sensor for monitoring the reaction with alkali metal in said chamber and means for controlling the introduction of said gas in dependence on an output of said sensor. The sensor is preferably selected from (a) a pressure sensor for sensing pressure in the chamber, (b) a temperature sensor for sensing temperature in the chamber and (c) a hydrogen concentration sensor for sensing hydrogen concentration in the chamber.
In yet another aspect, the invention provides apparatus for treatment of a battery comprising a component containing an alkali metal, said apparatus comprising a closable chamber having a plurality of intercommunicating compartments comprising at least (a) a first compartment provided with means for opening an outer casing of said battery, and (b) a second compartment having means for introducing thereto a gas containing water vapor for reaction with said alkali metal.
The apparatus may include means for agitating, e.g. vibrating, the battery components during the treatment or means for stirring the battery components.
Further preferred and optional features of the invention and methods and apparatus of carrying it out will now be described generally.
To efficiently and safely decompose and recover active materials such as a battery active material and electrolytic solution contained in a high energy density battery, the battery is processed while controlling the decomposition rate of the target materials. The method of processing a battery according to the present invention has an advantage in that the decomposition rate of an active material of the negative electrode can be controlled by use of a processing gas containing the vapor of a material reactive with the active material, and further by adjusting at least one of the supply rate, concentration and temperature of the processing gas. As for the electrolytic solution, it may be separately recovered using a suitable cleaning liquid.
The battery processing apparatus of the present invention typically includes a processing chamber for processing an active material of a battery in a controlled atmosphere, which may be based on a dry inert gas, nitrogen gas or air. It is desirable to prevent the entrapment of an external water content in the processing chamber when a battery is moved between the processing chamber and the outside of the apparatus. For this purpose, there is proposed a method of using an inlet-chamber (lock chamber) capable of replacing the gas atmosphere from the atmospheric air with the dry gas by means of a vacuum pump. In this method, a port of the preparing chamber is first opened to move the battery into the inlet chamber; the port is closed to allow evacuation of the atmospheric air in the preparing chamber; dry atmospheric gas is introduced into the inlet chamber; and a port separating the inlet chamber from the processing chamber is opened to allow the battery to move into the processing chamber. In this method, since the processing chamber is not opened to the atmospheric air, the dry state in the processing chamber is maintained. Moreover, to improve the operability of the battery processing apparatus, to reduce the operational cost, and to shorten the battery processing time, there may be provided an inlet chamber having an air curtain mechanism of a dry gas at the entry port of the processing chamber, thereby maintaining the dry state of the interior of the processing chamber in a more simple manner as compared with the above-described gas replacement system.
Next, there will be described one preferred process of inactivating a high energy density battery containing an alkali metal. First, a battery is completely discharged outside the apparatus of the present invention. A suitable method of discharging the battery is by short-circuiting the terminals of the battery by way of a resistor or by dipping the battery in a solution containing sodium chloride or a dilute acid. In the latter method, the battery discharge is accompanied by corrosion of the battery casing so that a large number of small size batteries, of the AA size for example, may be treated together at one time. After being discharged in this way, the battery is carried into the processing chamber by way of the inlet chamber. A drive type transporting device such as a belt conveyor may be provided between the inlet chamber and the processing chamber for easy movement of the battery therebetween. The inlet chamber has a gas supply system and a gas exhaust system for communicating the dry atmospheric gas to the inlet chamber even when it uses either an air curtain system or gas replacement system. Moreover, to exhaust a combustible gas such as hydrogen gas generated in the inactivation of the battery or a harmful gas such as PF 5 from the processing chamber, the processing chamber has a gas supply system and gas exhaust system. While the humidity in the processing chamber is controlled, the battery components are exposed using a battery crusher, such as a hammer crusher, having a function of crushing the battery together with the casing, or a battery disjointing device, such as a grinder or a diamond cutter, having a function of cutting the casing of the battery and taking out the battery components. The processing chamber is connected to a supply system and exhaust system of a processing gas and liquid.
After the battery components are exposed inside or outside the battery casing, the electrolytic solution contained in the battery vessel, electrodes, separator and the like is removed using a cleaning liquid. As the cleaning liquid, there may be used an aprotic organic solvent such as propylene carbonate, 1,2-dimethoxyethane, diethoxyethane or the like. By distilling the waste cleaning liquid, the electrolyte can be recovered. Next, nitrogen gas, other inert gas (e.g. Ar or He) or air containing water or alcohol vapor in dilute form is introduced into the processing chamber, to gradually decompose the active material of the negative electrode.
The water content in the introduced gas is preferably in the range 0.5-2 g per litre, and the preferred temperature of the gas is in the range 100°-150 ° C. Relative humidity of the gas may be 80-100%. Alternatively, vapor of an alcohol such as methanol, ethanol, propanol and butanol is present in the gas. Preferable alcohol content in the processing gas is 0.5-5 g per litre. A mixture of water vapor and alcohol vapor (e.g. in the amounts given above), which is more reactive to alkali metal than the respective alcohol, is also useful in decomposition to alkali metals. The processing is performed by injecting the processing gas to the component. The processing gas may be introduced from the liquid supply system connected to the processing chamber. At the initial stage, the processing gas decomposes the negative electrode, and it may become less reactive to the electrode in the progress of the processing. In this case, liquid water or a liquid mixture of water and alcohol is sprayed or dropped onto the negative electrode. These liquids are introduced from the supply system of the processing gas, if the vapor generator is switched off. The spent processing gas is exhausted from the processing chamber by way of the liquid exhaust system.
The concentration of hydrogen gas generated during the processing of the negative electrode desirably should for safety reasons be less than the explosion limit, preferably 4% or less. The hydrogen gas accumulating in the processing chamber is readily exhausted from the processing chamber together with the inert gas, nitrogen gas or air introduced into the processing chamber. A gas separator is mounted in the gas exhaust system for recovering hydrogen gas.
For execution of the above described process, there may be used apparatus having a processing chamber and including: a processing gas supply system having storage vessels storing a plurality of processing materials, supply ports for processing gas, and a waste liquid exhaust system having exhaust ports for the spent processing liquids and waste liquid storage vessels. For processing the negative electrode using water vapor, a humidifying device having a function for controlling the water vapor concentration is mounted in the processing gas supply system. Gas flow rate control means are provided. A plurality of gas supply ports may be provided in the processing chamber; or supply ports for introducing different processing gases to a plurality of processing chambers may be provided in a plurality of the processing chambers, to process the batteries using processing gases which are different in reactivity in a stepwise manner from each other. The gas supply means may apply liquids, when the gas supply is stopped.
The automation of the operation of the above-described battery processing apparatus is desirable to improve the efficiency and safety of the processing of the battery. To automate the apparatus, there are provided for example a flow rate controller for controlling the supply amount and exhaust amount of processing gas; a sensor for measuring the pressure, temperature and hydrogen concentration in the processing chamber; and an arithmetic and control unit for controlling the flow rate controller of the processing gas according to the state of the processing chamber monitored by the sensor. The flow rate controllers may be provided in the supply pipe and exhaust pipe connected to the inlet chamber and the processing chamber. The sensor is provided in the processing chamber, and may include a temperature sensor, infrared ray sensor or hydrogen sensor. The measured data such as the temperature and the hydrogen concentration in the processing chamber are transmitted from the sensor to the arithmetic control unit. The arithmetic and control unit operates the flow rate controllers and vapor generators according to the analyzed result of the measured data for adjusting the supply amount and exhaust amount of the processing gas or liquid, and the temperature of the gas and the vapor content, as desired. When an abnormal decomposition rate occurs midway in the processing of the battery, the introduction of the processing gas may instantly be stopped or a large amount of an inactive liquid may be added to the active material being decomposed, to suppress the decomposition. Moreover, it is possible to easily exhaust the combustible gas such as hydrogen which maybe excessively generated, through the exhaust system. By incorporating such a controlling system in the apparatus, the operation of the battery processing apparatus can be automated, thus improving the efficiency and safety of the decomposition process of the battery.
Various materials can be recovered from the solutions produced by the methods of the invention. Alkali metal can be extracted from the hydroxide by distilling to obtain oxide, followed by electrolysis. Electrolyte may be recovered by vacuum distillation. Other metals such as Co, Ni, Fe and Al can be recovered from the battery components also, by processes such as incineration, reduction and electrolysis.
The cost required to recover valuable materials from the waste liquid in processing of the battery is dependent on the concentration of the target material contained in the waste processing liquid exhausted from the battery processing apparatus. For recovering the target material from the waste liquid having a low concentration, a process of enriching the waste liquid by extraction or distillation is required, which increases the recovery cost. In the present invention, it becomes possible to fractional-recover the waste processing liquid exhausted from the battery processing chamber, to enrich only the processing liquid low in the concentration of the valuable material, and to recover the valuable material from all the waste processing liquid. Materials which may be recovered are alkali metals and transition metals such as Fe, Ni, Mn, Co. Alkali metal may be obtained by extraction and electrolysis, while transition metals may be obtained by various metallurgical processes such as incineration, reduction and electrolysis. The battery processing apparatus of the present invention makes it possible to fractional-recover the waste processing liquids of valuable materials having different concentrations, and to reduce the cost in regenerating the valuable materials.
In the case of using water vapor as a reactive material for decomposing the negative electrode, a carrier gas such as an inert gas, nitrogen or air mixed with water vapor is contacted with the negative electrode, to decompose the active material of the negative electrode. When using water and alcohol vapors, the contents in the carrier gas may be controlled by varying the mixing ratio of alcohol and water. At the initial stage of decomposition, the concentration of water and/or alcohol vapor is kept low to reduce the reactivity of the processing, thus suppressing the abrupt decomposition of the active material of the negative electrode. As the decomposition proceeds, decomposition products such as alkoxides become deposited on the surface of the component. By increasing the water and/or alcohol vapor concentration as the decomposition rate of the negative electrode is lowered, the reactivity of the gas is increased and decomposition of the negative electrode is continued. Finally, liquid water may be directly contacted with the negative electrode, thus completing the decomposition and solution of the alkali metal as hydroxide. This method is effective to reduce the cost of the processing liquid and to reduce the environment load due to the waste processing liquid.
The processing gas may initially contain an alcohol, or the alcohol may be included after an initial period when water vapor only is present in the processing gas. The water vapor reacts to generate alkali metal hydroxide. If a solution is produced in the chamber, it may be removed as it is, or water may be added, when the reactivity of the battery residue is much reduced, to form a solution to be withdrawn.
INTRODUCTION OF THE DRAWINGS
Embodiments of the invention will now be described by way of non-limitative example, with reference to the accompanying drawings, in which:
FIG. 1 is a diagrammatic view of a lithium battery processing apparatus including ports with a sliding type door according to one embodiment of the present invention.
FIG. 2 is a diagrammatic view of a lithium battery processing apparatus in which the processing chamber is partitioned by a partitioning plate according to another embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the several drawings, the same reference numerals identify the same or corresponding elements.
FIG. 1 shows a battery processing apparatus of the present invention, which includes a processing chamber 1 and inlet and outlet chambers 2a and 2b respectively connected to opposite sides of the processing chamber 1. The processing chamber 1 and each of the chambers 2a and 2b have outer sizes of 1 m×1 m×2.5 m and 0.5 m×0.5 m×1 m, respectively. Ports 3a and 3b, each having an opening/closing plate, are respectively mounted at the outer side of the chambers 2a and 2b for maintaining the air-tightness of the chambers 2a and 2b. Ports 4a and 4b, each having an opening/closing plate, are provided between the chambers 2a and 2b and the processing chamber 1. A belt conveyor indicated at 5 is provided within this apparatus for transporting a battery, battery components and the like. Three sets of gas supply systems including a gas supply device 6 for drying and supplying an atmospheric gas, gas supply pipes 7a, 7b and 7c, and valves 8a, 8b and 8c are connected to the processing chamber 1 and the inlet and outlet chambers 2a and 2b. In this embodiment, as the atmospheric gas, nitrogen gas is used.
To recover the hydrogen gas generated in the processing chamber 1 during the processing of a battery, the gas in the processing chamber 1 is transported to a gas separator 9 by way of a gas exhaust pipe 10 having a valve 8d. The hydrogen is separated from the gas at the gas separator 9, and is recovered in a gas storage vessel 14 connected to a transporting pipe 13 having a valve 8f. To store hydrogen gas, a hydrogen storage alloy such as LaNi 5 is present in the gas storage vessel 14. The nitrogen gas remaining in the gas separator 9 is transported to the gas supply device 6 by way of a transporting pipe 11 having a gas transporting pump 12 and a valve 8e. Upon decomposition of a negative electrode, nitrogen is circulated by opening the valves 8b, 8d and 8e and continuously driving the pump 12.
The apparatus has means 21b for supplying humidified air via a flow rate control valve 22b, an optional liquid pump 23b through a pipe 25b and via a heater 29 to an injector 24b in the processing chamber. The water vapor content of the air can be adjusted. This arrangement is also capable of supplying liquid water. Alternatively, separate means for supplying humidified gas and liquid water respectively may be provided.
EXAMPLE 1
In this example, five 3 Wh lithium secondary batteries are processed, each of which includes a positive electrode made of LiCoO 2 , a negative electrode made of a lithium-lead alloy, and an electrolyte made of an organic electrolytic solution containing LiPF 6 . The battery has a cylindrical shape having a diameter of 18 mm .o slashed. and a length of 65 mm. First, outside the battery processing apparatus shown in FIG. 1, each battery was short-circuited by way of a resistor of 10Ω to be perfectly discharged. The port 3a was opened, and each battery 15 was placed on the belt conveyor 5 in the inlet chamber 2a, after which the port 3a was closed. The valve 8a was then closed and a valve 17a mounted in a gas exhaust pipe 16a was opened.
After that, an exhaust pump 18a was operated, to evacuate air present in the inlet chamber 2a. After the inlet chamber 2a was evacuated, the valve 17a was closed and the pump 18a was stopped. Next, dry nitrogen gas was supplied to the inlet chamber 2a by way of the gas supply pipe 7a. The port 4a was then opened, and the batteries 15 were moved to the processing chamber 1, after which the port 4a was closed.
The casing of the batteries was crushed in the processing chamber 1 by means of a battery crusher 19 including a hammer crusher and a cutter mixer. The crushed pieces were stored in a polypropylene vessel 20 having its bottom surface provided with a polypropylene fibre mesh material as a filter. The time required for crushing was 20 min.
In this example, 1,2-dimethoxyethane is used for cleaning the electrolytic solution adhering to the battery crushed pieces. A liquid storage vessel 21a, in which 1,2-dimethoxyethane is stored, is connected to the processing chamber 1 by means of a pipe 25a including a valve 22a, a liquid transporting pump 23a and a sprayer 24a. 1,2-dimethoxyethane in an amount of 1 litre was sprayed onto the battery crushed pieces stored in the vessel 20 at a rate of 100 ml/min, to clean the electrolytic solution from the battery pieces. The bottom surface of the processing chamber 1 was formed in a conical shape at two portions for collecting the cleaning liquid supplied from the sprayer 24a. The collected cleaning liquid was stored in a waste liquid storage vessel 28a by way of a processing liquid exhaust pipe 27a having a valve 26a.
Next, the belt conveyor 5 was driven, and the vessel 20 was carried to a portion under the injector 24b.
A telescopic joint capable of adjusting height was mounted on the liquid supply pipe 25b and the injector 24b was attached at the leading end thereof. The injector 24b was moved to be close to the vessel 20 containing the crushed battery pieces, and it injected air at 100° C. containing water vapor with a humidity of 90% to the crushed pieces at a rate of 1000 ml/min. Water bubbles were gradually generated from the crushed pieces, to thus decompose the active material of the negative electrode.
After an elapse of 25 min, the heater 29 heated the humidified air to 150° C. The humidified air was then further injected onto the crushed pieces for 30 min at the same rate. Next, the supply of the humidified air from means 21b was stopped, and only water was supplied from the means 21b, so that water was added to the battery crushed pieces by the pump 23b at a rate of 100 ml/min. The waste water was stored in the waste liquid storage vessel 28b by way of the pipe 27b. After an elapse of about 15 min, the desired decomposition of the crushed pieces was completely finished, and the battery crushed pieces were then taken from the preparing chamber 2b as described below.
The hydrogen gas generated during treatment of the batteries was exhausted to the gas separator 9 by way of the gas exhaust pipe 10 together with air. The hydrogen gas recovered by the gas separator 9 was stored in the storage vessel 14 including LaNi 5 alloy by way of the pipe 13 having the valve 8f which was opened, and was stored in the storage vessel 14 including LaNi 5 alloy. The gas remaining in the gas separator 9 was returned to the gas supply device 6 by way of the pipe 11.
To remove the residue of the batteries, the atmospheric air in the chamber 2b was exhausted by a gas exhaust system including a valve 17b, a pump 18b and a gas exhaust pipe 16b. The valve 17b was then closed, after which the valve 8c was opened and dry nitrogen was introduced into the outlet chamber 2b by way of the gas supply pipe 7c. After the chamber 2b was filled with dry nitrogen, the plate of the port 4b was opened, and the vessel 20 was moved into the outlet chamber 2b. The plate of the port 4b was closed and the plate of the port 3b was then opened, and thus the vessel 20 containing the crushed pieces was taken from the chamber 2b.
The waste water stored in the waste liquid storage vessel 28b was distilled and the lithium metal was recovered by electrolytic refining. Lithium was recovered from the crushed residue by extraction and electrolysis. The recovered ratio of lithium was 95% based on the total amount of lithium contained in five cylindrical lithium secondary batteries.
From the 1,2-dimethoxyethane solution of LiPF 6 stored in the waste liquid storage vessel 28a, LiPF 6 was recovered by vacuum distillation.
EXAMPLE 2
50 cylindrical lithium secondary batteries each having the same specification as those processed in the Example 1, were previously discharged in a salt water containing sodium chloride or the like and processed in the battery processing apparatus shown in FIG. 1. First, each lithium battery was dipped for two days in a salt water containing sodium chloride in an amount of 50 g per 21 of water. By this, part of the battery vessel was corroded. Each battery was carried into the processing chamber 1 by the same procedure as in Example 1, and was crushed using the battery crusher 19 having the hammer crusher and the cutter mixer. The crushed pieces were then stored in the polypropylene vessel 20 having the bottom surface provided with the mesh. The time required for crushing the batteries was 20-23 min. The batteries in the number being 10 times that of the batteries in the Example 1 were crushed for about the same time. As in this embodiment, by corroding the vessel of the batteries in a solution containing a salt such as sodium chloride or potassium chloride or a diluted hydrochloric acid, the time required for crushing of batteries could be shortened even when the number of the batteries was increased. 1,2-dimethoxyethane stored in the liquid storage vessel 21a was added to the battery crushed pieces for 20 min at a rate of 100 ml/min, to clean the electrolytic solution stuck on the crushed pieces. The waste cleaning liquid was stored in the waste liquid storage vessel 28a. Subsequently, water stored in the liquid storage vessel 21b was heated at the heater 29 to produce an air-water vapor mixture gas containing 0.5 g water per 1 l at 100° C. The gas was injected onto the crushed pieces of the batteries at a rate of 1 l/min for 40 min. During decomposition of lithium-lead alloy particules in the crushed materials, the hydrogen concentration in the processing chamber was kept below 0.5% or less. No evolution of hydrogen from the crushed pieces was observed after supplying the gas for an elapse of 60 min. Finally 1 l of liquid was added to the crushed pieces to terminate decomposition of the lithium alloy. In this example, the total time required for processing fifty 3 Wh lithium secondary batteries 15 was about 1.8-2.0 hr. The volume of aqueous liquid containing lithium ions recovered in the waste liquid storage vessel 28b was 0.8-0.9 l. By electrolytic refining, 20% of lithium metal contained in the original lithium batteries was recovered. From the residue obtained from the vessel 20, lithium cobalt, iron, and aluminium was re-generated by incineration and reduction or electrolysis. Nearly 85% of the total amount of lithium metal in the lithium batteries was recovered. The regenerated amounts of cobalt, iron and aluminium were 75˜80% of the amounts initially contained in the batteries. From the 1,2-dimethoxyethane solution of LiPF 6 remaining in the waste liquid storage vessel 28a, 93% of LiPF 6 was recovered by vacuum distillation.
EXAMPLE 3
Using five pieces of the lithium batteries having the same specification as those in the Example 1, an experiment was made to shorten the time required for processing the batteries. 1,2-dimethoxyethane was used as a cleaning liquid for recovering an electrolytic solution of the batteries. Each battery was crushed using the battery crusher 19 having the hammer crusher and the cutter mixer in the same procedure as in the Example 1. The crushed pieces were stored in the polypropylene vessel 20 with a polypropylene filter. 1,2-dimethoxyethane in an amount of 1 l was added to the crushed battery components at a rate 100 ml/min from the sprayer 24a. The waste cleaning liquid was stored in the waste liquid storage vessel 28a. The vessel 20 containing the battery crushed pieces was placed directly under the injector 24b. First, in such a state that the heater 29 was operated, gas at 150° C. was injected onto the battery crushed pieces at a rate of 1 l/min from the injector 24b using nitrogen gas carrier. Water content was 1 g per litre. The time required for supplying the processing gas was 30-35 min. The hydrogen concentration in the processing chamber 1 during the processing of the negative electrode was 1% or less, and accordingly the negative electrode could be safely decomposed without the fear of explosion of hydrogen. Water in liquid form was added to complete the decomposition. The waste liquid stored in the waste liquid storage vessel 28a was distilled in vacuum, and thereby 95% of the total LiPF 6 contained in the batteries was recovered. The waste liquid stored in the waste liquid storage vessel 28b was subjected to electrolytic refining, to recover 25% of the total lithium metal contained in the batteries. From the residue obtained from the vessel 20, lithium, cobalt, iron, and aluminium was regenerated by incineration and reduction or electrolysis. Nearly 83% of the total amount of lithium metal in the lithium batteries was recovered. The regenerated amounts of cobalt, iron and aluminium were 75˜80% of the amounts initially contained in the batteries.
EXAMPLE 4
The battery processing time may be shortened by agitating crushed battery components during supply of the gas. Five pieces of the lithium secondary batteries having the same specification as those in Example 1 were processed. Each lithium battery was discharged through a resister of 10Ω and was crushed using the battery crusher 19 having the hammer crusher and the cutter mixer in the processing chamber 1. The crushed pieces were put in the polypropylene (PP) vessel 20 with the PP filter. They were cleaned with 1,2-dimethoxyethane supplied from the liquid storage vessel 21a. The processing gas contains water vapor at 0.5 g/l at 100° C. It was supplied from the nozzle 24b to the crushed pieces of batteries in the PP vessel 20. The flow rate of processing gas was 1 l/min. Next, a rotary mixer was inserted in the vessel 20 containing the battery crushed pieces, and the pieces were agitated. After the generation of hydrogen was no longer observed from the crushed pieces, the liquid product was discharged from the vessel 20 to the waste liquid storage vessel 28b by way of the liquid exhaust pipe 27b. Finally, 1 l of water at 25° C. was added to the crushed pieces from the nozzle 24b, after the steam generator 29 was switched off. The decomposition time by the gas was 18-20 min, and the total battery processing time was 1.3-1.4 hr. The battery processing time was shortened compared with Example 1 by the agitation of the crushed component. The waste liquid stored in the waste storage vessel 28a was distilled in vacuum, so that 95% of the total LiPF 6 contained in the batteries was recovered. The waste processing liquid stored in the waste liquid storage vessel 28b and the residue of the crushed battery pieces was subjected to electrolytic refining, to recover 80% of the total lithium metal contained in the batteries.
In FIG. 1 a hydrogen sensor 30 having a function of detecting the hydrogen concentration in the processing chamber 1 is provided in the processing chamber 1. The hydrogen sensor 30 was connected to an arithmetic and control unit 32 though a signal input cable 31. The arithmetic and control unit 32 is connected to the flow rate adjuster 22b and the liquid supply pump 23b by means of signal input cables 33a and 33b, respectively. The hydrogen sensor 30 measures the hydrogen concentration in the processing chamber 1, and transmits an electric signal proportional to the measured value to the arithmetic and control unit 32. The arithmetic and control unit 32 calculates the electric signal supplied from the hydrogen sensor 30, and transmits the electric signal corresponding to the processing result to the flow rate adjuster 22b or the liquid supply pump 23b for controlling their operation. In this embodiment, the allowable value of hydrogen concentration and the total supply amount of the processing gas are previously stored in a memory unit of the arithmetic and control unit 32, and the calculating condition of the arithmetic and control unit 32 may for example be in accordance with the following items (1) to (5) singly or in combination.
(1) When the hydrogen concentration in the processing chamber 1 is smaller than the allowable value, the arithmetic and control unit 32 controls the flow rate adjuster 22b for increasing the supply rate of the processing gas. In this embodiment, the permitted hydrogen concentration in dry gas is within the range from 0 to 4%.
(2) When the average hydrogen concentration in the processing chamber 1 is less than 0.01% for a selected period, e.g. in the range 1 to 5 minutes, the supply of processing gas or liquid is stopped.
(3) When an electric signal transmitted from the hydrogen sensor 30 to the arithmetic and control unit 32 is abruptly increased to more than a hydrogen concentration allowable value, the flow rate adjuster 22b and pump 23b are closed by way of the signal input cables 33a and 33b, to stop the processing supply. The hydrogen concentration allowable value in this case may be set at 10%.
(4) The arithmetic and control unit 32 accumulates the supply amount of the water and the accumulated value is stored in the memory unit of the arithmetic and control unit 32.
(5) When the accumulated value in (4) reaches the upper limit of the total supply amount of the processing water stored in the memory unit of the arithmetic and control unit 32, the flow rate adjuster 22b and pump 23b are closed.
EXAMPLE 5
The apparatus shown in FIG. 1 was operated under the control conditions described above. Five lithium batteries 15 of the same specification as those in Example 1 were crushed in the battery crusher 19 and the electrolyte was cleaned off as in Example 1. Then the active materials of the negative electrodes were decomposed with the water vapor containing gas. The gas contained water of 0.5 g/l at 100° C., and the carrier gas was nitrogen. It was supplied from the nozzle 24b to the crushed pieces of the batteries. The processing time was 25 min. After this treatment, water (1 l) was added to the pieces from nozzle 24b. The water amount supplied from the liquid storage vessel 21b was 41. The total time required for putting the batteries in the processing apparatus and taking the battery crushed pieces from the processing apparatus was 1.4-1.5 hr. The waste cleaning liquid stored in the waste liquid storage vessel 28a was distilled in vacuum, so that 95% of the total LiPF 6 of the batteries was recovered. The water processing liquid stored in the waste liquid storage vessel 28b was subjected to electrolytic refining, and 23% of the total lithium metal of the batteries could be recovered. Metallurgical methods such as extraction and reduction recovered 60% lithium from the crushed pieces. In this embodiment, as compared with Example 1, it becomes possible to shorten the battery processing time, and to automate the battery processing allowing unmanned operation.
In a variation of the embodiment of FIG. 1, to shorten the battery processing time, the preparing chambers 2a and 2b each have an air curtain mechanism. The ports 3a, 3b, 4a and 4b include sliding type opening/closing plates. In this apparatus, the gas storage vessel 6 was replaced by a supply device 6 for usually supplying dry air to the processing chamber 1 and the preparing chambers 2a and 2b. Moreover, the gas exhaust pumps 18a and 18b were not required. When the port 3a was opened, dry air was supplied from the dry air supply device 6 to the preparing chamber 2a. The dry air was discharged to the exterior of the apparatus through the gas exhaust pipe 16a by opening of the valve 17a. With this air curtain mechanism, humidified air outside the apparatus was not permitted to enter the processing chamber 1. Even when the processed battery components were taken from the preparing chamber 2b, dry air was supplied from the dry air supply device 6 to the preparing chamber 2b, and was communicated to the gas exhaust pipe 16b by opening of the valve 17b.
EXAMPLE 6
Five lithium batteries of the same specification as in Example 1 were processed in the modified apparatus just described, by the procedure of Example 3. The time required for the processing of the negative electrode by gas containing water vapor was 25-30 min as in Example 3, and the time required for crushing of the batteries was the same as in the Example 3. The hydrogen concentration in the processing chamber 1 during reaction between ethanol and the battery crushed pieces was maintained at 1% or less. In this embodiment, the gas replacement in the inlet and outlet chambers 2a and 2b was eliminated, thus shortening the total processing time to be 1 hr.
FIG. 2 is a battery processing apparatus in which two sets of processing fluid supply systems and liquid exhaust systems are independently provided. A partitioning plate 34 is provided in the upper portion of the processing chamber 1 to provide two working areas and sprayers 24a and 24b are provided in the upper portion of the processing chamber 1. Diethoxyethane for cleaning electrolytic solution is stored in a liquid storage vessel 21a, and is introduced from the sprayer 24a to the first compartment of the processing chamber 1 by way of a liquid transporting pipe 25a having a valve 22a and a pump 23a. Ethanol and water are stored in vessels 21b and 21c and are supplied with a carrier gas (dry air) for decomposing a negative electrode from the injector 24b to the second compartment of the processing chamber 1 by way of pipe system 25b having valves 22b and 22c and pump 23b and 23c. The supply means 21b can also supply water vapor only in air, if required. For example a mixture of 50% ethanol and 50% water by weight is supplied. The liquid supply means 21b and 21c have the capability of generating vapors of the liquids by heating.
To individually recover the cleaning liquids or processing liquids used in the partitioned areas, two portions of the bottom surface of the processing chamber 1 were formed in a conical shape, and two waste liquid exhaust pipes 27a and 27b are connected to the two portions. As another method of recovering waste liquids, a partitioning plate is arranged on the bottom surface of the processing chamber 1 under the belt conveyor 5, so that the waste liquids can be fractional-recovered without any mixing of the waste liquids. Valves 26a and 26b control the waste liquid exhaust pipes 27a and 27b, respectively. Dry air to be supplied to the processing chamber 1 and the inlet/outlet chambers 2a and 2c was introduced to the apparatus from a gas supply device 6 having a function of drying air. The dry air was continuously supplied from the gas supply device 6 to the chambers 2a and 2b of the battery processing apparatus by way of a pipe 7a, and was exhausted from a gas exhaust pipe 16a by opening of the valve 17a.
EXAMPLE 7
The lithium battery used in this example is a square lithium secondary battery including a positive electrode made of LiCoO 2 , a negative electrode made of carbon electrochemically absorbing and releasing lithium ions, and an electrolyte made of organic electrolytic solution in which LiPF 6 is dissolved in a mixture of 50 vol % of ethylene carbonate and 50% vol of 1,2-dimethoxyethane. The battery has a size of 50 mm×80 mm×40 mm, and a rating capacity of 30 Wh. In this embodiment, five of these batteries were processed. First, each battery 15 was discharged using a resistor of 10Ω outside the battery processing apparatus shown in FIG. 2. The sliding plate 3a of the inlet chamber 2a was opened, and each battery 15 was placed in the chamber 2a. The plate 3a was closed and the plate 4a was opened, and the batteries 15 was carried into the processing chamber 1. A battery disjointing machine 19 having a diamond cutter and a cutter mixer was provided in the processing chamber 1. The upper portion of each battery vessel was cut using the diamond cutter of the battery disjointing machine 19. The upper portion of each battery 15 was removed, and battery components were taken out from the battery vessel.
The electrolytic solution on a separator, the battery vessel and electrodes was cleaned by 1,2-dimethoxyethane supplied from the sprayer 24a. The waste cleaning liquid was stored in a waste liquid storage vessel 28a by way of a liquid exhaust pipe 27a. The cleaned negative electrode was finely cut using the cutter mixer of the battery disjointing machine 19, and was stored in the PP vessel 20 having the bottom surface provided with a PP filter. The other battery members were placed on a belt conveyor 5 as they were. The belt conveyor 5 was driven, and the vessel 20 was moved directly under the nozzle 24b. The nozzle 24b provided the air containing ethanol and water vapor at 50/50% weight ratio (total 0.5-3.0 g/l) at 3 l/min to the negative electrode in the vessel 20. The processing time was 50 min.
The hydrogen concentration in the processing chamber 1 was 3% or less. After an elapse of about 40 min from the start of the processing, hydrogen was difficult to be generated as lithium alcoholate (alkoxide) with white color was precipitated, and the hydrogen concentration in the processing chamber 1 was 0.1% or less. After the supply of the ethanol + water vapor was stopped, the flow rate controller 22c was stopped, and only the air containing water vapor at 0.5 g/l was added to the negative electrodes from the nozzle 24b. The flow rate of air was 3 l/min. This processing time was 30 min. Finally, the air flow was switched off, and water (51) was supplied to the crushed pieces of the batteries.
The plate 4b was opened, and the vessel 20 and the electrode members were carried into the outlet chamber 2b. The plate 4b was closed and the plate 3b was opened, for removal of all of the processed battery components. The total time required for processing of the five batteries was 2.2-2.3 hr. The total volumes of the ethanol and water used in the processing of the negative electrodes were about 0.51 and 61, respectively. In all of the processes of this embodiment, the hydrogen concentration in the processing chamber 1 was suppressed to be 3% or less. The waste liquid in the waste liquid storage vessel 28a was distilled in vacuum, so that 95% of the total LiPF 6 contained in the five batteries could be recovered. The waste liquid obtained in the waste liquid storage vessels 28b was distilled, so that 30% of the total lithium contained in the batteries was recovered by electrolytic refining. From the crushed pieces obtained after the deactivation of negative electrodes, lithium was reproduced by extraction and reduction. The lithium amount was 55% of the total amount of lithium included in the batteries.
A battery having energy capacity being 10 times that of the lithium secondary battery processed in FIG. 1 can be continuously processed using the battery processing apparatus shown in FIG. 2. The processing time for each battery can be short, and the hydrogen generated upon processing was recovered in a produced gas storage vessel 14 containing LaNi 5 alloy, thereby ensuring the safety of the process. The waste processing liquids from respective processing chambers can be stored in separate tanks. This makes it possible to regenerate the electrolyte and lithium by fractional-recovering them, to simplify the distillation of the waste liquid stored in the waste liquid storage vessel 28b containing lithium ions of a high concentration, and to reduce the cost required in the process of enriching the waste liquid by the fractional-recovery.
EXAMPLE 8
A cylindrical 3 Wh lithium secondary battery including a positive electrode made of V 6 O 13 , a negative electrode made of Li metal, and a solid high molecular electrolyte made of a mixture of polyethylene oxide and LiCF 3 SO 3 was processed using the battery processing apparatus shown in FIG. 2. In the same procedure as in the Example 6, five of the lithium secondary batteries were carried into the processing chamber 1, and were crushed using the battery crusher 19 having the hammer crusher and cutter mixer. The crushed pieces were put in the PP vessel 20 having the bottom surface provided with the PP filter. 1,2-dimethoxyethane stored in the liquid storage vessel 21a was sprayed from the sprayer 24a onto the crushed pieces. The waste cleaning liquid was stored in the waste liquid storage vessel 28a by way of the liquid exhaust pipe 27a. The vessel 20 was then moved directly under the nozzle 24b by the belt conveyor 5, and the nozzle 24b injected the ethanol and water vapor as used in Example 6 onto the crushed pieces in the vessel 20. The processing time was 20 min. After 15 min the hydrogen generating rate was decreased. Then air containing 0.5 g water in 1 l was supplied from the nozzle 24b. The unreacted alloy contained in the negative electrode was started to be decomposed, and hydrogen was generated. The processing time was 20 min. The waste liquid in the waste liquid storage vessel 28a was distilled in vacuum, so that 90% of the total LiPF 6 contained in the five batteries was recovered. The waste liquid obtained in the waste liquid storage vessel 28b was distilled, and 25% of the total lithium contained in the batteries was recovered by electrolytic refining. The recovered lithium from the crushed battery pieces was 57-60% of the total amount.
While the invention has been illustrated by several embodiments, it is not limited to them, and many variations, modifications and improvements are possible, within the scope of the inventive concept. | A safe and controllable method of treating a secondary battery having at least one component containing alkali metal, comprises the steps of opening the battery casing, and introducing a gas containing at least one of water vapor and alcohol vapor into a closed chamber containing the battery thereby to form alkali metal hydroxide. To control hydrogen concentration, the rate of introduction of water and/or alcohol vapor may be varied. Apparatus for carrying out this method is also described. | 8 |
This is a continuation-in-part of application Ser. No. 06/274,519, filed June 17, 1981 now abandoned.
BACKGROUND OF THE INVENTION
Underwater gear, such as instruments, bottom sampling equipment or fish traps, has to be moved frequently over the sea bed, and this invention provides a means of doing this without having to use a boat.
SUMMARY OF THE INVENTION
The invention consists of an inflatable float, with timer means of controlling its inflation and deflation. A hydrofoil moves the gear laterally in the course of its vertical movements, one method of timing control uses tidal movements, and there may be a chemical source of gas for inflation.
BRIEF DESCRIPTION OF THE DRAWINGS
In the accompanying drawings of the preferred embodiment, FIG. 1 is an elevation view of the float system with a section of the float chamber.
FIG. 2 is a plan view on the section line A--A, illustrating one system of controlling inflation of the float.
FIG. 3 is a sectional elevational view, taken on the line B--B, showing a typical corrodable link and cam of the control system of FIG. 2.
FIG. 4 is an elevational view of part of the valve control mechanism of the gas source, with the flooding valve of the float chamber shown in section.
FIG. 5 is an elevational view of the same valve mechanism in the direction C--C.
FIG. 6 is a plan view of a hydrofoil sinker.
FIG. 7 is an elevational view of the same.
FIG. 8 is an elevational view with sectional detail, of the float system when controlled by a timer which is responsive to tidal movements.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In FIG. 1, 1 is a cylinder containing air under pressure, held in a frame 2 by retaining pin 3. A string of fish traps, for example, can be attached to frame 3 at lug 4.
The upper end of frame 2 is attached to pressure-resistant float chamber 5, which contains an inflatable bladder 6. Valve 7 controls the release of air from cylinder 1, and is actuated by arcuate movement of arm 8. Valve 10 is a standard item, actuated by ambient water pressure so as to control the deflation of bladder 6. Normally, valve 10 will open when ambient water pressure equals atmospheric pressure, that is, when the system reaches the surface. However, it can be set to operate at any desired ambient water pressure, that is, when the system has risen to any desired depth. Air passes from cylinder 1 to bladder 6 through tube 11.
Water can enter and leave chamber 5 through flooding valve 12, to the underside of which is fixed fork 13 which straddles arm 8.
As shown in FIG. 4, compression spring 14 normally keeps valve 12 in the open position. The relationship between fork 13 and arm 8 is shown in detail in FIG. 5. Rotatable stem 16 of valve 7 in housing 15, is fixed at right angles into arm 8 at its mid-point. Pin 17 in arm 8 helps to keep arm 8 and fork 13 in their correct relative positions.
In FIG. 3, cam 18 can move along guide rods 19,19 under the influence of tension spring 20, unless restrained by corrodable link assembly 21. The movement of cam 18 is such that it displaces arm 8 in passing it, but at the end of its travel is completely clear of arm 8. An array of such cams, springs and links is mounted in frame 22, which in turn is mounted on frame 2. Cams on opposite sides of valve stem 16 also act on opposite surfaces of arm 8, as shown in FIG. 2, so that the force of every cam, irrespective of its position in the array, always acts so as to turn arm 8 arcuately in the same direction, which rotates valve stem 16 to open valve 7.
In FIGS. 6 and 7, hydrofoil section 23 has attached to it booms 24, 24, carrying tailplane 25, 25 and vertical fins 26, 26. Mounting bracket 27 attaches rope 28 to section 23.
In operation, a string of items of gear such as fish traps on line 28, attached at one end to the float at lug 4, and at the other end to the hydrofoil sinker at bracket 27, is laid on the sea bed from a boat in the usual way. Since the float is not operating, chamber 5 will be filled with water and bladder 6 will be compressed into a small volume by the pressure of this water. After a predetermined time, the corrodable link 21 with the shortest life will fail, permitting its associated cam 18 to move under the force of spring 20. The resulting displacement of arm 8 turns valve stem 16, which opens valve 7 to permit air to pass from cylinder 1, through tube 11, to inflate bladder 6. When the pressure in bladder 6 exceeds that of the water outside the chamber, it presses upon flooding valve 12 and closes it. This causes fork 13 to move downwards on to arm 8 and restore it to its starting position, which movement closes valve 7. With water displaced from the chamber, this now rises towards the surface, carrying the gear and hydrofoil sinker with it. As it rises, the external water pressure drops and when this reaches the level where valve 10 is actuated, air is released from bladder 6, and water re-enters chamber 5 through flooding valve 12, causing the entire system to sink again.
Because of its hydrofoil construction, however, the sinker does not fall vertically downwards, but "glides", thus pulling the attached gear horizontally. The gear will therefore land on a different part of the sea bed to that from which it was lifted by the float. After a further predetermined time the next corrodable link breaks to inaugurate a second cycle of lift and gliding fall, and so on until all links in the array have broken. For retrieval, the system may have a conventional marker float and line attached to it, or, for compactness, the marker float line may be held on a reel whose unwinding is controlled by a corrodable link assembly in which the link has a longer time to failure than the longestlasting link in the release array.
It will be clear that the mechanism of bladder 6, valve 12, fork 13, arm 8 and valve 7, for isolating the gas source from the bladder, requires no setting for any particular depth. It will always operate as soon as pressure in the bladder exceeds ambient water pressure, whether this is high or low. Ignoring the small pressure required to overcome the force of spring 14, this means that the isolating mechanism can operate down to a depth where the ambient water pressure equals the residual pressure in the gas source after charging the bladder. It can also operate when ambient water pressure is at its lowest, i.e. when the apparatus is at the surface, where pressure is atmospheric for all practical purposes, and at any intermediate depth.
In certain locations it may be possible to use the periodicity of the tides as a timer, instead of corrodable links, and this is illustrated in FIG. 8. In this version, bearing 29 is mounted on top of chamber 5 so that it can pivot in a horizontal plane around axle 30. Bearing 29 carries one arm of crank 31, the free arm having fixed to it, slightly buoyant reaction surface 32. Crank 31 is drivably connected to valve stem 16 of cylinder 1 through flexible shaft 33 and ratchet or free-wheel clutch 34. When this system is dropped on to the sea bed in a tidal current, the force of the current on reaction surface 32 pulls this over in the current direction, and aligns the free arm of crank 31 in the plane of the current flow by pivoting bearing 29 about axle 30. From then onwards, crank 31 will move reciprocally with the reversals in the tidal flow, and act upon valve stem 16. The effect of free-wheel clutch 34 is to use movement in one direction only and to prevent a movement being cancelled by a reverse movement of the crank. Each tide therefore results in a quarter turn of valve stem 16, and this valve can be arranged to open after any required number of quarter turns. All other elements of the system are the same as when corrodable links are used as timers, except that arm 8 can be short, as there are no cams. Return of arm 8 under the action of fork 13, although it turns valve stem 16, is not impeded by flexible shaft 33 because the connection is through ratchet clutch 34.
The air under pressure in cylinder 1 may simply be introduced from a compressor. An alternative method, however, is to obtain gas by chemical or electro-chemical means. A mixture of Sodium Borohydride and sea water, for example, is a plentiful source of hydrogen, and such a mixture could be introduced into the cylinder before laying the gear. Hydrogen is also evolved during galvanic corrosion of Magnesium, according to the equation Mg.+2H 2 O=Mg. (OH) 2 ≠H 2 . A suitable galvanic couple could also be introduced into the cylinder before laying the gear. In both cases, there is ample time between "lifts" for pressure to be built up.
Alternative means of carrying the invention into effect, which do not go beyond the limits of its protection as claimed, include: All valves could be microprocessor-controlled, and actuated by solenoids, or by opening circuits to impress a current on links made from material that is high in the galvanic series in sea water. Valve 10 could be timer controlled like valve 7 instead of depending upon external water pressure. Since the speed of ascent could be established by calculation or experiment, such timed actuation could be related to a predetermined water depth, or the time interval after inflation could be such as to ensure that the gear will have reached the surface, i.e. zero depth. Valve 10 could also be arranged to leak gas at a predetermined rate.
Release of gas from the buoyancy chamber or cylinder could be used instead of the hydrofoil sinker, to achieve lateral movement of the system. Hydrofoils attached directly to the frame 2 could function in the same manner as the hydrofoil sinker, and would cause lateral movement during ascent as well as fall.
A differential pressure valve could be incorporated in the system to bleed off excess pressure in the bladder 6 as the apparatus rises through the water. This would enable container 5 to be more lightly constructed, since it would not have to be pressure-resistant to any significant extent. | An inflatable float with timer and pressure controls to enable underwater gear to be automatically lifted off the sea bed at intervals and moved to a new location. The gas for inflating the float may be generated by chemical means or galvanic action. | 1 |
BACKGROUND OF THE INVENTION
[0001] The invention relates generally to improvements in the manufacture of expandable stents and, more particularly, to new and improved methods and apparatus for direct laser cutting of stents in providing stents of enhanced structural quality.
[0002] Stents are expandable endoprosthesis devices which are adapted to be implanted into a patient's body lumen, such as a blood vessel or coronary artery, to maintain the patency of the artery. These devices are typically used in the treatment of atherosclerotic stenosis in blood vessels, coronary arteries, and the like.
[0003] In the medical arts, stents are generally tubular-shaped devices which function to hold open a segment of a blood vessel or other anatomical lumen. Stents are very high precision, relatively fragile devices and, ideally, the most desirable stents incorporate a very fine precision structure cut from a very small diameter, thin-walled cylindrical tube. In this regard, it is extremely important to make precisely dimensioned, smooth, narrow cuts in the thin-walled tubing in extremely fine geometries without damaging the narrow struts that make up the stent structure. Prior art stents typically are cut by a laser and held by collet in a computer controlled machine that translates and rotates the stent as the laser cuts through the outer surface of the metal tubing. In order to stabilize the stent tubing, typically a bushing surrounds the stent tubing and is positioned between the laser and the collet holding the stent. Prior art bearings or bushings create a small amount of friction between the stent tubing and the bearing which can cause slight imperfections in the laser cutting process as the stent tubing is moved relative to the bearing.
[0004] Accordingly, the manufacturers of stents have long recognized the need for improved manufacturing processes and to reduce the amount of friction between the bearing and the stent tubing during the laser cutting process. The present invention fulfills these needs.
SUMMARY OF THE INVENTION
[0005] In general terms, the present invention provides a new and improved method and apparatus for direct laser cutting stents by enabling greater precision, reliability, structural integrity and overall quality.
[0006] The present invention provides an improved system for producing stents with a fine precision structure cut from a small diameter, thin-walled, cylindrical tube. The tubes are typically made of stainless steel, other biocompatible materials, or biodegradable materials, and are fixtured under a laser and positioned utilizing a CNC machine to generate a very intricate and precise pattern. Due to the thin wall and the small geometry of the stent pattern, it is necessary to have very precise control of the laser, its power level, the focus spot size, and, importantly, the precise positioning of the laser cutting path.
[0007] In keeping with the invention, a stent tubing is held in a collet in a CNC machine so that the stent tubing is able to rotate and translate relative to a fixed laser beam. In order to support the stent tubing, a bearing or bushing supports the stent tubing just proximal to the laser beam (between the collet and the laser beam). In this manner, the stent tubing is prevented from sagging or deflecting away from the laser beam, which would otherwise create inaccuracies in the cut stent pattern. In the present invention, a fluid bearing includes a housing having a gas inlet port and a fluid inlet port on its outer surface. A bearing is positioned within the housing and the bearing has multiple blades that are aligned with the gas inlet port on the housing. The bearing is free to rotate within the housing without touching the housing. The gas inlet port is positioned to inject a high pressure gas on the blades in order to impart a high speed rotation of the bearing within the housing. The fluid inlet port on the housing is positioned to inject fluid onto an inner surface of the bearing so that as the bearing rotates at high speed, a thin film of fluid adheres to the inner surface of the bearing. The stent tubing is inserted through an inner diameter of the bearing so that the bearing supports the stent tubing just proximal of the laser beam. As the bearing rotates at high speed, on the order of about 1,000 to 10,000 rpm (or higher), the film of fluid adheres to the inner surface of the bearing so that the film of fluid is between the inner surface of the bearing and the outer surface of the stent tubing. Since the bearing is rotating at high speed and a film of fluid is formed between the inner surface of the bearing and the outer surface of the stent tubing, the stent tubing is centered within the bearing thereby creating a near frictionless environment as the stent tubing translates and rotates relative to the laser beam. The fluid film has very low friction and will not place a significant resistive load on the stent tubing as the collet or CNC system rotates and translates the stent tubing relative to the laser beam.
[0008] The advantages of the present invention will be apparent from the following more detailed description when taken in conjunction with the accompanying drawings of exemplary embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a plan view depicting a prior art laser cutting assembly for cutting a pattern in stent tubing.
[0010] FIG. 2 is a perspective view of a prior art bushing used to support stent tubing during a laser cutting operation.
[0011] FIG. 3 is a partial elevational view of a prior art laser cutting assembly in which a bushing receives the stent tubing for support during a laser cutting process.
[0012] FIG. 4 is a plan view of a laser cutting assembly in which a fluid bearing is used to support stent tubing during a laser cutting process.
[0013] FIG. 5 is a perspective view depicting a fluid bearing assembly for use in supporting stent tubing during a laser cutting process.
[0014] FIG. 6 is a partial cross-sectional view depicting a fluid bearing for supporting stent tubing during a laser cutting process.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0015] Referring to FIGS. 1-3 , a typical prior art laser assembly is shown in which a laser beam is used to cut a pattern in stent tubing. The stent tubing is mounted in the collet of a CNC controller which will move the stent tubing in a translational and rotational direction while the laser beam cuts through one wall of the stent tubing to form a pattern. As shown, a bushing is used to support the stent tubing between the collet and the laser beam (or proximal to the laser beam). The prior art bushings typically support the stent tubing, however, because the inner diameter of the support bushing is closely matched to the outer diameter of the stent tubing, there is some amount of drag or friction between the bushing and the stent tubing. The control system must supply sufficient force to overcome the inertia of the tubing and the drag caused by the interface between the bushing and the stent tubing, and at the same time accurately position the stent tubing for laser cutting. It is therefore a goal to reduce cutting errors due to sticking and choppiness in the movement of the stent tubing and to improve yields.
[0016] In keeping with the present invention, as shown in FIGS. 4-6 , a laser cutting assembly 10 includes a CNC controller 12 and a laser beam assembly 14 . The laser beam assembly is well known in the art and includes numerous components such as a focusing lens, coaxial gas jet, and the laser beam itself. The laser cutting assembly 10 also includes a collet 16 , which is well known in the art, and is used for the purpose of holding a stent tubing 18 and moving the stent tubing in a translational and rotational direction. The stent tubing 18 is mounted in the collet 16 and the stent tubing extends away from the collet so that it is positioned directly under the laser beam assembly 14 . Typically, the laser beam assembly, and the laser beam itself, remain stationary during the stent cutting process, while the stent tubing translates and rotates while the laser beam removes material from the tubing.
[0017] In further keeping with the invention, a fluid bearing 20 is provided to support the stent tubing 18 . More specifically, the fluid bearing includes a housing 22 that will be anchored at one end so that the housing is stationary and firmly supports the stent tubing. The housing has a gas inlet port 24 and a fluid inlet port 26 on its outer surface 28 . Depending upon the specific requirements, more than one gas inlet port 24 and fluid inlet port 26 can be provided and spaced along the outer surface 28 of the housing 22 . Typically, the multiple gas inlet ports or fluid inlet ports would extend in alignment circumferentially around the outer surface 28 of the housing 22 . A bearing 30 is contained within the housing 22 so that the bearing can rotate at high speed within the housing without hitting or touching the walls of the housing. The bearing 30 has one or more blades 32 that are positioned in grooves 33 in the housing 22 which align with the gas inlet port 24 . When high pressure gas is injected into gas inlet port 24 , the gas will impinge on the blades 32 thereby causing the bearing 30 to rotate at high speeds. For example, it is contemplated that the bearing 30 will rotate at speeds between 1,000 rpm up to 10,000 rpm. In another embodiment, it may be appropriate for the bearing 30 to rotate at speeds between 10,000 rpm up to 100,000 rpm.
[0018] With reference in particular to FIG. 6 , the bearing 30 has one or more fluid channels 34 that will allow fluid to pass from the fluid inlet port 26 into a cavity 36 and through the fluid channels 34 onto the inner surface 38 of the bearing 30 .
[0019] In use, the present invention provides a low friction fluid film between the bearing and the stent tubing so that the amount of friction between the bearing and the stent tubing is substantially reduced from the prior art devices. Again, referring to FIGS. 4-6 , a fluid is injected through fluid inlet port 26 on the housing 22 and a high pressure gas is injected through gas inlet port 24 , also on housing 22 . The high pressure gas impinges on the blades 32 which cause the bearing 30 to rotate at a high speed as previously disclosed. As the bearing 30 rotates at high speed, the fluid is forced from the fluid inlet port into cavity 36 where it can flow through fluid channels 34 in the bearing 30 and onto the inner surface of the bearing 38 . As the bearing 30 rotates at high speeds, the shear between the bearing and the fluid will cause a film of fluid to adhere to the bearing inner surface 38 and this film will separate the outer surface 40 of the stent tubing 18 from the bearing 30 . The fluid film has a very low coefficient of friction, and accordingly will not place a significant resistive load on the stent tubing as the collet 16 attempts to rotate and translate the stent tubing relative to the laser beam. Further, the high rotational speeds of the bearing 30 , in conjunction with the film fluid that adheres to the inner surface 38 of the bearing, act to center the stent tubing 18 relative to the bearing 30 . This further allows the laser beam to precisely cut the stent pattern so that a more accurate stent pattern can be reproducably manufactured.
[0020] In one embodiment, the space between the blades 32 and the grooves 33 in the housing 22 may be sufficient to allow the high pressure gas to be directed toward the stent tubing. This serves several purposes including allowing the gas to exhaust from the bearing 30 , thereby allowing more gas to be injected to drive the bearing rotation. Further, as the gas exhausts, it may exert a pressure in the direction opposite to the flow of fluid along the stent tubing thereby forcing fluid out of the space between the bearing 30 and the stent tubing 18 in only one direction. This will prevent contamination of the region opposite to the exit location, namely where the laser is cutting the pattern in the stent tubing.
[0021] In an alternative embodiment, the blades 32 may be either flat fins or have a tilted configuration such as the blades found in a turbine (not shown). In either configuration, the grooves 33 that receive the blades 32 will be configured to accommodate the blades as the bearing 30 rotates. Further, the blades also can have a curved configuration and still provide the rotational forces on the bearing as described. In one embodiment, the blades have a rectangular shape and are substantially flat fins.
[0022] The fluid used with the present invention can be water, saline or any thin oil such as a mineral oil. Further, the high pressure gas typically will be air.
[0023] The housing 22 can be formed from any rigid material such as stainless steel, while the bearing 30 is formed from a low friction material such as a polymer, including such polymers such as PTFE.
[0024] It will be apparent from the foregoing that the present invention provides a new and improved method and apparatus for laser cutting stents thereby enabling greater precision, reliability and overall quality in forming precise stent patterns in stent tubing. Other modifications and improvements may be made without departing from the scope of the invention. Accordingly, it is not intended that the invention be limited, except by the appended claims. | A fluid bearing assembly provides support to stent tubing while the stent tubing is undergoing laser cutting to form a stent pattern. The fluid bearing assembly supports the stent tubing and provides a fluid barrier between the bearing and the stent tubing thereby providing nearly frictionless movement between the support bearing and the stent tubing. | 5 |
This application is a continuation-in-part of U.S. application Ser. No. 07/925,380, filed Aug. 3, 1992, now U.S. Pat. No. 5,423,887, which is a division of U.S. application Ser. No. 07/646,001, filed Jan. 24, 1991, now U.S. Pat. No. 5,163,955.
BACKGROUND OF THE INVENTION
This invention relates to the fabrication of bioprosthetic heart valve replacements. Valve replacements are required for patients having a heart valve which is diseased or otherwise incompetent. Commonly, heart valve bioprostheses are made from a combination of animal tissue and mechanical elements. These bioprostheses have an advantage over purely mechanical valves in that they do not require the use of anticoagulant therapy that plagues purely mechanical valves.
U.S. Pat. No. 5,163,955 (the '955 patent) discloses such a bioprosthetic valve, in which an inner stent, on which the tissue used to construct the valve is wrapped, is inserted into a spreadable outer stent containing a self-adjusting tensioning spring around the circumference of its base. The inner stent posts are fitted with a plurality of outwardly-projecting pegs which register with holes cut in the tissue, and the inner stent assembly is covered with cloth. The spread outer stent clamps the stents together at its base and at a plurality of posts projecting from the bases of both the inner and outer stents. This clamping thus secures the tissue while compensating for irregularities and supplying a clamping force which is evenly distributed over the entire circumference of the tissue.
The outer stent disclosed in the '955 patent has an annular base constructed with a groove around its circumference, into which a self-adjusting tensioning means such as a garter spring is fitted. The garter spring provides a clamping force when the inner stent is inserted into the outer stent. Additionally, the posts on the outer stent are configured with windows surrounded by struts, which give shape to the post. The window is shaped to conform to the shape of the inner stent posts while leaving a small gap between the inner stent posts and the struts when the inner stent is inserted into the outer stent. Such an arrangement facilitates the insertion of the inner stent into the outer stent and provides for a uniform application of the clamping force to the tissue.
At the bottom of each of the windows in the outer stent posts are slots which segment the base into a plurality of arcuate portions. The slots enable the outer stent to be spread open so that it can easily be fitted over the inner stent without damaging the tissue during the valve assembly process.
An elastomeric sewing ring is bonded to the base of the outer stent assembly to facilitate the sewing of the assembled heart valve into the patient. The entire assembly is covered with a fabric cover, typically made out of DACRON, which is bonded to the bottom of the outer stent base.
SUMMARY OF THE INVENTION
In accordance with the present invention, an improved outer stent is provided for a heart valve for securing an inner stent with a base and a plurality of posts extending and spaced around the base and having tissue wrapped thereon. The inner and outer stents cooperate to form a heart valve implanted into a patient, typically by the use of sutures.
The outer stent has a base including a plurality of slots and preferably two tensioning springs disposed around the circumference of the base to prevent the inner and outer stents from becoming unsecured if one of the springs breaks. The provision of more than one tensioning spring is an advantageous feature of the present invention which gives the valve redundancy, for if one spring breaks, another will continue to provide the outer stent's clamping force on the inner stent.
Additionally, the slots around the outer stent base are advantageously fashioned to be narrow enough to decrease the potential for the suturing needle becoming entangled in the tensioning springs during the insertion procedure. Their width is selected to be the minimum sufficient to allow the outer stent to supply an adequate clamping force if a small amount of tissue or debris becomes lodged in the slot.
The outer stent has a plurality of posts extending upwardly from its base connected to each other by scalloped portions and registering with the inner stent when the inner and outer stents are secured together. The posts each include a window to allow the registry of the corresponding inner stent posts with the outer stent. A further advantageous feature of the present invention is the provision of a wedge-shaped elastic ring bonded to the base of the outer stent to provide a better fit for the valve in the patient's aortic root.
The geometry of the inner and outer stents is determined using three basic parameters, the inner stent post width, the height of the scallops on the inner stent connecting its posts, and the inner diameter of the valve. These parameters are chosen based on the size required of the heart valve to be replaced. The chosen values for these parameters are then input into a computer-aided design (CAD) software package, which utilizes curve-fitting algorithms to generate three-dimensional surfaces corresponding to the inner stent blank. Next, the outer stent geometry is derived from the curves developed during computation of the inner stent geometry. An important object of the outer stent geometry computation process is the provision of sufficient clearance between the inner and outer stents at all points to prevent the tissue from being too tightly clamped and forming stress raisers which increase the chances of fatigue tearing of the tissue.
The outer stent assembly is typically molded out of DELRIN or another suitable thermoplastic and is covered by a fabric sock, typically of DACRON. In the preferred embodiment of the present invention, the sock is attached to the stent by first bonding it to the bottom surface of the base of the outer stent at a first weld, then wrapping the covering around both the outer and inner surfaces of the outer stent, covering the base of the outer stent a second time, and finally securing the other end of the sock to the top of the outer stent base with a second weld. This method of construction is a significant feature of the present invention, since it provides two layers of fabric around the outside of the base of the outer stent. The outermost layer of fabric covers the first weld and thus keeps it out of the patient's bloodstream, thereby preventing blood clots from forming on the weld and entering the patient's bloodstream. The extra layer also provides increased strength for the valve base assembly by virtue of the double thickness it imparts to the cloth covering.
Along the segments where the fabric covers the slots in the stent, the two layers of fabric covering the outer stent base are advantageously bonded together with a suitable adhesive. This is done to prevent a tunnel from forming between the layers at points over the slots in the base; such a tunnel could serve as the formation point for blood clots.
The stent of the present invention therefore achieves the objects of providing a reliable securing force for the tissue mounted on the inner stent of a bioprosthetic heart valve while minimizing insertion difficulties and preventing the formation of blood clots.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the major components in the valve assembly.
FIG. 2 is a view of the geometry of construction of the inner stent.
FIG. 3 is a wireframe view of a partially-constructed inner stent, particularly showing the scallop geometry.
FIG. 4 is a perspective view of a portion of the inner stent.
FIG. 5 is a partial cross-sectional view of a portion of an outer stent of the present invention.
FIG. 6 is a side view of the bare inner stent inserted into the outer stent.
FIG. 7 is a cutaway view of the inner and outer stents mated together, showing the relevant clearances between the inner and outer stents.
FIG. 8 is a perspective view of the mated inner and outer stents.
FIG. 9 is an exploded view of the outer stent, securing springs, and covering sock of the present invention.
FIG. 10 is a cross section of a post of the outer stent, showing part of the process of covering the outer stent with a fabric sock.
FIG. 11 is a cross section of a post of the outer stent when fully covered with a fabric sock, showing the bonding of the fabric to the surface of the outer stent.
FIG. 12 a side view illustrating the placement of adhesive between the fabric layers covering the outer stent.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The components which make up the assembled valve are illustrated in FIG. 1. As illustrated, these components include outer stent 1, tissue 2, and inner stent 3. The inner and outer stents have frames, respectively constructed out of a thermoplastic such as DELRIN or the like using injection molding to form the entire component using unibody construction techniques, instead of welding or the like to attach any protuberances. Unibody construction is less risky to the patient than welding, since welded bonds can break more easily, leading to the injection of valve components or fragments into the bloodstream.
Once constructed, the outer stent frame is integrated with other components, including a sewing ring and a plurality of garter springs or similar tensioning members, and both frames are covered with a fabric such as DACRON or the like, to form the completed inner and outer stents used in the valve assembly.
The inner stent frame is preferably constructed with an annular base 12 with three posts 14, 16, and 18 extending from the annular base along the axis of the valve in the direction of blood flow through the valve. Preferably, three such posts are spaced uniformly around the annular base, i.e. such that the centers of adjacent posts are separated by 120 degrees on a circle passing through all three. The posts are connected by scalloped walls, such as that illustrated at 20. The posts are configured with a plurality of outward-facing members 22. These members are later shaped into tissue alignment members for use in holding the tissue in place while the valve is being assembled. Finally, the inner stent is covered by a fabric sock made of DACRON or a similar material, the sock being secured by bonding to the base of the inner stent.
Referring to FIG. 5, the outer stent 1 has a base 99, from which rise scalloped edges 90, which separate the outer stent posts, such as that shown at 92. The post 92 includes a strut 93 and has a window 94 cut out of it for receiving an inner stent post. At the bottom of the window are fillets 96 and slots 98 segmenting the base of the outer stent into arcuate portions, such as 100. An important advantage of the present invention is that the slots 98 are made as thin as possible to minimize the risk that the sutures used in implanting the valve in the patient will become entangled in the securing springs located around the base of the outer stent. However, if the slots are made too thin, they may pinch the tissue and prevent the outer stent from supplying the clamping force necessary to hold the inner stent in place. In practice, it has been found that a width of 0.050 inches is satisfactory clearance. This width is approximately equal to twice the sum of the tissue and cover thickness.
The tissue 2 is preferably taken from the patient during the surgical procedure, and is preferably pericardium. However, other types of tissue, such as autologous fascia lata or animal or cadaver tissue, may also be used as well. After being harvested from the patient, the tissue is immersed in a weak glutaraldehyde solution for a brief period of time, and is preferably cut into the proper shape using a die described in the '955 patent, which is fully incorporated herein by reference. The current assignee's co-pending application, Ser. No. 08/169,620, filed Dec. 17, 1993, discloses an improved tissue cutting die, and is also incorporated herein by reference. The use of other means of cutting the tissue, such as a scalpel, is also possible.
The completed valve is assembled by wrapping the tissue 2 around the inner stent 3, spreading open the outer stent 1, and inserting the inner stent into the outer stent. A technique and tools for performing this operation are disclosed in the present assignee's application Ser. No. 08/238,463, filed Dec. 17, 1993, and incorporated fully herein by reference.
The design of the inner and outer stents must achieve several important objectives. Firstly, the inner and outer stents should remain slightly separated from each other when mated. If they do not, the tissue wrapped on the inner stent will be pinched by the outer stent at the locations where they have insufficient separation, potentially resulting in fatigue tearing and failure of the tissue. Secondly, the tissue wrapped around the inner stent should form three spherically-shaped cusps to distribute the stresses of closure as evenly as possible over the valve. Finally, the inner stent scallops on which the tissue rests should have a horizontal profile to prevent the formation of stress raisers at the points of contact between the tissue and the scallops.
The outer and inner stents are designed with a complex, three-dimensional shape corresponding to the desired valve size in order to achieve these goals. The design is preferably carried out on a computer using computer-aided design (CAD) software having the capability to represent three-dimensional objects. As described below, in the preferred embodiment, the designer first creates a basic geometry for the stents and uses this to define the scallop geometry. This scallop geometry is used to split a rotational surface created to define the stent blank, creating the proper shape for the stent in three dimensions. Necessary surfaces and fillets are finally added to this shape to create the final stent shape. This shape is then input into machine tooling which cuts an electrode into the corresponding shape. Finally, the electrode is used to dissolve a pattern into a block of a suitable metal, such as a nickel-steel alloy, into the final mold for injection-molding the stents.
The basic geometry of the inner stent 3 is determined by three parameters dependent on the size and strength of the valve desired, namely the post width, the scallop height above the base, and the inner diameter of the valve. The post width is determined from the strength desired for the inner stent and the requirement that the completed valve fully close. The post must be made wide enough to give the inner stent sufficient strength but must not be made so wide that the amount of tissue draped over the inner stent posts is so great that the valve cannot properly close. Representative values for this dimension which have been found acceptable in practice for variously-sized valves are given in column K in Table 1.
The scallop height must be sufficient to achieve three objectives: (1) allow the leaflets of the valve to completely close, (2) provide sufficient flexibility to absorb the shock of valve closure, and (3) distribute the stresses encountered during normal use of the valve evenly throughout the tissue leaflet area. The choice of the inner diameter of the valve is based on the size of the patient's annulus, as measured during the surgical procedure with an obturator such as that disclosed in the present assignee's pending application Ser. No. 08/169,618, filed Dec. 17, 1993, which is incorporated by reference herein. Values for the scallop height as a function of inner diameter which have been determined to be satisfactory in practice can be determined by subtracting dimension D in Table 1, which is the distance from the scallop base to the top of the inner stent posts, from the height of the inner stent, shown as dimension E in Table 1.
An important advantage of the design methodology of the present invention is that it allows the use of a single method to easily fabricate size-specific stent kits corresponding to varying annulus diameters. The parameters associated with each annulus diameter are easily input into the computer-aided design (CAD) software, which generates a corresponding stent geometry while requiring little user input.
Referring to FIG. 2, which illustrates the construction of the inner stent basic geometry from these parameters, the designer, typically operating on a computer having CAD software, creates inner and outer circles 30 and 32 respectively in the x-z plane of the space in which the valve design will be created. A stent post primitive 34, which represents a cross section of the inner stent blank, is rotated about the y-axis to create the stent blank. The stent post primitive has a base section 36, which has a taper, typically approximately 15 degrees, and an upper section 38, to which the outwardly-projecting members 22 are attached. The upper section 38 is preferably parallel to the y axis. The taper helps bias the valve into a closed position, which enables the valve to close more easily in low-pressure conditions. It also produces a "jet nozzle" effect which reduces turbulence as blood flows through the valve, leading to a smaller net pressure drop across the valve and resulting in less energy loss to the cardiac cycle.
The stent post width is shown as dimension A in FIG. 2 and is drawn onto the annulus between the circles 30 and 32 at three equally-spaced intervals separated by 120 degrees, creating locations 37, 39, and 41, which represent the positions of the stent posts of the completed stent. In FIG. 2, posts 37 and 41 are shown spaced 30 degrees each from the x-axis to facilitate understanding of the construction process described below. For each post, such as 37, a vector, such as that shown at 40, is drawn from a point 42 at the intersection of the post edge closest (in the x-direction) to the center of the circles and the circle 32, to a point 44 corresponding to the intersection of the post edge closest (in the x-direction) to the center of the circles and the circle 30.
This vector is projected onto the x axis, forming a line having endpoints 46 and 48. This procedure is repeated for post 41, resulting in a projection having endpoints 50 and 52. The geometry of the scalloped edge separating posts 37 and 41 is determined from the points 46, 48, 50, and 52 that result from the projection operations described above as follows: vertical lines parallel to the y-axis, 54, 56, 58, and 60 are dropped from the respective points 46, 48, 50, and 52, and semicircles 62 and 64 are constructed to intersect, at their edges, the lines 50, 56, 54, and 60 respectively. The semicircles are constructed to be tangent to a line parallel to the x axis and spaced a distance β, the height of the scallop above the outer stent base, from the base of the stent primitive. The union of these semicircles and their respective vertical lines forms curves which will be referred to hereinafter as splines 66 and 68. As will be seen, these splines, when projected onto the surface of rotation formed with the stent primitive, determine the shape of the scalloped edge separating posts 37 and 41. The projection of vectors such as 40 onto the x-axis to create another vector lying in the x axis and having endpoints 46 and 48 is performed to ensure that the resulting splines, when projected onto the inner stent blank and ruled as described below, will form smooth surfaces intersecting the stent blank along their entire length. By rotating the inner stent about the y-axis by 120 degrees, an identical procedure may be used to construct the other two splines.
As shown in FIG. 3, the three-dimensional solid model of the inner stent is created by revolving the inner stent post primitive 34 about the y-axis, thereby creating an inner surface 70 and an outer surface 72 of the inner stent. The inner spline 66 is then projected onto the inner surface 70 in three dimensions, and the outer spline 68 is projected onto the outer surface 72. The resulting spline curves 74 and 76 are thus functions of all three spatial variables.
Next, a ruled surface 78 connecting splines 74 and 76 is created. This ruled surface may be transformed into a b-surface containing many nodes by a suitable surface-fitting algorithm to more precisely define the scallop surface, if required by the particular CAD system employed in the design process. The ruled surface 78 or a similar b-surface represents the actual surface in space of the scallop connecting stent posts 37 and 41 and will eventually be sectioned out of the surface of revolution defining the solid model of the inner stent blank.
An important feature of the present invention is that the scallop profile is perpendicular to the axis of the stent, i.e. that a line connecting the inner and outer surfaces of the inner stent along the surface defining the scallop is always parallel to the x-z plane at all positions along the scallop. This feature permits the tissue, which is draped over the scallops, to contact the inner stent along its entire width, thereby preventing the formation of possible points of fatigue on the tissue.
Another advantageous feature of the present invention is that the inner stent is designed so that cusps of the valve are spherical sections. The arcs 62 and 64 are chosen to be circular because such a geometry results in a spherical configuration for each cusp of the heart valve. This spherical configuration is important in ensuring adequate stress distribution throughout the tissue comprising the valve leaflets.
After the creation of the ruled surface 78 between the stent posts 37 and 41, two other ruled surfaces constructed in an identical fashion to the ruled surface 78 are added between the other stent post 39 and the posts 37 and 41. These surfaces are used to form the scallops by splitting the solid model of the inner stent blank at their intersection with the solid inner stent model.
The finished three-dimensional model of the inner stent, which is output to programmable tooling, is created by deleting the remaining surfaces and adding the fillets 80 and 82 to the inner stent posts, as shown in FIG. 4, to smooth the upper surfaces of each of the posts. The outward-facing tissue alignment members 22 are also added. Then, the programmable tooling is used to fabricate an electrode having a shape corresponding to that output by the CAD system. This electrode dissolves a pattern into a block of a suitable alloy into the proper shape to create the final injection mold for the inner stent.
The geometry of the outer stent 1 is determined much the same way as that of the inner stent 3 in the preferred embodiment of the present invention. Referring to FIG. 5, the outer stent post primitive 84 is created with a tapered portion 86 and a vertical portion 88. The lower portion of the outer stent primitive is displaced outwardly a suitable distance, typically 20 mils, from the location of the corresponding inner stent primitive 34, and the outer stent blank is revolved about the y-axis to create an outer stent solid model (not shown). As with the inner stent, the solid model is cut by calculated ruled or b-surfaces defining the scallops, and the required fillets are added to the final model. During the design of the external shape of the outer stent, the scalloped edges 90 are created somewhat differently from those of the inner stent, however.
An important objective in the design of the outer stent 1 is the maintenance of sufficient clearance between it and the inner stent 3 to prevent the tissue 2 wrapped around the inner stent from being pinched by the outer stent when the stents are mated together during the valve assembly process. Such pinching could lead to the formation of stress raisers in the tissue and ultimately result in tearing of the valve tissue. As seen in FIGS. 6 and 7, unwanted pinching could occur, for example, in the radially-outward direction at the base of both stents at location 95, between the posts of the inner stent and the windows 94 of the outer stent in both the radial and tangential directions at location 97, or anywhere in the volume formed between the inner and outer stents connecting these locations. It is thus important to provide sufficient clearance along the entire inner/outer stent mating region, which passes through these locations.
The outer stent design must also simultaneously achieve the objective of providing sufficient strength to the posts 92 to withstand the wear the valve will be subjected to over the life of its user. Both of these objectives are advantageously realized by forming the window 94 into a spaded shape by including the fillet 96 and slightly deforming the ruled or b-surfaces used to create the outer stent scalloped edges to contain a cusp, as shown at numeral 90 in FIG. 8. The spaded window shape allows the outer stent posts to maintain sufficient clearance in both the tangential and radial directions with the inner stent posts and the tissue wrapped thereon, while the cusp-shaped scallop design imparts sufficient thickness to each of the struts 93 to provide the required strength to each post 92.
While the above-described method for designing the shapes of the inner and outer stents has proven satisfactory, it will be understood that the use of other techniques to determine the scallop and post geometry is possible as well.
The clearance required between the inner and outer stents along the mating surfaces, as at locations 95 and 97, is typically approximately 20 mils if a thin DACRON sock is used to cover the inner and outer stents, and tissue having a thickness of approximately 15 mils is used to fabricate the valve. Such a value for the clearance also allows the tissue to penetrate the interstices of the DACRON cover, resulting in less slippage between the tissue and the stents. Other dimensions for the inner and outer stents are identified with the letters A-K in FIGS. 6 and 7. These dimensions are proportional to the size of the annulus to be fitted with the valve. Table 1 shows the preferable relationship between these dimensions (in inches) and a variety of possible sizes of the annulus to be fitted:
__________________________________________________________________________SIZE(MM) A DIA B DIA C DIA D E F G H J K__________________________________________________________________________17 .641 .895 .482 .299 .373 .454 .022 .021 .085 .04919 .708 .992 .540 .342 .419 .506 .025 .021 .090 .05421 .773 1.079 .592 .378 .460 .553 .027 .023 .092 .06023 .844 1.180 .650 .414 .505 .606 .030 .025 .103 .06025 .915 1.277 .708 .450 .549 .657 .033 .027 .115 .069TOL. -.040 +.040 -.005 +.005 +.005 +.005 +.002 -.003 +.005 -.005__________________________________________________________________________
Other valve sizes are possible, such as valves configured for young children, where the annulus size might be as small as 14 mm.
The dimensions in Table 1 have proven to be acceptable in practice, and allow the formation of spherical cusps, which have the advantages described above, from the tissue 2 in the completed valve.
Other features incorporated into the outer stent are illustrated in FIGS. 10-11. In the preferred embodiment, the base 99 of the outer stent is provided with a plurality of garter springs 102 or other securing members extending around the length of its base. The garter springs 102 provide the tension force which secures the inner and outer stents together. More than one garter spring is advantageously used in the present invention to increase the redundancy of the valve. If one garter spring breaks, the presence of another spring ensures that the outer stent is still able to fulfill its role of clamping the tissue around the inner stent. Such a result would not be possible if only one spring is used around the base of the outer stent.
Another advantageous feature of the present invention is the provision of a wedge-shaped sewing ring 104, which is attached to the annular base of the outer stent. The sewing ring 104 provides a site on the valve assembly for securing it into the patient's annulus by use of sutures or similar means. A wedge-shaped sewing ring has been found to fit better into the aortic root of a patient than other shapes when the valve is used as an aortic replacement.
As shown in FIGS. 9-12, the outer stent is covered with a DACRON sock 106. Covering the stent frame accomplishes the purpose of isolating nonbiological material, such as the stent frame thermoplastic, from the body. This also helps avoid the problem of thromboembolism, which occurs with the use of mechanical valves. It also accomplishes the purpose of promoting tissue ingrowth into the interstices of the fabric, to further isolate the nonbiological material from the body, and integrate the valve into the heart. Additionally, it accomplishes the purpose of providing an interface to the tissue clamped between the stents which is gentle, and which helps nourish the tissue and promote its viability by allowing free passage of blood to the tissue.
To cover the outer stent frame, first, a three-fingered DACRON sock is formed by heat seaming inner and outer sections of DACRON fabric together utilizing either hot wire or ultrasonic techniques. Alternatively, the sock can be woven as one piece or sewn. The sock is then pulled over the outer stent frame and its outer section 107 is secured at the outer stent base at weld 108. Next, the sock's inner section 109 is wrapped around the inner surface of the outer stent, as well as around the outer stent base itself. The inner layer is secured to the top of the base at a second weld 110. The use of these two welds on the outer stent base advantageously provides two layers of fabric covering extending along the entire circumference of the outer stent base and thus increases the resilience of the base. Additionally, this method of securing the DACRON sock also achieves the object of isolating the securing weld 108 from the patient's bloodstream, minimizing the risk that blood clots would form on the weld and enter the patient's bloodstream.
Along the portions of the outer stent base having slots, it is not possible to bond the inner section of the DACRON sock 106 to the upper surface of the base 99. Nevertheless, it is desirable to bond the inner and outer sections of the sock to each other at these locations to prevent the separation of these sections and the possibility of thromboemboli formation. Consequently, the present invention advantageously utilizes a medical-grade adhesive, such as RTV silicone adhesive, to secure the outer and inner sections of the sock together along segments such as 112. Adhesive is applied to the inner or outer section along the portions of the outer stent base overlying a slot.
While embodiments and applications of this invention have been shown and described, it should be apparent to those skilled in the art that many more modifications are possible without departing from the scope of the present invention. The invention is therefore not to be restricted, except in the spirit of the appended claims. | An improved set of stents for autologous tissue heart valves is provided. The stents are designed with the aid of a computer-aided-design (CAD) system, and nest within each other to securely clamp a piece of tissue which forms the leaflets of the heart valve. The geometrical features of the stents are designed to provide uniform nesting between the stents to prevent the formation of stress raisers on the tissue. Additionally, the windows in the stent posts are narrowed to prevent the suturing needle used during implantation of the valve from becoming lodged in the garter springs which clamp the outer stent to the inner stent. Finally, the sock covering the outer stent is bonded to the stent base at both upper and lower locations to isolate the bonds from the patient's blood flow. | 8 |
BACKGROUND
[0001] 1. Field of the Invention
[0002] The present invention generally relates to an assembly for protecting electronic components.
[0003] 2. Description of Related Art
[0004] Powertrain control modules are currently packaged in diverse mechanical configurations. Such mechanical configurations often involve expensive custom die cast and stamp metal covers bonded to other custom polymeric or metal parts to protect the electronic assembly. Powertrain control modules must be designed to operate in harsh, under hood environmental conditions. Yet the high volume required to fulfill an automotive application also requires a cost effective design. The current cost of a typical aluminum die cast housing may represent a significant cost of the overall module. In addition, stamped metal and die cast covers are susceptible to gaps between the top and bottom covers increasing susceptibility to environmental conditions and electromagnetic interference. Further, plastic configurations may offer no electromagnetic interference protection at all.
[0005] In view of the above, it is apparent that there exists a need for an improved assembly for protecting electronic components.
SUMMARY
[0006] In satisfying the above need, as well as, overcoming the enumerated drawbacks and other limitations of the related art, the present invention provides an assembly for protecting automotive electronics. The assembly includes a circuit board, a cover, and a metal housing. The metal housing is disposed over and around the circuit board. The cover and metal housing are crimped together to create a seal that protects the circuit board inside the metal housing and attaches the cover to the metal housing.
[0007] In another aspect of the present invention, the metal housing may be a deep drawn metal housing, or alternatively a rolled metal sheet joined at two ends to create a seam that is welded or soldered. In addition, the metal housing may be coated with an anti-corrosive material. To provide thermal dissipation and support the circuit board, a surface in the form of a groove or trough extending inward from the metal housing towards the circuit board.
[0008] In another aspect of the present invention, the cover may include an electrical connector providing electrical communication with the circuit board from outside the assembly. Further, the electrical connector may be molded into the cover thereby providing improved sealing between the cover and the connector.
[0009] In another aspect of the present invention, the crimped region attaching the cover to the metal housing extends along the entire perimeter or along substantially the entire perimeter between the metal housing and the cover. The enlarged region includes a portion of the metal housing and a portion of the cover crimped together forming mating surfaces on the metal housing and the flange, thereby attaching the metal housing to the cover.
[0010] Further objects, features and advantages of this invention will become readily apparent to persons skilled in the art after a review of the following description, with reference to the drawings and claims that are appended to and form a part of this specification.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a top view of an assembly for protecting electronic components in accordance with the principles of the present invention;
[0012] FIG. 2 is an assembly utilizing a rolled metal sheet to form a housing for protecting electronic components in accordance with the principles of the present invention;
[0013] FIG. 3 is a sectional side view of the assembly with the metal housing having portions to support the circuit board and aid in thermal dissipation;
[0014] FIGS. 4A and 4B are a sectional side view of the crimped region illustrating a rolled crimp in accordance with the principles of the present invention;
[0015] FIG. 5A -D are a sectional side view of the crimped region where the cover is folded over the flange;
[0016] FIGS. 6A and 6B are a sectional side view of the crimped region where both the cover and flange are folded over and crimped; and
[0017] FIG. 7 is a sectional side view of the crimped region where the flange is folded over the cover and the flange and cover are crimped.
DETAILED DESCRIPTION
[0018] Referring now to FIG. 1 , an assembly embodying the principles of the present invention is illustrated therein and designated at 10 . The assembly 10 includes a circuit board 12 , a metal housing 14 , and a cover 16 .
[0019] The cover 14 is disposed about the circuit board 12 to protect electronic components from the environment surrounding the assembly 10 . The cover 16 may include an electrical connector 17 with electrical contacts 18 that provide an electrical connection through the cover 16 to the printed circuit board 12 . The electrical connector 17 may be molded as part of the cover 16 to provide a robust seal therebetween. The metal housing 14 is attached to and seals with the cover 16 in a crimped region 20 . The metal housing 14 may be a deep drawn metal housing, as shown in FIG. 1 , or alternatively, the metal housing 14 may be a seamed metal housing made of a rolled metal sheet, as shown in FIG. 2 . If the metal housing 14 is made of the rolled metal sheet, the seam joining the two ends of the sheet may be welded or soldered. In addition, an anti-corrosive coating may be applied to the inner or outer surfaces of the deep drawn or rolled metal housing.
[0020] Now referring to FIG. 3 , a sectional side view of the assembly 10 is provided. The circuit board 12 is attached to and extends from the cover 16 . The metal housing 14 is disposed about a portion of the circuit board 12 extending from the cover 16 . Electrical components 32 are mounted on a first surface of the circuit board 12 and a layer of thermal adhesive is disposed therebetween to secure the electrical components 32 and aid in dissipating heat generated by the electrical components 32 . A surface 30 of the metal housing 14 extends inwardly toward the circuit board 12 . The surface 30 provides additional surface area in close proximity to the component to aid in heat dissipation. In addition, the surface 30 may be configured to support the circuit board 12 . In the example shown, a thermal adhesive 34 is disposed between the surface 30 and the circuit board 12 allowing the surface 30 to mechanically support the circuit board 12 and also providing a more efficient thermal path between the electrical components 32 and the metal housing 14 . Although, a thermal adhesive 34 is shown disposed between the surface 30 of the metal housing 14 , the metal housing 14 may directly support the circuit board 12 or alternatively, other elastic materials may be disposed therebetween.
[0021] Now referring to FIG. 4A , the crimped region 20 attaching the cover 16 and the metal housing 14 is provided in more detail. Extending from the metal housing 14 a flap 38 extends from the metal housing 14 . The cover 16 has a flange 36 extending from the cover 16 substantially parallel to the flap 38 . A crimped region 20 is formed by rolling the flap 38 together with the flange 36 such that a surface 40 of the flap 38 mates with a surface 42 of the flange 36 , thereby creating a seal and attaching the metal housing 14 to the cover 16 as shown in FIG. 4B . Further, the flange 36 may be made of a conductive metal and crimped around the entire or substantially the entire perimeter of the metal housing 14 , thereby creating a continuous electromagnetic shield including the metal housing 14 and the cover 16 , around the circuit board 12 . For future repair of the circuit board 12 , the flap 38 and flange 36 may be unrolled or straightened allowing access to the circuit board 12 , then resealed with the old cover or a new cover by rerolling or recrimping the metal housing 14 to the cover 16 .
[0022] Now referring to FIG. 5A , another embodiment of the crimped region 20 is provided in accordance with the present invention. The flap 38 may extend beyond the length of the flange 36 as shown in FIG. 5A . The flap 38 may then be folded over the flange 36 as depicted in FIG. 5B . As such, the sealed surface area between the flap 38 and the flange 36 increases over the previous rolled embodiment. A crimp 39 is introduced to both the flap 38 and the flange 36 such that a first surface 46 of the flap 38 mates with a first side 48 of the flange 36 and a second surface 52 of the flap 38 mates with a second side 50 of the flange 36 , thereby creating a seal and attaching the metal housing 14 to the cover 16 , as shown in FIGS. 5C and 5D .
[0023] Now referring to FIG. 6A , another embodiment of the crimped region 20 is provided. In this embodiment both the flap 38 and the flange 36 are folded over together and the crimp 39 is created in all four layers (two layers of the flange and two layers of the flap). The crimp 39 creates a controlled bend in the flap 38 and flange 36 such that, a first surface 54 of the flap 38 mates with a first surface 56 of the flange, a second surface 58 of the flange 36 mates with a third surface 60 of the flange 36 , a fourth surface 62 of the flange 36 mates with a second surface 64 of the flap 38 , thereby creating a seal and attaching the metal housing 14 to the connector cover 16 , as depicted in FIG. 6B .
[0024] Now referring to FIG. 7 , another embodiment of the crimped region 20 is provided. In the embodiment shown in FIG. 7 , both the flange 36 and the flap 38 are folded at a 90° angle. The flap 38 and flange 36 may be folded to extend along the metal housing 14 , although it is contemplated that the flap 38 and flange 36 may also be folded to extend along the cover 16 . A crimp 39 is imparted to the flange 36 and flap 38 . The crimp 39 forms a mating surface 66 on the flap 38 and a mating surface 68 on the flange 36 , thereby forming a seal and attaching the metal housing 14 to the cover 16 .
[0025] As a person skilled in the art will readily appreciate, the above description is meant as an illustration of implementation of the principles this invention. This description is not intended to limit the scope or application of this invention in that the invention is susceptible to modification, variation and change, without departing from spirit of this invention, as defined in the following claims. | The present invention provides an assembly for protecting automotive electronics. The assembly includes a circuit board, a cover, and a metal housing. The metal housing is disposed over and around the circuit board. The cover and metal housing are crimped together to create a seal that protects the circuit board inside the metal housing and attaches the cover to the metal housing. | 7 |
TECHNICAL FIELD
The present invention relates generally to apparatus utilized to control fluid flow in a subterranean well and, more particularly provides a choke for selectively regulating fluid flow into or out of a tubing string disposed within a well.
BACKGROUND
Typically, a flow control apparatus is used to throttle or choke fluid flow into a production tubing string of a subterranean hydrocarbon well. Such flow control chokes are particularly useful where multiple zones are produced and it is desired to regulate the rate of fluid flow into the tubing string from each zone. Additionally, regulatory authorities may require that rates of production from each zone be reported, necessitating the use of a choke apparatus or other methods of determining and/or controlling the rate of production from each zone. Safety concerns may also dictate controlling the rate of production from each zone.
Flow chokes are also useful in single zone completions. For example, in a single wellbore producing from a single zone, an operator may determine that it is desirable to reduce the flow rate from the zone into the wellbore to limit damage to the well, reduce water coning and/or enhance ultimate recovery.
Downhole valves, such as sliding side doors, are designed for operation in a fully closed or fully open configuration and, thus, are not useful for variably regulating fluid flow therethrough. Downhole chokes typically are provided with a fixed orifice which cannot be variable without intervention. These are placed downhole to limit flow from a certain formation. Unfortunately, conventional downhole valves and chokes are also limited in their usefulness because intervention is required to change the fixed orifice or to open or close the valve. Additionally, it is difficult to open a sliding side door slowly against a large differential pressure (such as, in excess of 2500 psi) without damage to any of the door seals because these seals must pass through the flow.
What is needed is a flow control apparatus which is rugged, reliable, and long-lived, so that it may be utilized in completions without requiring frequent service, repair or replacement. To compensate for changing conditions, the apparatus should be adjustable. The apparatus should be resistant to erosion, even when it is configured between its fully open and closed positions, and should be capable of accurately regulating fluid flow. Additionally, there is a need for a variable choke which can open against a high differential pressure without excessive damage to the choke seals.
Such a downhole variable choking device would allow an operator to maximize reservoir production into the wellbore. It would be useful for completions, including any well where it is desired to control fluid flow, such as gas wells, oil wells, and water and chemical injection wells, in sum, in any downhole environment for controlling the flow of fluids.
This is accordingly an object of the present invention to provide such a flow control apparatus which permits infinitely variable downhole flow choking as well as the ability to shut off fluid flow, and associated methods of controlling fluid flow within a subterranean well.
SUMMARY
In carrying out the principles of the present invention, in accordance with an embodiment thereof, an annular choke apparatus, and methods of use, are provided for use within a subterranean well. In broad terms, a choke tool apparatus is provided which includes an outer housing having an outer housing wall with a least one flow port therethrough, and a variable annular flow-area choke disposed within the outer housing, the variable annular flow-area choke having a first generally tubular member sealingly disposed within the outer housing, the first tubular member having a shoulder with a sealing surface, a second generally tubular member slidingly and sealingly disposed within the outer housing, the second tubular member having a shoulder with a sealing surface, the second member movable between a sealed position wherein the sealing surfaces are in sealing abutment and an open position wherein the sealing surfaces are spaced apart. The sealing surfaces preferably provide a metal-to-metal seal. The variable annular flow-area choke described herein preferably provides for infinite adjustment between open and closed positions for precise flow regulation. The apparatus may include an actuator, locking, adjustment and biasing assemblies. In gas lift and other operations it may be desirable to variably regulate the flow without sealing the valve.
These and other aspects, features, objects, and advantages of the present invention will be more fully appreciated following careful consideration of the detailed description and accompanying drawings set forth hereinbelow.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A-C are sectional views taken along line A—A of FIG. 4, of successive longitudinal portions of a choke embodying principles of the present invention, the choke shown in a configuration for running into a subterranean wellbore;
FIG. 2 is a sectional view of the choke shown in a partially open position;
FIGS. 3A-C are sectional views taken along line B—B of FIG. 4, of the choke shown in a fully open position;
FIG. 4 is an end view of the upper end of the tool assembly;
FIGS. 5A-D are detail views of various choke assemblies; and
FIG. 6 is a graphical representation of the choke's open flow-area versus the travel of the choke members.
DETAILED DESCRIPTION
Illustrated in FIGS. 1A-C is a tool assembly 10 embodying the principles of the invention. In the following description of the tool assembly 10 and other apparatus and methods described herein, directional terms, such as “above”, “below”, “upper”, “lower”, etc., are used for convenience in referring to the accompanying drawings. Although the tool assembly 10 and other apparatus, etc., shown in the accompanying drawings are depicted in successive axial sections, it is to be understood that the sections form a continuous assembly. Additionally, it is to be understood that the various embodiments of the present invention described herein may be utilized in various orientations, such as inclined, inverted, horizontal, vertical, etc., without departing from the principles of the present invention.
The tool assembly 10 , as shown, includes a choke assembly 12 disposed within a generally tubular outer housing 14 . An actuator assembly 16 , adjustment assembly 18 , locking assembly 20 , and biasing assembly 22 may also be included.
In a method of using the tool assembly 10 , the variable annular flow-area choke assembly 12 and actuator assembly 16 are positioned within a subterranean well as part of a production tubing string 24 extending to the earth's surface. As representatively illustrated in FIGS. 3A-C, fluid (indicated by arrows 26 ) may flow axially through the tool assembly 10 , and to the earth's surface via the tubing string 24 . The fluid 26 may, for example, be produced from a zone of the well below the tool assembly 10 . In that case, an additional portion of the tubing string 24 including a packer (not shown) would be attached in a conventional manner to a lower adaptor 40 of the tool assembly 10 and set in the well in order to isolate the zone below the tool from other zones of the well. The tool assembly 10 enables accurate regulation of fluid flow between the external area 28 and an internal axial fluid passage 30 extending through the choke.
In another method of using the tool assembly 10 , multiple chokes may be installed in the tubing string 24 , with each of the tools corresponding to a respective one of multiple zones intersected by the well, and with the zones being isolated from each other external to the tubing string. Thus, the tool assembly 10 also enables accurate regulation of a rate of fluid flow from each of the multiple zones, with the fluids being commingled in the tubing string 24 .
It is to be understood that, although the tubing string 24 is representatively illustrated in the accompanying drawings with fluid 26 entering the lower adaptor 40 and flowing upwardly through the fluid passage 30 , the lower connector 40 may actually be closed off or otherwise isolated from such fluid flow in a conventional manner, such as by attaching a bull plug thereto, or the fluid 26 may be flowed downwardly through the fluid passage 30 , for example, in order to inject the fluid into a formation intersected by the well, without departing from the principles of the present invention.
The outer housing 14 preferably has a lower adapter 40 and upper adapter 42 for attaching the tool assembly 10 as part of a tubing string 24 . The upper adapter 42 is integrally formed with outer housing 14 while the lower adapter 40 is sealingly attached at threads 48 to form part of the housing 14 . It is understood that various portions of the tool assembly may be integrally formed with one another or attached together as is known in the art. As shown, the tool has only a single body joint thread enabling manufacture at a reduced cost compared to other designs. The generally tubular outer housing wall 44 separates an exterior area 28 from an internal fluid passageway 30 . Wall 44 defines an interior surface 46 . The Figures show the generally tubular fluid passage 30 offset from the center of the generally tubular outer housing 14 . Such an arrangement better allows for placement of hydraulic inlets, fluid ports, control lines, and the like. It is understood that any of the generally tubular assemblies and parts described herein may be arranged concentrically or not, as desired, may be circular in cross-section, as shown, or may contain irregularities.
The variable annular flow-area choke assembly 12 is sealingly attached to the actuator assembly 16 , shown in FIGS. 1A-C. The actuator assembly 16 is used to operate the variable choke 12 . The actuator assembly shown is only an example of actuators known in the art and hydraulically controlled, but it is understood that the actuator may be hydraulically, electrically, mechanically, magnetically or otherwise controlled as is known in the art.
The actuator assembly 16 axially displaces mandrel 50 along the interior of outer housing 14 . Preferably, mandrel 50 is connected to choke assembly 12 through locking assembly 20 and adjustment assembly 18 , as shown, however, other arrangements can be employed as desired. Mandrel 50 includes profile sleeve 52 and is attached thereto by latch ring assembly 54 . Mandrel 50 and sleeve 52 may be integrally formed, but for tool assembly purposes are preferably separate. Profile sleeve 52 moves axially along the interior wall surface 46 of the outer housing 14 . Upward movement of sleeve 52 is limited, as seen in FIGS. 3A-C, by contact between mating shoulder surface 56 on the upper end 60 of mandrel 50 and corresponding shoulder 58 defined by the interior surface 46 of outer housing 14 .
Mandrel 50 is hydraulically reciprocally actuated. Hydraulic supply lines (not shown) supply hydraulic pressure at upper and lower hydraulic inlets 60 and 62 , as seen in FIG. 4 . Pressure is transmitted along upper and lower hydraulic passages 64 and 66 and upper and lower hydraulic ports 68 and 70 , which are preferably defined within housing wall 44 as shown. Hydraulic inlet ports 60 and 62 may be attached to a hydraulic control line fitting 63 as seen in FIG. 3 .
Upper hydraulic port 68 supplies hydraulic pressure to upper hydraulic chamber 72 in the annular space between mandrel 50 and outer housing wall 44 . Upper piston 76 is attached externally about mandrel 50 . Upper piston preferably includes bearing rings 78 and 80 and circumferential seals 82 , preferably a vee-packing seal. Upper piston 76 is engaged with mandrel 50 such that axial movement of the piston 76 by the actuator assembly 16 causes a corresponding axial displacement of the mandrel 50 . Movement of the piston 76 causes movement of the choke assembly 12 from a closed position 150 , as seen in FIGS. 1A-C, towards an open position 152 , as seen in FIGS. 3A-C. The variable annular flow-area choke 12 is preferably infinitely variable and is seen in an intermediate or partially open position in FIG. 2 .
The mandrel 50 is sealingly received in the outer housing 14 . Circumferential seal 86 sealingly engages the mandrel 50 externally and permits fluid isolation between the upper hydraulic chamber 72 and lower hydraulic chamber 74 . Seal 86 is preferably a vee-packing seals and may include bearing rings 82 and 84 .
Lower hydraulic port 62 supplies pressure to lower hydraulic chamber 74 in the annular space between mandrel 50 and wall 44 below seal 86 and is operable to axially move lower piston 90 . Lower piston 90 preferably includes seal 92 , and retaining rings 98 which cooperate with corresponding grooves 96 in mandrel 50 . Axial displacement of lower piston 90 facilitates corresponding axial displacement of mandrel 50 and operates to move the choke assembly 12 from any open position, such as seen in FIGS. 2 and 3, towards a closed position 150 , as in FIG. 1 .
It is understood that selective operation of actuator assembly 16 operates to selectively open and close choke assembly 12 . The choke 12 may be moved to an open position 152 , as in FIG. 3, or a closed position 150 , as in FIG. 1, or any position therebetween, making the choke infinitely variable.
Axial displacement of the mandrel 50 is accomplished by applying fluid pressure to one of the chambers 72 or 74 , thereby applying an axially directed biasing force to the pistons 76 or 90 , respectively. For example, if it is desired to displace the mandrel 50 axially upward to permit or increase fluid flow through the choke 12 or to decrease resistance to fluid flow therethrough, fluid pressure may be applied to the upper chamber 72 . Conversely, if it is desired to downwardly displace the mandrel 50 to prevent or decrease fluid flow through the choke 12 or to increase resistance to fluid flow therethrough, fluid pressure may be applied to the lower chamber 74 .
It is understood that the actuator assembly 16 may be of various types, mechanical, hydraulic or others. Alternate actuator assemblies and other tool parts may be found in U.S. Pat. No. 5,979,558 issued to Bouldin, which is hereby incorporated by reference for all purposes.
Choke assembly 12 , shown in FIGS. 1A-C, includes upper choke member 110 and lower choke member 112 . Choke members 110 and 112 are generally cylindrical and are circumferentially and sealingly disposed within outer housing 14 .
Upper choke member 110 is slidably disposed in the outer housing 14 and is operably connected to the actuator assembly 16 for axial movement within the housing. Although it is preferable that the upper choke member be mounted for movement, it is understood that either or both of the choke members may be so mounted. The upper end 114 of the upper choke member 110 is sealingly attached to adjustment assembly 18 by retaining ring 116 and seal 118 , preferably an o-ring seal. The mating end 120 of the upper choke member 110 has a preferably integrally-formed mating shoulder 122 formed thereon for abutment with a similar mating shoulder 124 on the lower choke member 112 . Upper choke member 110 preferably includes annular projection 129 which extends, at least when the upper choke member 110 is in a closed position, as shown in FIGS. 1A-C, into the interior 158 within the choke end 128 of lower choke member 112 . Projection 129 of upper choke member 110 preferably includes a flow regulating surface 126 .
The outer surface 126 of projection 128 acts as flow regulator. The shape and features of the projection surface 126 determines the fluid flow rates through the variable annular flow-area port 148 as the choke members are opened or closed along path of travel 154 . The projection surface 126 shape and features can be selected to regulate fluid flow as desired. For example, an arcuate surface, as shown in FIGS. 1-3, produces flow-area characteristics as shown in the graph of FIG. 6 which charts the increase in open flow-area, measured in square inches, versus the axial travel, in inches, of the upper choke number. The arcuate surface provides the desirable ability to open the choke area, and therefore reduce fluid pressure, slowly resulting in less damage to the formation than would occur with sudden pressure loss.
The flow regulating surface 126 can be of any desired shape and produce any desired flow-area to travel curve. Additionally, other features may be added to the projection surface to regulate fluid flow. Alternate projection shapes and features are shown in FIGS. 5A-D. FIG. 5A shows a blunt-nosed projection. FIG. 5B shows the addition of a labyrinth seal 131 to the projection surface 126 . Labyrinth seals are known in the art to regulate fluid flow and various types of labyrinth seal can be employed on projection 129 . FIG. 5C shows a stair-stepped projection surface 126 and FIG. 5D shows a conical surface 126 . Other projection shapes and various combinations of the shapes and features may be used. For example, a labyrinth seal 131 can be used in conjunction with the stair-stepped projection surface.
The lower choke member 112 is preferably slidably and sealingly disposed within outer housing 14 . The mating end 128 of the lower choke member 112 has a preferably integrally-formed mating shoulder 124 formed thereon for abutment with mating shoulder 122 of the upper choke member. Mating shoulder 124 abuts shoulder 125 of the housing wall 46 to prevent upward axial movement of the lower choke member 112 when the choke is open. The lower end 130 of lower choke member 112 abuts a biasing assembly 22 , and specifically bias spring 132 . Recess 134 , integrally formed on lower choke member 112 , forms an annular space for spool assembly 136 . Spool assembly 136 sealingly engages housing 14 at piston seal 140 and rod seal 142 . Alternately, lower choke member 112 may be stationary with respect to upper member 110 , or may be integrally formed with or attached to housing 14 .
Upper and lower choke members 110 and 112 abut at mating shoulders 122 and 124 forming an infinitely adjustable annular choke at annular seal 144 . The annular seal is preferably of a hard, erosion-resistant material, such as ceramic or metal such as tungsten carbide, stellite or of alloy. Other seals, as are known in the art, may be used. The annular seal 144 may seal against liquid and/or gas pressure, as desired. A hard-surfaced seal, unlike rubber, plastic or other soft seals, is preferred.
The choke assembly 12 , upper and lower choke members 110 and 112 and annular seal 144 are shown in a closed position 150 in FIGS. 1A-C. The choke assembly is movable between the closed position 150 and the open position 152 , seen in FIG. 3 . The choke assembly is infinitely variable, that is, the choke member may be positioned, as desired, anywhere between the opened and closed positions, as shown for example, in FIG. 2 . The exemplary embodiment illustrated can be opened to any position along stroke-path 154 which extends a longitudinal distance 156 . The size of annular flow port 148 is controlled by adjustment of the choke members relative to one another. The stroke-path distance 156 may vary, but preferably allows projection 128 to fully clear the interior space 158 of lower choke member 112 , as seen in FIG. 3 .
Fluid flow from external area 28 into fluid passage 30 of tool assembly 10 is controlled through the infinitely variable annular flow port 148 . The variable choke may be opened slowly against a large differential pressure, up to the working pressure of the choke, without damage to the seals. Typical sliding-door chokes can only be opened against a differential pressure of about 1500 psi without damaging the seals.
In gas lift and other operations, it may be desirable to maintain the variable annular area valve in a partially open, or cracked-open, position to allow unloading of the well. That is, in such an application, it would be undesirable or unnecessary to seal annular seal 144 or completely close the valve. In such a case the upper member 110 may be maintained in a partially open position, such as seen in FIG. 2, by use of hydraulic pressure or a stop, lock or other movement limiting device employed such that member 110 is prevented from sealing annular seal 144 . The shoulders 122 and 124 would not need to seal off flow through valve 144 . In the partially open position the shoulders 122 and 124 are adjacent one another, thereby restricting, but not eliminating fluid flow. The variable annular flow-area valve can be moved towards and into the fully open position, seen in FIG. 3, to allow greater fluid flow.
Annular fluid port 148 is preferably adjacent outer housing fluid port 160 , which may consist of multiple openings through housing wall 44 . The housing ports 160 may be placed anywhere along the housing wall 44 , as long as they are in fluid communication with annular port 148 , and may vary in size, design and placement, as desired.
The tool preferably includes a biasing assembly 22 , as shown. The bias spring 132 abuts lower choke member 112 at shoulder 164 and abuts the tool housing 14 at shoulder 166 . The bias spring may be of any type known in the art, such as the cylinder spring, shown, or belleville, coil or other springs. The bias spring 132 exerts a seating load on lower choke member 112 such that the annular flow port 148 remains sealed when the actuator assembly exerts little pressure on upper choke member 110 . Further, where the upper choke member 110 is not under any sealing load, such as when in a locked closed run-in position, bias spring 132 acts to seal the annular valve. The bias spring also takes up any tolerances in the choke assembly. The bias spring 132 may have a deflection 168 and bias force as desired, and operates to move lower choke member 112 longitudinally within the outer housing for up to the defection distance.
The upper choke member 110 may be operably connected to the actuator assembly 16 through an adjustment assembly 18 and a locking assembly 20 . The seat attachment subassembly 170 of the adjustment assembly 18 attaches to upper choke member 110 preferably via a retaining ring assembly 172 , as shown. Other means for attachment may be used as desired. The seat attachment subassembly 170 is a cylindrical mandrel slidably and sealingly engaged within the outer housing 14 . A sealing assembly 174 , which may include spacers 176 and a sealing element 178 , seals the annular space between the exterior of the seat attachment subassembly 170 and the interior wall 46 of the housing 14 . The sealing element 178 is preferably a vee-packing seal, as shown, but may be any suitable.
The adjustment assembly 18 further includes an adjustment mandrel 180 which is adjustably attached to the seat attachment subassembly 170 , preferably via a threaded assembly 182 , as shown. The overall length of the adjustment assembly 18 may be selected by adjusting the attachment of the adjustment mandrel 180 to the seat attachment subassembly 170 . An adjustment locking mechanism 184 is provided, such as the setscrew shown, to allow the adjustment assembly length to be selectively set. Adjustment mandrel 180 abuts the actuator mandrel 50 at shoulder 186 .
Locking assembly 20 includes a retainer ring 190 threadingly attached to adjustment mandrel 180 . The retainer ring 190 acts with lock ring assembly 192 , including lock ring 194 and corresponding recess 196 , and expander ring 198 in a manner known in the art. The retainer ring 190 has an inset shoulder 200 that mates with mandrel shoulder 202 .
In use, the choke tool assembly 10 is run-in to a subterranean well to the desired depth. The tool assembly is preferably part of a tool string which may include numerous choke tool assemblies as well as other downhole tools. The lower and upper adapters 40 and 42 are provided for attachment to a tool string.
The tool assembly preferably has a locked closed run-in position 151 as shown in FIG. 1 . In the locked position 151 , the locking assembly 20 holds the choke assembly 12 in the sealed closed position 150 during run-in operations without hydraulic pressure in the actuator assembly 16 . The locking assembly 20 acts in unison with the biasing assembly to maintain the choke in the closed position. In the locked position, the retainer ring 190 and lock ring assembly 192 maintain the choke assembly 12 in the closed position. Lock ring 194 cooperates with recess 196 in the inner surface 46 of the outer housing wall 44 and the expander ring 198 to prevent mandrel 50 from upward movement.
The locking assembly 20 may be unlocked, as is known in the art, by hydraulically actuating or mechanically engaging the mandrel 50 or profile sleeve 60 and pulling upwards to unlock the lock ring assembly 192 . Shoulder 202 on mandrel 50 mates with shoulder 200 on the retainer ring 190 such that an upward force on the mandrel 50 will force retainer ring 198 upward as well, thereby forcibly moving the lock ring 194 from the recess 196 . The locking assembly 20 is then in an unlocked position 153 , and the choke may be operated. The locking assembly may be locked closed without requiring hydraulic actuator pressure being maintained.
The actuator assembly 16 operates to control the choke assembly 12 . To move the upper choke member 110 towards the open position 152 , hydraulic pressure is applied to upper hydraulic chamber 72 of the actuator assembly 16 . Hydraulic pressure is supplied to upper hydraulic inlet 60 via hydraulic lines (not shown) and then along upper hydraulic passage 64 , through upper port 68 and into upper hydraulic chamber 72 . The hydraulic pressure acts upon upper piston 76 thereby moving the mandrel 50 upwards. Mandrel 50 , which is attached to the locking and adjustment assemblies, causes the upper choke member 110 to similarly move in an upward direction, toward the open choke position 152 . Hydraulic pressure can be applied, as desired, to move the upper choke member 110 any desired distance along choke path 154 between the closed and open positions 150 and 152 up to the total stroke distance 156 .
In the closed position 150 , the upper choke member 110 is sealingly engaged with the lower choke member 112 at mating shoulders 122 and 124 at metal-to-metal seal 144 . As the upper choke member 110 is moved upwardly, the biasing assembly 22 also moves the lower choke member 112 upwardly. The lower choke member 112 will continue to move upwardly for a portion of the deflection distance, as determined by the selection of the deflection device. Once the upper and lower choke members 110 and 112 have moved the deflection distance 168 , continued upward movement by the upper choke member 110 will unseat the mating shoulders 122 and 124 thereby creating an annular flow port 148 defined by the spaced apart mating shoulders.
The annular flow port 148 allows fluid connection between the external area 28 , via fluid port 160 , and the fluid passage 30 . Fluid flow through the annular port 148 is controlled by selective movement of the upper choke member 110 to regulate the flow area available.
Preferably, the choke end 120 of the upper choke member 110 includes projection 129 which extends into the interior space 158 of the lower choke member 112 . The outer surface of the projection 129 defines a choke regulating surface 126 . The choke regulating surface 126 may be of any desired shape and may have additional features as desired. The shape of the regulating surface 126 , by defining the shape of the annular port 148 , regulates the flow area into the flow passage 30 . Preferably, the stroke distance 156 of the choke member 110 is greater than the length of projection 129 such that, at the full open position 152 , the projection 129 does not extend into the interior 148 of the lower choke member 112 .
The upper choke member 110 may be moved downwardly, or towards the closed position 150 , using the actuator assembly 16 . Hydraulic pressure is supplied via hydraulic lines (not shown) to lower hydraulic inlet 62 , through lower hydraulic chamber 74 . An increase in hydraulic pressure within chamber 74 forces lower hydraulic piston 90 downward, thereby moving the mandrel 50 and upper choke member 110 downwardly.
By regulating the hydraulic pressure supplied to upper and lower chamber 72 and 74 , the upper choke member 110 may be moved, or held stationary, as desired to any location along path 154 , that is, in the open or closed positions, 150 and 152 , or anywhere inbetween. Consequently, the choke is infinitely variable and flow through the annular port 148 can be infinitely regulated. The spacing of the choke member 110 and 112 and the design of projection 128 determine the flow rate through the annular port 148 .
Described herein, the choke assembly and methods of controlling fluid flow within the well using the choke assembly, which provided reliability, ruggedness, longevity, and do not require complex mechanisms. Of course, modifications, substitutions, additions, deletions, etc., may be made to the exemplary embodiment described herein, which changes would be obvious to one of ordinary skill in the art, and such changes are contemplated by the principles of the present invention. Accordingly, the foregoing detailed description is to be clearly understood as being given by way of illustration and example only, the spirit and scope of the present invention being limited solely by the appended claims. | In carrying out the principles of the present invention, in accordance with an embodiment thereof, an annular choke apparatus, and methods of use, are provided for use within a subterranean well. In broad terms, a choke tool apparatus is provided which includes an outer housing having an outer housing wall with at least one flow port therethrough, and a variable annular flow-area choke disposed within the outer housing, the variable annular flow-area choke having a first generally tubular member sealingly disposed within the outer housing, the first tubular member having a shoulder with a sealing surface, a second generally tubular member slidingly and sealingly disposed within the outer housing, the second tubular member having a shoulder with a sealing surface, the second member movable between a sealed position wherein the sealing surfaces are in sealing abutment and an open position wherein the sealing surfaces are spaced apart. The sealing surfaces preferably provide a metal-to-metal seal. The variable annular flow-area choke described herein preferably provides for infinite adjustment between open and closed positions for precise flow regulation. The apparatus may include an actuator, locking, adjustment and biasing assemblies. | 4 |
FIELD OF INVENTION
The present invention relates to an integrated electronic device and a fabrication method thereof, more particularly to the integrated electronic device having an electric connection for connecting a semiconductor chip with a circuit board and fabrication method thereof.
DESCRIPTION OF THE PRIOR ART
For higher integration of semiconductor chips on a circuit board, a flip-chip method has been developed which enables bare semiconductor chips to be mounted directly on a circuit board by connecting each of electrodes between the semiconductor chips and the circuit board using soldering metal. However, a drawback on a soldering metal connection is a fact that a surface of an aluminium interconnection layer, widely used in LSI circuit, has repellency against melt of soldering metal, which is often called a wettability problem. It could be avoided by coating the aluminium surface by a metal having an adhesive tendency to soldering metal, but it eventually makes the fabricating steps more complex. Another unfavorable effect of a soldering metal connection is that as shown in FIG. 7, a rigid connection between electrodes 32, 34 by soldering metal 33 often results in a crack 36 due to a repetitive local stress concentration caused by discrepancy in thermal expansion coefficient between a semiconductor chip and a circuit board. To avoid these foregoing problems, as shown in FIG. 8A, a bump 55 containing dispersed liquid metal particles 53 of indium-gallium in flux vehicle 54 for a liquid connection on a gold electrode 52 has been proposed, however, surface tension of the liquid metal 53 against gold surface is still so high that the liquid metal often makes itself droplets 53 on the gold electrode 52 after heating process as shown in FIG. 8B.
SUMMARY OF INVENTION
It is an object of the present invention to provide a method for fabricating an integrated electronic device having a soldering metal connection between a semiconductor chip and a circuit board free from the wettability problem on the soldering metal connection to an electrode of the semiconductor chip.
It is another object of the present invention to provide a method for fabricating an integrated electronic device having a soldering metal connection between a semiconductor chip and a circuit board free from disconnection failures caused by thermal stress.
It is a further object of the present invention to provide an integrated electronic device having a soldering metal connection between a semiconductor chip and a circuit board free from the wettability problem on the soldering metal connection to an electrode of the semiconductor chip.
It is a still further object of the present invention to provide an integrated electronic device having a soldering metal connection between a semiconductor chip and a circuit board free from disconnection failures caused by thermal stress.
One aspect of the present invention is a method for fabricating an integrated electronic device having an electric connection between a first electrode of a semiconductor chip and a second electrode of a circuit board comprising the steps of:
forming a first bump made of a first metal component on the first electrode, a surface of the first electrode having repellency against melt of the first metal component;
forming a second bump made of a second metal component on the second electrode opposite to the first bump in a position; and
forming a connection part made of an eutectic alloy consisting of the first metal component and the second metal component between the first bump and the second bump so as to make an electric connection between the first electrode and the second electrode.
Another aspect of the present invention is a method for fabricating an integrated electronic device having an electric connection connecting a first electrode of a first substrate with a second electrode of a second substrate, both surfaces of the first and second electrodes having an adhesive tendency to molten metal, the method comprising the steps of:
forming a metal bump on the surface of the first electrode, the metal bump being made of a soldering metal alloy consisting of a solid phase component and a liquid phase component at an operating temperature; and
forming an electric connection between the first electrode and the second electrode by heating the soldering metal alloy so as to adhere to the surface of the second electrode.
Still another aspect of the present invention is a method for fabricating an integrated electronic device having an electric connection between a first electrode of a first substrate and a second electrode of a second substrate comprising the steps of:
forming a first metal layer on a surface of a first electrode on a first substrate, the first metal layer capable of composing an eutectic alloy with gallium (Ga);
forming a bump of Ga-rosin mixture on the first metal layer selectively; and
forming the electric connection between the first electrode and the second electrode by heating the bump of Ga-rosin mixture maintaining the bump of the Ga-rosin mixture in contact with the second electrode to react gallium in the Ga-rosin mixture with the first metal layer into the alloy capable to adhere to the first and second electrodes.
The technique according to the present invention can be applied to an electro-mechanical device such as a saw-tooth device or an optoelectronic device as well as a multi-chip semiconductor module having a multi-layered circuit board.
BRIEF DESCRIPTION OF DRAWINGS
Preferred embodiments of the invention are described with reference to the accompanying drawings, in which:
FIG. 1A a diagrammatic section view of a pair of soldering metal bumps on a chip and a circuit board before connecting to each other related to the first embodiment.
FIG. 1B is a diagrammatic section view of a pair of soldering metal bumps on a chip and a circuit board after connecting to each other related to the first embodiment.
FIG. 2A is a diagrammatic section view of a pair of soldering metal bumps on a chip and a circuit board before connecting to each other related to the second embodiment.
FIG. 2B is a diagrammatic section view of a pair of soldering metal bumps on a chip and a circuit board after connecting to each other related to the second embodiment.
FIG. 3 is a diagrammatic section view of a solid-liquid soldering metal connection between a chip and a circuit board related to the third embodiment.
FIGS. 4A-4E are diagrammatic section views of an eutectic alloy connection between a chip and a circuit board in various processing steps related to the first embodiment.
FIGS. 5A-5E are diagrammatic section views of a solid liquid soldering metal connection between a chip and a circuit board in various processing steps related to the third embodiment.
FIGS. 6A-6F are diagrammatic section views of a liquid metal connection between a chip and a circuit board in various processing steps related to the fourth embodiment.
FIG. 7 is a diagrammatic section view of a rigid soldering metal connection having a crack between a chip and a circuit board in the prior art.
FIG. 8 is a diagrammatic section view of a bump containing dispersed liquid metal particles of gallium-indium in a flux vehicle for a liquid metal connection on a gold electrode in the prior art.
FIG. 8B is a diagrammatic section view of liquid metal droplets left on the gold electrode after heating process in the prior art.
FIG. 9 (table) shows examples setting forth combination of the first and second bump metals and their connection temperatures.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1A, a semiconductor chip 1 has an electrode pad 2 of aluminium which has repellency against molten metal chromium or titanium are other suitable materials for electrode pad 2. The first soldering metal bump 3 made of the first metal component is formed on the electrode pad 2, while a circuit board 6 has an electrode pad 5 of copper which has adhesive tendency to molten metal. The second soldering metal bump 4 made of the second metal component is formed on the electrode pad 5. These metal components are capable to compose an eutectic alloy having a specific compound ratio, and that a melting temperature of the first metal component is higher than a contact temperature of the second metal component. The contact temperature is a process temperature to form an alloy between two metal components.
Referring to FIG. 1B, a connection part made of an eutectic alloy consisting of the first metal component and the second metal component is formed between the first soldering metal bump and the second soldering metal bump by heating the both soldering metal bumps at a temperature lower than the melting temperature of the first metal component to maintain the first soldering metal bump in a solid phase at an interface with the aluminium electrode and then cooling down to solidify both of the bumps before the eutectic reaction reaches the aluminium electrode pad 2, in order to prevent the aluminium electrode pad from repelling the first soldering metal bump.
Referring to FIG. 2A, a semiconductor chip 1 has an electrode pad 2 of aluminium has repellency against molten metal. The first soldering metal bump 3A is formed on the electrode pad 2 in a trapezoidal shape by deposition technique using a mask having an opening with the same pattern as the first electrode pad, while a circuit board 6 has an electrode pad 5 of copper has adhesive tendency to molten metal. The second soldering metal bump 4A is formed on the electrode pad 5. A melting temperature of the first soldering metal bump is higher than that of the second soldering metal bump.
Referring to FIG. 2B, electric connection between the electrode pad 2 and the electrode pad 5 is made by heating the both soldering metal bumps in contact to each other at a temperature lower than the melting temperature of the first metal bump to melt the second soldering metal bump 4A without melting the first soldering metal bump 3A and then cooling down to solidify the second soldering metal bump. The soldering metal is not limited to an eutectic alloy in this embodiment. Preferred mixing ratios for the first and second soldering metal bumps are Pb-5% (wt) Sn and Pb-65% (wt) Sn in weight, respectively. The melting temperatures of the first and second metal bumps are 315° C. for Pb-5% (wt) Sn and 185° C. for Pb-65% (wt) Sn, respectively. In this particular example, a preferred processing temperature to melt the second soldering metal bump is 200-230° C. Since the first soldering metal bump is not melted in this process, the trapezoidal shape on the electrode pad 2 is maintained after the electric connection is accomplished.
The electric connection implemented in the first and second embodiments described above does not have disconnection failure due to repellency of molten soldering metal by the electrode surface in the fabrication process. That reduces electric resistance and increases mechanical strength of the connection.
Referring to FIG. 3, an electrode 2A on a semiconductor chip 1 and an electrode 5 on a circuit board 6 are connected to each other by solid-liquid soldering metal 8. The surfaces of both electrodes have adhesive tendency to molten soldering metal. The solid-liquid soldering metal 8 consists of a solid phase component 10 and a liquid phase component 9 at an operating temperature. The operating temperature is a temperature of an integrated electronic device when the device is active in a normal condition. The eutectic reaction will take place in the solid-liquid soldering metal, where the solid and liquid phases are in thermal equilibrium to each other at a solid-liquid interface. For instance, at a sufficiently low temperature when the integrated circuit device is not operated, the solid-liquid soldering metal is solely composed of a solid phase matrix, and as temperature elevates by device operation, a liquid phase component grows in the solid phase matrix. At further higher temperature, a solid phase component 10 is dispersed in a liquid phase matrix 9 as illustrated in FIG. 3. This mechanism releases the soldering metal from a thermal stress, which prevents from disconnection between the electrodes.
Such a process is more particularly described with reference to FIGS. 4A-4E, where a semiconductor chip 11 has an array of electrodes 12A-12F on the surface. FIG. 4A shows that a metal mask 31 having windows was aligned to the semiconductor chip 11 so as to expose each of aluminum electrodes 12A-12F on the semiconductor chip within each of the windows. As shown in FIG. 4B, the first bumps of 100 μm thick indium (In) layer 13A-13F were deposited on the aluminium electrodes through the windows pressing the mask 31 against the surface of the semiconductor chip 11. As shown in FIG. 4C, the In-bumps 13A-13F were exposed by removing the metal mask 31 on which In layer 13 was deposited. FIG. 4D shows that the second bumps of 100 μm thick tin (Sn) layer 14A-14F were formed on copper electrodes 15A-15F of a circuit board 16 by depositing tin through a metal mask. The first and second bumps were aligned to each other as shown in FIG. 4D, then kept contact to each other and heated at a connection temperature which was lower than a melting temperature of indium 156.6 ° C. and higher than an eutectic temperature of In-Sn alloy 117° C , such as 130 ° C, the connection temperature is a processing temperature at which the first and second metal components make an alloy at an interface which provides an electric and mechanical connection, so that a connection part made of an eutectic alloy 17 was formed between the first and second bumps as in FIG. 4E. Since the connection temperature was sufficiently lower than the melting temperature of indium in this process, a molten metal was so localized to the connection part 17 that the aluminium electrode maintained a wide contact area with the first bump, which resulted in low contact resistance free from the repellency problem. Some of the preferred combinations of metals for the first and second bumps, and the connection temperature are shown in Table 1.
Referring to FIGS. 5A-5E, both first electrode pads 19A-19F on a semiconductor chip 11 and the second electrode pads 15A-15F on a ceramic circuit board 16 have an adhesive tendency to molten metal. Each of the first electrode pads 19A-19F was coated by about 0.3 μm thick film of gold, silver, or nickel. Subsequently, about 30 μm high soldering metal bumps 18A-18F consisting of indium (In) and 20% (wt) bismuth (Bi), namely In -20% (wt) Bi, were formed on the first electrode pads 19A-19F by depositing the soldering metals through a mask 31 as shown in FIGS. 5A-5C, similarly to FIGS. 4A-4C. As shown in FIGS. 5D-5E, the semiconductor chip 11 was firmly mounted on the ceramic circuit board 16 by melting at a temperature of about 300° C. and then solidifying the soldering metal bumps into each connection part 18 which connected each of the first electrode pads 19A-19F with each of the second electrode pads 15A-15F.
The connection part 18 shown in FIG. 5E made of In-20% (wt)Bi soldering metal which has deviated in composition ratio by 14% (wt) on Indium side from the In-Bi eutectic alloy having a composition ratio of In:Bi =66:34 in weight. Since the eutectic temperature was 72° C, the In-20% (wt)Bi soldering metal consisted of a solid phase component and a liquid phase component above the eutectic temperature. Therefore, a liquid phase component coexsisted with a solid phase component in the connection part 18 between 75° C.-85 20 C. in the overall operating temperature range from 5° C. to 85° C. of the semiconductor chip. The mechanism that a liquid phase component increases with temperature releases a thermal stress in the connection part 18 caused by a difference in thermal coefficient between the semiconductor chip and the circuit board, and furthermore prevents metal fatigue that would be accumulated in the connection part 18 due to thermal hysteresis. Comparative study of experiments shows that no crack failure was observed in an integrated electronic device according to this embodiment after more than 100 cycles of thermal hysteresis in the operating temperature range from 5° C. to 85° C., while a crack was observed in a solid soldering metal of a prior art after 50 cycles of the same thermal hysteresis in avarage.
The foregoing connection part having solid-liquid phase coexistence in an operating temperature range can be implemented by a soldering metal alloy of various mixing ratios. A soldering metal alloy of the first type is essentially made of an eutectic alloy but has an additional minor component that is harmless for the soldering metal alloy to have the liquid phase component at an operating temperature of the integrated electronic device. The additional minor component gives the eutectic alloy phase separation in an upper part of the operating temperature range, such as an In-Bi eutectic alloy with a minor component of 2-3% (wt) Pb or Ge. A soldering metal of the second type is a soldering metal alloy which consists of the same metal components as those of an eutectic alloy and that the mixing ratio is slightly deviated from that of the eutectic alloy. Some of the eutectic alloys are a tertiary or four-element alloy such as Sn-Bi-In soldering metal based on an eutectic alloy of Sn:Bi:In=16.5:32.5:51 (wt %) with an eutectic temperature of 60° C., Sn-Pb-Bi-In soldering metal based on an eutectic alloy of Sn:Pb:Bi:In=19:17:53.5: 10.5 (wt %) with an eutectic temperature of 60° C., and Sn-Pb- Bi-In soldering metal based on an eutectic alloy of Sn:Pb: Bi:Cd=13.3:26.7:50:10 (wt %) with an eutectic temperature of 50° C.
Referring to FIGS. 6A-6F, processing steps for fabrication of an integrated electronic device having electric connection made of In--Ga liquid metal between a semiconductor chip and a circuit board are described. Ga-rosin mixture was prepared before fabrication of the liquid In--Ga electric connection, for which Ga was mixed with a flux vehicle at mixing ratio of 9 to 1 in weight. After the Ga mixed flux vehicle was heated at 40 ° C. to melt Ga in it, it was stirred until fine Ga droplets of about 20-30 μm diameter were dispersed homogeneously in the flux vehicle. The flux vehicle was monobutylcarbithol including 60% rosin, 2% thichener, 0.5% activator (hydrochloric diethylamine). The semiconductor chip 21 shown up-side do in FIG. 6A, has an array of electrodes 22A-22F on a surface of the semiconductor chip. The first metal mask 31 made of covar was pressed tightly to the surface of the semiconductor chip so that an exposed area of the surface was masked. A 10 μm thick indium (In) film 23 was deposited on the entire surface of the semiconductor chip by evaporation technique. As shown in FIG. 6B, an array of In-coated electrodes was obtained by removing the first metal mask 31. As shown in FIG. 6C, a 200-300 μm thick Ga-rosin mixture 24 was selectively squeezed into each of windows of the second metal mask 32 having a thickness of 200-300μm by a squeezer just as used in a printing technique. After removing the second metal mask 32 left a bump of Ga-rosin mixture 24 on the In-film 23, the semiconductor chip was heated at 200° C. so that Ga in the Ga-rosin mixture 24 and the underlayered In-film 23 were united to each other by eutectic reaction and vaporizing organic components as shown in FIG. 6D. 100 μm high In-Ga liquid connections 27A-27F made of an eutectic alloy between Ga and In were formed on each of the array of the electrodes 22A-22F shown in FIG. 6E. The eutectic reaction proceeded at the interface indicated by a dotted line 23 between In and Ga, which prevented the electrodes from repelling the liquid connection. As shown in FIG. 6F, the semiconductor chip 21 having an array of the liquid connections 27A-27F was mounted on a circuit board 26 having an array of electrodes 25A-25F by flipping the semiconductor chip 21 so that the liquid connection of the semiconductor chip and the electrode on the circuit board was aligned to each other with a certain height by maintaining a certain distance between the semiconductor chip and the circuit board by a spacer 28. The appropriate height of the liquid connection was 100 μm. In the foregoing embodiment, the surface of the electrode has such a good adhesive tendency to a liquid connection that the entire surface of the electrode is covered with the liquid metal, which eventually reduces the electric resistance of the connection. Indium of the eutectic alloy is replaceable by tin (Sn), silver (Ag), or zinc (Zn). | An integrated electronic device having an electric connection between a first electrode of a semiconductor chip and a second electrode of a circuit board. One embodiment according to the present invention is a method for fabricating an integrated electronic device having an electric connection between a first electrode of a semiconductor chip and a second electrode of a circuit board, both surfaces of the first and second electrodes having an adhesive tendency to molten metal, the method comprising the steps of forming a metal bump on the first electrode, the metal bump being made of a soldering metal alloy consisting of a solid phase component and a liquid phase component at an operating temperature; and forming an electric connection between the first electrode and the second electrode by heating the soldering metal alloy so as to adhere to the surface of the second electrode. | 7 |
BACKGROUND AND SUMMARY
1. Background of the Invention
The present disclosure relates to semiconductor memory devices and, more particularly, to a method of providing block state information in a semiconductor memory device having a flash memory.
A claim of priority is made under 35 U.S.C. §119 from Korean Patent Application 10-2006-0107556, filed on Nov. 2, 2006, the contents of which are hereby incorporated by reference in their entirety.
2. Description of the Related Art
Memory devices can be generally classified into two broad categories. These categories are volatile memory devices and non-volatile memory devices. Volatile memory devices do not retain their stored data in the event of a power loss. However, non-volatile memory devices retain their data even in the event of a power loss.
A commonly used non-volatile memory device is a flash memory device. In a flash memory device, data is stored in memory cells. Furthermore, transistors generally function as memory cells in flash memory devices. A flash memory device may be programmed with data or data stored in a flash memory may be deleted using different programming and data deletion techniques. For example, a flash memory device may be programmed by use of a tunneling effect. In the tunneling effect, a relatively large positive potential difference is created between a control gate and a substrate of the transistor. This potential difference causes the electrons on the surface of the substrate to be pushed and trapped to the floating gate. These electrons act as a barrier between the control gate and the channel on the substrate, thus increasing the threshold voltage of the cell transistor. Alternatively, a hot carrier effect may be used to program and/or delete data to/from a memory cell.
In either case, as the number of programming and delete operations increase, the reliability of the memory cells (and thus of the memory device) reduces. That is, there is a limit to the number of programming and delete operations that may be performed on flash memory devices without compromising on the reliability of the device. After such a limit is reached, there may be a substantial increase in programming errors on the device.
To counter the effects of having defective memory blocks, flash memory devices use techniques to replace bad memory blocks with reserved memory blocks that are known to be reliable, i.e., good memory blocks. Many of these techniques involve checking the address of a memory block during a read or write operation. If there is an error in the read or write operation, the block is determined to be a bad block and is then replaced by a reserved block which is assigned the same physical address as that of the bad block. A write or read operation of data is then performed through the reserved block.
FIGS. 1 and 2 illustrate a configuration of general flash memory. As shown in FIGS. 1 and 2 , a flash memory includes meta blocks, user blocks and reserved blocks.
The meta block is a block that is generally used to store information associated with bad blocks, information associated with reserved blocks, and mapping information. The user block is generally used to store data. The reserved block, as described above, is used to replace a bad block.
Referring to FIG. 1 , if blocks 32 and 34 go bad, these are each replaced with reserved blocks 35 and 36 . In this case data is not written to or read from blocks 32 and 34 . Instead, data is written to or read from blocks 35 and 36 . Now, if another block such as block 38 were to go bad, then block 38 would be replaced with a reserved block 40 .
However, when all the bad blocks (including the initial bad blocks), are replaced during the operation, that is, when all the reserved blocks are exhausted, the stability of semiconductor memory device can be no longer guaranteed. At this time, in order to maintain the integrity of the data already stored in the device, the semiconductor memory device automatically goes into a write prohibition state or read-only state. At this time, a user realizes that the life of the memory device is over and therefore executes a memory retention procedure such as, for example, a data backup.
While the integrity of stored data can be maintained as described above, there is no procedure to forewarn the user of the memory device that all the reserved memory blocks are about to be used up. If the user were forewarned, he may be able to take other preventive measures rather than just backing up the data. There is therefore a need for systems and methods which provide memory block state information upon receipt of a request from a user.
SUMMARY
One aspect of the present disclosure includes a method of providing block state information in a semiconductor memory device including a flash memory. The method comprises storing block state information on at least one bad block of the flash memory and a plurality of reserved blocks which replace the at least one bad block, and providing the stored block state information to a user in response to a command provided by the user.
BRIEF DESCRIPTION OF THE DRAWINGS
The present disclosure will become more fully understood from the detailed description given hereinbelow and the accompanying drawings which are given by way of illustration only, and thus are not limitative of the present disclosure, and wherein:
FIGS. 1 and 2 illustrate a configuration of a general flash memory;
FIG. 3 is a block diagram of a semiconductor memory device including a flash memory according to an exemplary disclosed embodiment;
FIG. 4 illustrates a command format of SMART commands according to an exemplary disclosed embodiment;
FIG. 5 illustrates a data structure for a result value of a ‘SMART READ DATA’ command according to an exemplary disclosed embodiment;
FIG. 6 illustrates a data region that provides block state information according to an exemplary disclosed embodiment;
FIG. 7 illustrates a format of a command to control a warning time point according to an exemplary disclosed embodiment; and
FIG. 8 illustrates an output for a command to provide a warning to a user according to an exemplary disclosed embodiment.
DETAILED DESCRIPTION
Exemplary embodiments of the present disclosure will now be described more fully hereinafter with reference to FIGS. 3 to 8 , in which embodiments of the invention are shown. This disclosure may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Unless otherwise defined, all terms (including 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. It will be further understood that terms used herein should be interpreted as having a meaning that is consistent with their meaning in the context of this specification and the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
FIG. 3 is a block diagram of a semiconductor memory device including a flash memory according to an exemplary disclosed embodiment. Referring to FIG. 3 , the semiconductor memory device includes a flash memory 30 and a controller 20 to load a user program 10 .
Data is read from or written to the flash memory 30 via the controller 20 . Specifically, the controller 20 performs a control function such that a given data operation is implemented in the flash memory 30 . Typically, the data operation is performed based on the contents of the user program 10 that is loaded into the controller 20 .
The controller 20 includes a file system 22 which loads the user program 10 , and a flash translation layer (hereinafter, referred to as ‘FTL’) 24 . In an exemplary embodiment, the FTL 24 performs an operation of mapping a logical address generated in the file system with a physical address of the flash memory 30 .
Similar to RAMs, nonvolatile memories, and magnetic memories, the flash memory can be randomly accessed. However, the flash memory is deleted in blocks, unlike RAMs, nonvolatile memories, and magnetic memories. Further, in the case of the flash memory, before writing, deletion is performed in blocks. Furthermore, in general, a data unit in which the deletion operation is performed may be more than a data unit in which the writing operation is performed.
This deletion of large quantities of data may be a problem not only because it may be difficult to use the flash memory as a main memory but also because it may be difficult to keep the file system intact as a general hard disk when using the flash memory as an auxiliary memory device. Thus, in order to hide the deletion operation of the flash memory, the FTL 24 between the file system 22 and the flash memory 30 is used.
Through the address mapping function of the FTL 24 , a host can recognize the flash memory 30 as a hard disk driver, and can access the flash memory device by the same method as the host would access a hard disk driver. The FTL 24 may be realized as a hardware type independent from host system, or may be realized as a device driver type within the host system.
In using the semiconductor memory device described above as an SSD (Solid State Disk) or hard disk, to provide block state information for bad blocks of flash memory and reserved blocks remaining after a replacement for the bad blocks to a user, an exemplary embodiment of the disclosure employs S.M.A.R.T related commands of an ATA (Advanced Technology Attachment) interface.
The SMART is an abbreviation of ‘Self-Monitoring, Analysis and Reporting Technology’. Problems like breakdown causable in the near future relating to a disk driver may be predicted through the SMART function.
Values observed through the SMART function used by different vendors differ based on the vendor. For example, there may be a difference between vendors as to what kinds of formats will be used for reporting values such as, for example, head flying height, data throughput performance, spin-up time, re-allocated sector count, seek time error, seek time performance, spin time performance, spin try recount, and drive calibration retry count.
FIG. 4 illustrates a command format in which SMART commands are classified according to a value of ‘feature register’. The SMART commands shown in FIG. 4 are well known to those skilled in the art, thus its detailed description will be omitted.
In these SMART commands, nine commands, ‘SMART READ DATA(D0h)’, ‘SMART ENABLE/DISABLE ATTRIBUTE AUTOSAVE(D2h)’, ‘SMART SAVE ATTRIBUTE VALUES(D3h)’, ‘SMART EXECUTE OFF-LINE IMMEDIATE(D4h)’, ‘SMART READ LOG(D5h)’, ‘SMART WRITE LOG(D6h)’, ‘SMART ENABLE OPERATIONS(D8h)’, ‘SMART DISABLE OPERATIONS(D9h)’ and ‘SMART RETURN STATUS’, are standardized.
To provide the block state information a ‘SMART READ DATA’ command having a ‘feature register’ value of ‘D0h’ may be used. Furthermore, as a command to provide the block state information, a command, e.g., ‘FFh’, corresponding to one ‘feature register’ value within a range of E0h˜FFh as an area of ‘feature register’ value usable by a vendor, may be used. Additionally, any one of the nine standard commands may be used.
‘F’ indicates that a content of corresponding byte is fixed and unchangeable, and ‘V’ indicates that a content of corresponding byte is variable and changeable. ‘R’ indicates a content of corresponding byte is reserved and it should become ‘0’. ‘X’ designates that a content of corresponding byte is usable by a vendor and may be fixed or variable.
A structure of data for a result value of the ‘SMART READ DATA’ command is shown in FIG. 5 . As shown in FIG. 5 , the data structure of the ‘SMART READ DATA’ command may be constructed of 512 bytes. Specifically, information on reserved blocks, initial bad blocks, additional bad blocks generated during the use of the flash memory, etc. may be stored in vendor-specific data areas (0 th to 361 st bytes and 386 th to 510 th bytes) of the ‘SMART READ DATA’ command. This is shown in FIG. 6 .
For example, as shown in FIG. 6 , information on a version of SMART data may be stored in the 0 th to 1 st bytes, information on the amount of useful information may be stored in the 2 nd to 3 rd bytes, information on the number of reserved blocks may be stored in the 4 th to 7 th bytes, information on the number of additional bad blocks may be stored in the 8 th to 11 th bytes, and information on the number of initial bad blocks may be stored in the 12 th to the 15 th bytes. In addition, in the remaining part of the vendor-specific data areas, other necessary information necessary may be stored.
Block state information for the reserved blocks or bad blocks may be already stored in the ‘FTL’ performing a mapping for blocks or in the meta blocks of the flash memory. Furthermore, a user may obtain information about the number of reserved blocks or bad blocks from the ‘SMART READ DATA’ command.
Additionally, to provide a point of time for execution of an operation such as a user-performed data backup, a warning may be provided to a user when the number of available reserved blocks reaches a reference value. The user may set the reference value, thereby being capable of controlling a warning time point. In an exemplary embodiment, in providing the warning or controlling the warning time point, a specific command in the SMART commands may be used.
As shown in FIG. 4 , for example, when the number of available reserved blocks reaches the reference value, a ‘SMART RETURN STATUS’ command having ‘feature register’ value of ‘DAh’ may be used in the SMART commands, to provide a warning to a user.
In addition, in order to provide warnings to a user, another command having another ‘feature register’ value, for example, ‘FFh’, within a range of E0h˜FFh usable by a vendor may be used. One skilled in the art will appreciate that the commands referred to above are discussed for exemplary purposes only. Commands from other areas may be used without departing from the scope of the disclosure. Furthermore, it may be possible to use any one of the nine standard commands.
The user may also set the reference value to provide a warning at the appropriate time, as described above. In this case, the reference value may be set in a vendor-specific area of a command having one of the ‘Feature register’ values of E0h˜FFh (for example, a command having the ‘Feature register’ value of ‘FFh’). For example, a warning time point may be determined by a command having the ‘Feature register’ value of ‘E0h’. This is shown in FIG. 7 .
FIG. 7 illustrates a format of a command to control a warning time point according to an exemplary disclosed embodiment. As shown in FIG. 7 , an ATA command may be defined as a command code and its accompanying variables. These variables are transferred through different registers. These registers may include, for example, ‘Feature register’, ‘Sector Count register’, ‘Sector Number register’, ‘Cylinder Low register’, ‘Cylinder High register’, ‘Device/Head register’ etc. Furthermore, ‘DEV’ of the ‘Device/Head register’ may indicate whether the semiconductor memory device is used as a master HDD or a slave HDD.
A command to control the warning time point is a sub command of the SMART command whose command code is ‘B0h’. Furthermore, the code of the sub command is ‘E0h’. A user may set the reference value in the ‘Sector Count register’. When the number of available reserved blocks reaches the reference value, a warning is issued.
FIG. 8 illustrates an output provided when a command, e.g., ‘DAh’, to provide a warning to a user, is used. When the semiconductor memory device does not reach the warning time point, the ‘Cylinder Low register’ preserves a setting of ‘4Fh’, and the ‘Cylinder High register’ keeps a setting of ‘C2h’ as shown in FIG. 8 . However, as shown in FIG. 9 , when the semiconductor memory device reaches the warning time point, the ‘Cylinder Low register’ is set as ‘F4h’, and the ‘Cylinder High register’ is set as ‘2Ch’. At this time, a user may execute an operation to back up the stored data so as to maintain the integrity of the stored data.
The disclosed system provides a warning to a user when the number of available reserved blocks reaches the reference value. This warning permits the user to execute an operation such as, for example, a data backup, in order to maintain the integrity of the stored data. In addition, the disclosed system permits the user to set the time point at which the warning is provided. That is, the user can set the reference value to be compared to the number of available reserved blocks, thereby being capable of controlling a warning time point.
It will be apparent to those skilled in the art that modifications and variations can be made in the present disclosure without deviating from the spirit or scope of the disclosure. Thus, it is intended that the present disclosure cover any such modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. Accordingly, these and other changes and modifications are seen to be within the true spirit and scope of the invention as defined by the appended claims. | A method of providing block state information in a semiconductor memory device including a flash memory comprises storing block state information on at least one bad block of the flash memory and a plurality of reserved blocks which replace the at least one bad block, and providing the stored block state information to a user in response to a command provided by the user. | 6 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application is a filing under 35 U.S.C. § 371 and claims priority to international patent application number PCT/GB02/04258 filed Sep. 12, 2002, published on Apr. 17, 2003 as WO03/031612, and to foreign application number 0123856.7 filed in Great Britain on Oct. 5, 2001, the entire disclosures of which are hereby incorporated by reference.
TECHNICAL FIELD
The present invention relates to a novel, non-destructive and dynamic process for determining the cell cycle position of living cells.
BACKGROUND TO THE INVENTION
Eukaryotic cell division proceeds through a highly regulated cell cycle comprising consecutive phases termed G1, S, G2 and M. Disruption of the cell cycle or cell cycle control can result in cellular abnormalities or disease states such as cancer which arise from multiple genetic changes that transform growth-limited cells into highly invasive cells that are unresponsive to normal control of growth. Transition of normal cells into cancer cells can arise though loss of correct function in DNA replication and DNA repair mechanisms. All dividing cells are subject to a number of control mechanisms, known as cell-cycle checkpoints, which maintain genomic integrity by arresting or inducing destruction of aberrant cells. Investigation of cell cycle progression and control is consequently of significant interest in designing anticancer drugs. (Flatt, P. M. and Pietenpol, J. A. Drug Metab. Rev., (2000), 32(3–4), 283–305; Buolamwini, J. K. Current Pharmaceutical Design, (2000), 6, 379–392).
Accurate determination of cell cycle status is a key requirement for investigating cellular processes that affect the cell cycle or are dependent on cell cycle position. Such measurements are particularly vital in drug screening applications where:
i) substances which directly or indirectly modify cell cycle progression are desired, for example, for investigation as potential anti-cancer treatments;
ii) drug candidates are to be checked for unwanted effects on cell cycle progression; and/or
iii) it is suspected that an agent is active or inactive towards cells in a particular phase of the cell cycle.
Traditionally, cell cycle status for cell populations has been determined by flow cytometry using fluorescent dyes which stain the DNA content of cell nuclei (Barlogie, B. et al, Cancer Res., (1983), 43(9), 3982–97). Flow cytometry yields quantitative information on the DNA content of cells and hence allows determination of the relative numbers of cells in the G1, S and G2+M phases of the cell cycle. However, this analysis is a destructive non-dynamic process and requires serial sampling of a population to determine cell cycle status with time. Furthermore, standard flow cytometry techniques examine the total cell population in the sample and yield limited data on individual cells, which precludes study of cell cycle status of different cell types that may be present within the sample under analysis.
EP 798386 describes a method for the analysis of the cell cycle of cell sub-populations present in heterogeneous cell samples. This method uses sequential incubation of the sample with fluorescently labelled monoclonal antibodies to identify specific cell types and a fluorochrome that specifically binds to nucleic acids. This permits determination of the cell cycle distribution of sub-populations of cells present in the sample. However, as this method utilises flow cytometry, it still yields only non-dynamic data and requires serial measurements to be performed on separate samples of cells to determine variations in the cell cycle status of a cell population with time following exposure to an agent under investigation for effects on cell cycle progression.
A further disadvantage of flow cytometry techniques relates to the indirect, and inferred assignment of cell cycle position of cells based on DNA content. Since the DNA content of cell nuclei varies through the cell cycle in a reasonably predictable fashion, ie. cells in G2 or M have twice the DNA content of cells in G1, and cells undergoing DNA synthesis in S phase have an intermediate amount of DNA, it is possible to monitor the relative distribution of cells between different phases of the cell cycle. However, the technique does not allow precision in determining the cell cycle position of any individual cell due to ambiguity in assigning cells to G2 or M phases and to further imprecision arising from inherent variation in DNA content from cell to cell within a population which can preclude precise discrimination between cells which are close to the boundary between adjacent phases of the cell cycle. Additionally, variations in DNA content and DNA staining between different cell types from different tissues or organisms require that the technique is optimised for each cell type, and can complicate direct comparisons of data between cell types or between experiments (Herman, Cancer (1992), 69(6), 1553–1556). Flow cytometry is therefore suitable for examining the overall cell cycle distribution of cells within a population, but cannot be used to monitor the precise cell cycle status of an individual cell over time.
Cell cycle progression is tightly regulated by defined temporal and spatial expression, localisation and destruction of a number of cell cycle regulators which exhibit highly dynamic behaviour during the cell cycle (Pines, J., Nature Cell Biology, (1999), 1, E73–E79). For example, at specific cell cycle stages some proteins translocate from the nucleus to the cytoplasm, or vice versa, and some are rapidly degraded. For details of known cell cycle control components and interactions, see Kohn, Molecular Biology of the Cell (1999), 10, 2703–2734.
One of the most extensively characterised cell cycle regulators in human cells is cyclin B1, temporal and spatial expression and destruction of which controls cell transition from G2 to M and its exit from M. Cyclin B1 expression is driven by a cell cycle phase specific promoter which initiates expression at the end of S phase and peaks during G2. Once expressed, this protein constantly shuttles between the nucleus and the cytoplasm during the G2 phase, but it is primarily cytoplasmic because the rate of its export is much greater than its import. At the start of mitosis, cyclin B1 rapidly translocates into the nucleus, when its rate of import substantially increases, and its export decreases, in a phosphorylation dependent manner ( FIG. 1 ). Thus, the localisation of cyclin B1 in the cell can be used to mark the transition from G2 phase to mitosis. Once a cell reaches metaphase, or, more accurately, when the spindle assembly checkpoint is satisfied, cyclin B1 is very rapidly degraded. Cyclin B1 destruction continues throughout the following G1 phase but stops once cells begin DNA replication. These events have been visualised in real time by micro-injection of fluorescently labelled cyclin B1 into living cells (Clute and Pines, Nature Cell Biology, (1999), 1, 82–87).
The controlling elements which regulate temporal expression and destruction have been elucidated in a number of studies. Biosynthesis of cyclin B1 has been shown to be controlled at the level of transcription by a promoter sequence that confines expression to the late S and G2 phases of the cell cycle (Piaggio et al, Exp. Cell. Research, (1995), 216, 396–402; Cogswell et al, Mol. Cell. Biology, (1995), 15, 2782–2790). Destruction of cyclin B1 at the appropriate time in M phase has been shown to be controlled by a 9 amino acid sequence, termed the destruction box (D-box) which targets the protein for proteolysis via ubiquitinylation. Expression of a Drosophila cyclin B-GFP fusion protein driven by a constitutive polyubiquitin promoter (Huang and Raff, EMBO Journal, (1999), 18(8), 2184–2195) has shown that fluorescently-tagged cyclin B mimics the behaviour of endogenous cyclin B in being degraded at the end of metaphase. Studies (Hagting et al, Current Biology, (1999), 9, 680–689) using human cyclin B1-GFP have shown that temporal changes in cytoplasmic and nuclear localisation of cyclin B1 with cell cycle progression is dependent on a nuclear export signal (NES), phosphorylation of which leads to nuclear import.
Other cell cycle checkpoints are similarly regulated by temporal and spatial control mechanisms and many of the components and interrelationships have been elucidated (Pines, J., Nature Cell Biology, (1999), 1, E73–E79).
A number of methods have been described which make use of certain components of the cell cycle control mechanisms to provide procedures which analyse or exploit cell proliferation status.
WO 00/29602 describes use of a cyclin A promoter to drive expression of GFP as a selectable marker for dividing transgenic stem cells to allow dividing cells to be isolated from a background of non-dividing cells by fluorescence activated cell sorting. While this method allows identification and selection of cells which have progressed past a certain stage in the cell cycle, it does not yield information on the cell cycle status of any given cell, other than historical information that the cell has or has not passed through the G2 phase of the cell cycle at some time in the past.
U.S. Pat. No. 6,048,693 describes a method for screening for compounds affecting cell cycle regulatory proteins, wherein expression of a reporter gene is linked to control elements which are acted on by cyclins or other cell cycle control proteins. In this method, temporal expression of a reporter gene product is driven in a cell cycle specific fashion and compounds acting on one or more cell cycle control components may increase or decrease expression levels. Since the assay system contains no elements which provide for the destruction of the reporter gene product nor for destruction of any signal arising from the reporter gene, the method cannot yield information on the cell cycle position of any cells in the assay and reports only on general perturbations of cell cycle control mechanisms.
U.S. Pat. No. 5,849,508 and U.S. Pat. No. 6,103,887 describe methods for determining the proliferative status of cells by use of antibodies which bind to cyclin A. These methods provide means for determining the percentage of proliferating cells in a test population relative to a control population.
U.S. Pat. No. 6,159,691 relates to a method for assaying for putative regulators of cell cycle progression. In this method, nuclear localisation signals (NLS) derived from the cell cycle phase specific transcription factors DP-3 and E2F-1 are used to assay the activity of compounds which act as agonists or antagonists to increase or decrease nuclear localisation of an NLS fused to a detectable marker.
A number of researchers have studied the cell cycle using traditional reporter molecules that require the cells to be fixed or lysed. For example Hauser and Bauer (Plant and Soil, 2000, 226, p 1–10) used β-glucuronidase (GUS) to study cell division in a plant meristem and Brandeis and Hunt (EMBO J., 1996, vol 15, pp 5280–5289) used chloramphenical acetyl transferase (CAT) fusion proteins to study variations in cyclin levels. Although these methods provide a means of studying the cell cycle position of a particular cell (using GUS) or the average cell cycle status of a population of cells (using CAT) both methods are destructive. Neither method allows the repeated analysis of a specific cell over time and they are therefore not suitable to follow the progression of a cell through the cell cycle.
None of the preceding methods, which use components of the cell cycle control mechanism, provide means for determining the cell cycle status of an individual cell or a population of cells. Consequently, methods are required that enable the cell cycle position of a single living cell to be determined non-destructively, allowing the same cell to be repeatedly interrogated over time, and which enable the study of the effects of agents having potentially desired or undesired effects on the cell cycle. Furthermore, it is desirable for cell cycle position to be determined from a probe controlled directly by cell cycle control components, rather than indirectly through DNA content or other indirect markers of cell cycle position as described above. The present invention describes a method which utilises key components of the cell cycle regulatory machinery in defined combinations to provide novel means of determining cell cycle status for individual living mammalian cells in a non-destructive process providing dynamic read out.
The present invention provides DNA constructs, and cell lines containing such constructs, that exhibit activation and destruction of a detectable reporter molecule in a cell cycle phase specific manner, by direct linkage of reporter signal switching to temporal and spatial expression and destruction of cell cycle components. This greatly improves the precision of determination of cell cycle phase status and allows continuous monitoring of cell cycle progression in individual cells. Furthermore, it has been found that key control elements can be isolated and abstracted from functional elements of the cell cycle control mechanism to permit design of cell cycle phase reporters which are dynamically regulated and operate in concert with, but independently of, endogenous cell cycle control components, and hence provide means for monitoring cell cycle position without influencing or interfering with the natural progression of the cell cycle.
SUMMARY OF THE INVENTION
Accordingly, in a first aspect of the invention, there is provided a nucleic acid reporter construct comprising a nucleic acid sequence encoding a detectable live-cell reporter molecule operably linked to and under the control of:
i) at least one cell cycle phase-specific expression control element, and
ii) a destruction control element;
wherein said reporter construct is expressed in a mammalian cell at a predetermined position in the cell cycle. Expression being defined as all of the processes involved in the biosynthesis of a protein from a gene. It will be further understood that the term ‘live-cell’, as it relates to reporter molecules, defines a reporter molecule which produces a detectable signal in living cells and is therefore suitable for use in live-cell imaging systems.
In a second aspect of the invention, there is provided a method for determining the position in the cell cycle of a mammalian cell said method comprising:
a) expressing in a cell a nucleic acid reporter construct comprising a nucleic acid sequence encoding a detectable live cell-reporter molecule operably linked to and under the control of:
i) at least one cell cycle phase-specific expression control element, and
ii) a destruction control element;
wherein said reporter construct is expressed in a cell at a predetermined point in the cell cycle; and
b) determining the position in the cell cycle by monitoring signals emitted by the reporter molecule.
In preferred embodiments of the first and second aspects, the nucleic acid reporter construct is also linked to and under the control of a cell cycle phase-specific spatial localisation control element.
Suitably, the nucleic acid reporter construct is a DNA construct.
The cell cycle phase-specific expression control element is typically a DNA sequence that controls transcription and/or translation of one or more nucleic acid sequences and permits the cell cycle specific control of expression. Any expression control element that is specifically active in one or more phases of the cell cycle may suitably be used for construction of the cycle position reporter construct.
Suitably, the cell cycle phase specific expression control element may be selected from cell cycle specific promoters and other elements that influence the control of transcription or translation in a cell cycle specific manner. Where the expression control element is a promoter, the choice of promoter will depend on the phase of the cell cycle selected for study.
Suitable promoters include: cyclin B1 promoter (Cogswell et al, Mol. Cell. Biol., (1995), 15(5), 2782–90, Hwang et al, J. Biol. Chem., (1995), 270(47), 28419–24, Piaggio et al, Exp. Cell Res., (1995), 216(2), 396–402); Cdc25B promoter (Korner et al, J. Biol. Chem., (2001), 276(13), 9662–9); cyclin A2 promoter (Henglein et al, Proc. Nat. Acad. Sci. USA, (1994), 91(12), 5490–4, Zwicker et al, Embo J., (1995), 14(18), 4514–22); Cdc2 promoter (Tommasi and Pfeifer, Mol. Cell Biol., (1995), 15(12), 6901–13, Zwicker et al, Embo J (1995), 14(18), 4514–22), Cdc25C promoter (Korner and Muller, J. Biol. Chem., (2000), 275(25), 18676–81, Korner et al, Nucl. Acids Res., (1997), 25(24), 4933–9); cyclin E promoter (Botz et al, Mol. Cell Biol., (1996), 16(7), 3401–9, Korner and Muller, J. Biol. Chem., (2000), 275(25), 18676–81); Cdc6 promoter (Hateboer et al, Mol. Cell Biol., (1998), 18(11), 6679–97, Yan et al, Proc. Nat. Acad. Sci. USA, (1998), 95(7), 3603–8); DHFR promoter (Shimada et al, J. Biol. Chem., (1986), 261(3), 1445–52, Shimada and Nienhuis, J. Biol. Chem., (1985), 260(4), 2468–74) and histones promoters (van Wijnen et al, Proc. Nat. Acad. Sci. USA, (1994), 91, 12882–12886).
Suitably, the cell cycle phase specific expression control element may be selected from cell cycle specific IRES elements and other elements that influence the control of translation in a cell cycle specific manner. An IRES element is an internal ribosomal entry site that allows the binding of a ribosome and the initiation of translation to occur at a region of mRNA which is not the 5′-capped region. A cell cycle-specific IRES element restricts cap-independent initiation of translation to a specific stage of the cell cycle (Sachs, A. B., Cell, (2000), 101, 243–5). Where the expression control element is selected to be an IRES, suitably its selection will depend on the cell cycle phase under study. In this case, a constitutively expressed (eg. CMV or SV40) or inducible (eg. pTet-on pTet-off system, Clontech) promoter may be used to control the transcription of the bicistronic mRNA (Sachs, A. B., Cell, (2000), 101, 243–5). Alternatively, a non cell cycle phase-dependent IRES element (eg. the EMCV IRES found in pIRES vectors, BD Clontech) may be used in conjunction with a cell cycle specific promoter element. Alternatively, more precise control of expression of the reporter may be obtained by using a cell cycle phase specific promoter in conjunction with a cell cycle phase specific IRES element.
IRES elements suitable for use in the invention include: G2-IRES (Cornelis et al, Mol. Cell, (2000), 5(4), 597–605); HCV IRES (Honda et al, Gastroenterology, (2000), 118, 152–162); ODC IRES (Pyronet et al, Mol. Cell, (2000), 5, 607–616); c-myc IRES (Pyronnet et al, Mol. Cell, (2000), 5(4), 607–16) and p58 PITSLRE IRES (Cornelis et al, Mol. Cell, (2000), 5(4), 597–605).
Table 1 lists some preferred expression control elements that may be used in accordance with the invention, and indicates the cell cycle phase in which each element is activated.
TABLE 1 Cell Cycle Phase-Specific Expression Control Elements Element Timing Element Timing Cyclin B1 promoter G2 DHFR promoter late G1 Cdc25B promoter S/G2 Histones promoters late G1/S Cyclin A2 promoter S G2-IRES G2 Cdc2 promoter S HCV IRES M Cdc25C promoter S ODC IRES G2/M Cyclin E promoter late G1 c-myc IRES M Cdc6 promoter late G1 p58 PITSLRE IRES G2/M
The destruction control element is a DNA sequence encoding a protein motif that controls the destruction of proteins containing that sequence. Suitably, the destruction control element may be cell cycle mediated, for example: Cyclin B1 D-box (Glotzer et al, Nature, (1991), 349, 132–138, Yamano et al, EMBO J., (1998), 17(19), 5670–8, Clute and Pines, Nature Cell Biology, (1999), 1, 82–87); cyclin A N-terminus (den Elzen and Pines, J. Cell Biol., (2001), 153(1), 121–36, Geley et al, J. Cell Biol., (2001), 153, 137–48); KEN box (Pfleger and Kirschner, Genes Dev, (2000), 14(6), 655–65), Cyclin E (Yeh et al, Biochem Biophys Res Commun., (2001) 281, 884–90), Cln2 cyclin from S. cerevisiae (Berset et al, Mol. Cell Biol., (2002), pp 4463–4476) and p27Kip1 (Montagnoli et al, Genes Dev., (1999), 13(9), 1181–1189, Nakayama et al, EMBO J., (2000), 19(9), 2069–81, Tomoda et al, Nature, (1999), 398(6723), 160–5).
Table 2 lists destruction control elements that may be used according to the invention and indicates the cell cycle phase in which each element is activated.
Alternatively, the destruction control element may be non cell-cycle mediated, such as PEST sequences as described by Rogers et al, Science, (1986), 234, 364–8. Examples of non cell-cycle mediated destruction control elements include sequences derived from casein, ornithine decarboxylase and proteins that reduce protein half-life. Use of such non cell-cycle mediated destruction control sequences in the method of the invention provides means for determining the persistence time of the cell cycle reporter following induction of expression by a cell cycle specific promoter.
TABLE 2 Destruction Control Elements Element Timing Cyclin B1 D-box Metaphase through to G1 phase Cyclin A N-terminus Prometaphase through to G1 phase KEN box anaphase/G1 p27Kip1 G1 Cyclin E G1/S boundary Cln2 G1/S boundary
Suitably, the live-cell reporter molecule encoded by the nucleic acid sequence may be selected from the group consisting of fluorescent proteins and enzymes. Preferred fluorescent proteins include Green Fluorescent Protein (GFP) from Aequorea Victoria and derivatives of GFP such as functional GFP analogues in which the amino acid sequence of wild type GFP has been altered by amino acid deletion, addition, or substitution. Suitable GFP analogues for use in the present invention include EGFP (Cormack, B. P. et al, Gene, (1996), 173, 33–38); EYFP and ECFP (U.S. Pat. No. 6,066,476, Tsien, R. et al); F64L-GFP (U.S. Pat. No. 6,172,188, Thastrup, O. et al); BFP, (U.S. Pat. No. 6,077,707, Tsien, R. et al). Other fluorescent proteins include DsRed, HcRed and other novel fluorescent proteins (BD Clontech and Labas, Y. A. et al, Proc Natl Acad Sci USA (2002), 99, 4256–61) and Renilla GFP (Stratagene). Suitable enzyme reporters are those which are capable of generating a detectable (e.g. a fluorescent or a luminescent) signal in a substrate for that enzyme. Particularly suitable enzyme/substrates include: nitroreductase/Cy-Q (as disclosed in WO 01/57237) and β-lactamase/CCF4.
In a preferred embodiment according to the present invention, the nucleic acid reporter construct may optionally include a cell cycle phase-specific spatial localisation control element comprising a DNA sequence encoding a protein motif that is capable of controlling the sub-cellular localisation of the protein in a cell cycle specific manner. Such a localisation control element may be used advantageously according to the invention where:
i) a specific sub-cellular localisation of the reporter is desirable; and/or
ii) more precise determination of the cell cycle position is required.
It may be required to determine the sub-cellular localisation of the reporter either to ensure its effective operation and/or destruction. More precise determination of the cell cycle position may be possible using a localisation control element since this will permit measurement of both intensity and location of the reporter signal.
Suitable spatial localisation control elements include those that regulate localisation of a cell cycle control protein, for example the cyclin B1 CRS.
The term, operably linked indicates that the elements are arranged so that they function in concert for their intended purposes, e.g. transcription initiates in a promoter and proceeds through the DNA sequence coding for the fluorescent protein of the invention. FIG. 2 ( 2 A/ 2 B/ 2 C) illustrates the general construction of a DNA construct according to the invention.
In a preferred aspect of the invention, the construct comprises a cyclin B1 promoter, a cyclin B1 destruction box (D-box), a cyclin B1 cytoplasmic retention sequence (CRS) and a green fluorescent protein (GFP).
In a particular example according to the present invention, the nucleic acid reporter construct comprises an expression vector comprising the following elements:
a) a vector backbone comprising:
i) a bacterial origin of replication; and
ii) a bacterial drug resistance gene;
b) a cell cycle phase specific expression control element;
c) a destruction control element; and
d) a nucleic acid sequence encoding a reporter molecule.
Optionally, the nucleic acid reporter construct additionally contains a cell cycle phase-specific spatial localisation control element and/or a eukaryotic drug resistance gene, preferably a mammalian drug resistance gene.
Expression vectors may also contain other nucleic acid sequences, such as polyadenylation signals, splice donor/splice acceptor signals, intervening sequences, transcriptional enhancer sequences, translational enhancer sequences and the like. Optionally, the drug resistance gene and the reporter gene may be operably linked by an internal ribosome entry site (IRES), which is either cell cycle specific (Sachs, et al, Cell, (2000), 101, 243–245) or cell cycle independent (Jang et al, J. Virology, (1988), 62, 2636–2643 and Pelletier and Sonenberg, Nature, (1988), 334, 320–325), rather than the two genes being driven from separate promoters. When using a non cell-cycle specific IRES element the pIRES-neo and pIRES-puro vectors commercially available from Clontech may be used.
In a particular embodiment of the first aspect, the nucleic acid reporter construct is assembled from a DNA sequence encoding the cyclin B1 promoter operably linked to DNA sequences encoding 171 amino acids of the amino terminus of cyclin B1 and a DNA sequence encoding a green fluorescent protein (GFP) ( FIG. 3 ). Motifs controlling the localisation and destruction of cyclin B1 have all been mapped to ˜150 amino acids in the amino terminus of the molecule. Consequently, an artificial cell cycle marker can be constructed using only sequences from the amino terminus of cyclin B1, which will not interfere with cell cycle progression since it lacks a specific sequence, termed the cyclin box, (Nugent et al, J. Cell. Sci., (1991), 99, 669–674) which is required to bind to and activate a partner kinase. Key regulatory motifs required from the amino terminus sequence of cyclin B1 are: i) a nine amino acid motif termed the destruction box (D-box). This is necessary to target cyclin B1 to the ubiquitination machinery and, in conjunction with at least one C-terminal lysine residue, this is also required for its cell-cycle specific degradation; ii) an approximately ten amino acid nuclear export signal (NES). This motif is recognised, either directly or indirectly, by exportin 1 and is sufficient to maintain the bulk of cyclin B1 in the cytoplasm throughout interphase; iii) approximately four mitosis-specific phosphorylation sites that are located in and adjacent to the NES and confer rapid nuclear import and a reduced nuclear export at mitosis. When expressed in a eukaryotic cell, the construct will exhibit cell cycle specific expression and destruction of the GFP reporter which parallels the expression and degradation of endogenous cyclin B1. Hence, measurement of GFP fluorescence intensity permits identification of cells in the G2/M phase of the cell cycle ( FIG. 4 ). Furthermore, since the fluorescent product of the construct will mimic the spatial localisation of endogenous cyclin B1, analysis of the sub-cellular distribution of fluorescence permits further precision in assigning cell cycle position. At prophase, cyclin B1 rapidly translocates into the nucleus, consequently the precise localisation of GFP fluorescence in the cell can be used to discriminate cells transitioning from interphase to mitosis. Once a cell reaches metaphase, and the spindle assembly checkpoint is satisfied, cyclin B1 is very rapidly degraded, and consequently the disappearance of GFP fluorescence can be used to identify cells at mid-M phase.
Expression of the construct in a population of unsynchronised cells will result in each cell exhibiting cyclical expression and destruction of the fluorescent product from the construct, resulting in a continuous blinking pattern of fluorescence from all cells in the population. Analysis of the fluorescence intensity of each cell with time consequently yields dynamic information on the cell cycle status of each cell as illustrated in FIG. 4 .
Further embodiments of the nucleic acid reporter construct according to the first aspect may be constructed by selecting suitable alternative cell cycle control elements, for example from those shown in Tables 1 and 2, to design cell cycle phase reporters which report a desired section of the cell cycle.
The construction and use of expression vectors and plasmids are well known to those of skill in the art. Virtually any mammalian cell expression vector may be used in connection with the cell cycle markers disclosed herein. Examples of suitable vector backbones which include bacterial and mammalian drug resistance genes and a bacterial origin of replication include, but are not limited to: pCl-neo (Promega), pcDNA (Invitrogen) and pTriEx1 (Novagen). Suitable bacterial drug resistance genes include genes encoding for proteins that confer resistance to antibiotics including, but not restricted to: ampicillin, kanamycin, tetracyclin and chloramphenicol. Eurkaryotic drug selection markers include agents such as: neomycin, hygromycin, puromycin, zeocin, mycophenolic acid, histidinol, gentamycin and methotrexate.
The DNA construct may be prepared by the standard recombinant molecular biology techniques of restriction digestion, ligation, transformation and plasmid purification by methods familiar to those skilled in the art and are as described in Sambrook, J. et al (1989), Molecular Cloning—A Laboratory Manual, Cold Spring Harbor Laboratory Press. Alternatively, the construct can be prepared synthetically by established methods, eg. the phosphoramidite method described by Beaucage and Caruthers, (Tetrahedron Letters, (1981), 22, 1859–1869) or the method described by Matthes et al (EMBO J., (1984), 3, 801–805). According to the phosphoramidite method, oligonucleotides are synthesised, eg. in an automatic DNA synthesizer, purified, annealed, ligated and cloned into suitable vectors. The DNA construct may also be prepared by polymerase chain reaction (PCR) using specific primers, for instance, as described in U.S. Pat. No. 4,683,202 or by Saiki et al (Science, (1988), 239, 487–491). A review of PCR methods may be found in PCR protocols, (1990), Academic Press, San Diego, Calif., U.S.A.
During the preparation of the DNA construct, the gene sequence encoding the reporter must be joined in frame with the cell cycle phase specific destruction control element and optionally the spatial localisation control element. The resultant DNA construct should then be placed under the control of one or more suitable cell cycle phase specific expression control elements.
In a third aspect, there is provided a host cell transfected with a nucleic acid reporter construct according to the present invention. The host cell into which the construct or the expression vector containing such a construct is introduced, may be any mammalian cell which is capable of expressing the construct.
The prepared DNA reporter construct may be transfected into a host cell using techniques well known to the skilled person. One approach is to temporarily permeabilise the cells using either chemical or physical procedures. These techniques may include: electroporation (Tur-Kaspa et al, Mol. Cell Biol. (1986), 6, 716–718; Potter et al, Proc. Nat. Acad. Sci. USA, (1984), 81, 7161–7165), a calcium phosphate based method (eg. Graham and Van der Eb, Virology, (1973), 52, 456–467 and Rippe et al, Mol. Cell Biol., (1990), 10, 689–695) or direct microinjection.
Alternatively, cationic lipid based methods (eg. the use of Superfect (Qiagen) or Fugene6 (Roche) may be used to introduce DNA into cells (Stewart et al, Human Gene Therapy, (1992), 3, 267; Torchilin et al, FASEB J, (1992), 6, 2716; Zhu et al, Science, (1993), 261, 209–211; Ledley et al, J. Pediatrics, (1987), 110, 1; Nicolau et al, Proc. Nat. Acad. Sci., USA, (1983), 80, 1068; Nicolau and Sene, Biochem. Biophys. Acta, (1982), 721, 185–190). Jiao et al, Biotechnology, (1993), 11, 497–502) describe the use of bombardment mediated gene transfer protocols for transferring and expressing genes in brain tissues which may also be used to transfer the DNA into host cells.
A further alternative method for transfecting the DNA construct into cells, utilises the natural ability of viruses to enter cells. Such methods include vectors and transfection protocols based on, for example, Herpes simplex virus (U.S. Pat. No. 5,288,641), cytomegalovirus (Miller, Curr. Top. Microbiol. Immunol., (1992), 158, 1), vaccinia virus (Baichwal and Sugden, 1986, in Gene Transfer, ed. R. Kucherlapati, New York, Plenum Press, p 117–148), and adenovirus and adeno-associated virus (Muzyczka, Curr. Top. Microbiol. Immunol., (1992), 158, 97–129).
Examples of suitable recombinant host cells include HeLa cells, Vero cells, Chinese Hamster ovary (CHO), U2OS, COS, BHK, HepG2, NIH 3T3 MDCK, RIN, HEK293 and other mammalian cell lines that are grown in vitro. Such cell lines are available from the American Tissue Culture Collection (ATCC), Bethesda, Md., U.S.A. Cells from primary cell lines that have been established after removing cells from a mammal followed by culturing the cells for a limited period of time are also intended to be included in the present invention.
Cell lines which exhibit stable expression of a cell cycle position reporter may also be used in establishing xenografts of engineered cells in host animals using standard methods. (Krasagakis, K. J et al, Cell Physiol., (2001), 187(3), 386–91; Paris, S. et al, Clin. Exp. Metastasis, (1999), 17(10), 817–22). Xenografts of tumour cell lines engineered to express cell cycle position reporters will enable establishment of model systems to study tumour cell division, stasis and metastasis and to screen new anticancer drugs.
Use of engineered cell lines or transgenic tissues expressing a cell cycle position reporter as allografts in a host animal will permit study of mechanisms affecting tolerance or rejection of tissue transplants (Pye D and Watt, D. J., J. Anat., (2001), 198 (Pt 2), 163–73; Brod, S. A. et al, Transplantation (2000), 69(10), 2162–6).
To perform the method for determining the cell cycle position of a cell according to the second aspect, cells transfected with the DNA reporter construct may be cultured under conditions and for a period of time sufficient to allow expression of the reporter molecule at a specific stage of the cell cycle. Typically, expression of the reporter molecule will occur between 16 and 72 hours post transfection, but may vary depending on the culture conditions. If the reporter molecule is based on a green fluorescent protein sequence the reporter may take a defined time to fold into a conformation that is fluorescent. This time is dependent upon the primary sequence of the green fluorescent protein derivative being used. The fluorescent reporter protein may also change colour with time (see for example, Terskikh, Science, (2000), 290, 1585–8) in which case imaging is required at specified time intervals following transfection.
The cell cycle position of the cells may be determined by monitoring the expression of the reporter molecule and detecting signals emitted by the reporter using an appropriate detection device. If the reporter molecule produces a fluorescent signal, then, either a conventional fluorescence microscope, or a confocal based fluorescence microscope may be used. If the reporter molecule produces luminescent light, then a suitable device such as a luminometer may be used. Using these techniques, the proportion of cells expressing the reporter molecule may be determined. If the DNA construct contains translocation control elements and the cells are examined using a microscope, the location of the reporter may also be determined. In the method according to the present invention, the fluorescence of cells transformed or transfected with the DNA construct may suitably be measured by optical means in for example; a spectrophotometer, a fluorimeter, a fluorescence microscope, a cooled charge-coupled device (CCD) imager (such as a scanning imager or an area imager), a fluorescence activated cell sorter, a confocal microscope or a scanning confocal device, where the spectral properties of the cells in culture may be determined as scans of light excitation and emission.
In the embodiment of the invention wherein the nucleic acid reporter construct comprises a drug resistance gene, following transfection and expression of the drug resistance gene (usually 1–2 days), cells expressing the modified reporter gene may be selected by growing the cells in the presence of an antibiotic for which transfected cells are resistant due, to the presence of a selectable marker gene. The purpose of adding the antibiotic is to select for cells that express the reporter gene and that have, in some cases, integrated the reporter gene, with its associated promoter, IRES elements, enhancer and termination sequences into the genome of the cell line. Following selection, a clonal cell line expressing the construct can be isolated using standard techniques. The clonal cell line may then be grown under standard conditions and will express reporter molecule and produce a detectable signal at a specific point in the cell cycle.
Cells transfected with the nucleic acid reporter construct according to the present invention may be grown in the absence and/or the presence of a test system to be studied and whose effect on the cell cycle of a cell is to be determined. By determining the proportion of cells expressing the reporter molecule and, optionally, the localisation of the signal within the cell, it is possible to determine the effect of the test system on the cell cycle of the cells, for example, whether the test system arrests the cells in a particular stage of the cell cycle, or whether the effect is to speed up or slow down cell division.
Thus, in a fourth aspect, there is provided a method of determining the effect of a test system on the cell cycle position of a mammalian cell, said method comprising:
a) expressing in a cell in the absence and in the presence of said test system a nucleic acid reporter construct comprising a nucleic acid sequence encoding a detectable live-cell reporter molecule operably linked to and under the control of:
i) at least one cell cycle phase-specific expression control element, and
ii) a destruction control element;
wherein said reporter construct is expressed in a cell at a predetermined point in the cell cycle; and
b) determining the cell cycle position by monitoring signals emitted by the reporter molecule wherein a difference between the emitted signals measured in the absence and in the presence of said test system is indicative of the effect of said test system on the cell cycle position of said cell.
In a fifth aspect, there is provided a method of determining the effect of a test system on the cell cycle position of a mammalian cell, the method comprising:
a) expressing in the cell in the presence of the test system a nucleic acid reporter construct comprising a nucleic acid sequence encoding a detectable live-cell reporter molecule operably linked to and under the control of:
i) at least one cell cycle phase-specific expression control element, and
ii) a destruction control element;
wherein the reporter construct is expressed in a cell at a predetermined point in the cell cycle; and
b) determining the cell cycle position by monitoring signals emitted by the reporter molecule, c) comparing the emitted signal in the presence of the test system with a known value for the emitted signal in the absence of the test system;
wherein a difference between the emitted signal measured in the presence of the test system and the known value in the absence of the test system is indicative of the effect of the test system on the cell cycle position of the cell.
In a sixth aspect, there is provided a method of determining the effect of a test system on the cell cycle position of a mammalian cell, said method comprising:
a) providing cells containing a nucleic acid reporter construct comprising a nucleic acid sequence encoding a detectable live-cell reporter molecule operably linked to and under the control of:
i) at least one cell cycle phase-specific expression control element, and
ii) a destruction control element;
wherein the reporter construct is expressed in a cell at a predetermined point in the cell cycle;
b) culturing first and second populations of the cells respectively in the presence and absence of a test system and under conditions permitting expression of the nucleic acid reporter construct; and
c) measuring the signals emitted by the reporter molecule in the first and second cell populations;
wherein a difference between the emitted signals measured in the first and second cell populations is indicative of the effect of the test system on the cell cycle position of the cell.
By the term test system, it is intended to mean an agent such as a drug, hormone, protein, peptide, nucleic acid and the like, to which the cell is exposed. Alternatively, the test system may be an agent such as a nucleic acid, peptide or protein that is expressed in the cell under study. For example, cells transfected with the nucleic acid reporter constructs according to the present invention may be used to determine whether expression of cDNA containing constructs encoding proteins under study have an effect on the cell cycle position of a cell. A series of cDNAs, inserted into a mammalian expression vector, may be transiently transfected into a cell stably expressing the cell cycle position reporter. By monitoring the expression and location of the nucleic acid reporter construct in these transfected cells, it is possible to determine the effects of the proteins encoded by the cDNAs on the cell cycle.
The cell cycle position nucleic acid reporter constructs according to the present invention may also be used in a method to determine the effect of the cell cycle position on a cellular process, or to determine the effect of the cell cycle position on the action of a test substance on a cellular process. It is well known that many cellular processes, including those that respond to external stimuli, are influenced by the cell cycle so as to operate or respond differently at different stages of the cell cycle. For example, endothelin receptors have been shown to be expressed at different levels during different phases of the cell cycle (Okazawa et al. J. Biol. Chem., (1998), 273, 12584–12592) and consequently the sensitivity of cells to endothelin induced apoptosis varies with the cell cycle position. Similarly, cellular Ca 2+ mobilisation responses to vasopressin differ according to cell cycle position (Abel et al. J. Biol. Chem., (2000), 275, 32543–32551) due to variations in the route of signal transduction which utilise different G-proteins at different cell cycle phases. Use of the cell cycle position reporter constructs will allow cell to cell variations in a biological assay, measured using an appropriate assay reporter, to be correlated with the signal from a cell cycle position reporter in order to determine if any variations in the assay signal correlate with the cell cycle position reporter signal and hence determine any cell cycle dependence of the assay signal. For example, assays may be devised in which the amount of a red fluorescently labelled ligand bound to a cell surface receptor is correlated with cell cycle status determined using a GFP cell cycle position reporter. By cellular process, it is meant the normal processes which living cells undergo and includes: biosynthesis, uptake, transport, receptor binding, metabolism, fusion, biochemical response, growth and death.
Two or more cell cycle position nucleic acid reporter constructs may be used in combination in applications that include reporting on transition through two or more, cell cycle phases within the same cell. To achieve such duplex or multiplex reporting, two or more different constructs are engineered and expressed in the same cell, wherein each reporter construct comprises a different combination of control elements linked to a different and distinguishable reporter. For example, cellular expression of a construct comprising a cyclin B1 promoter and cyclin B1 D-box operably linked to GFP in combination with expression in the same cell of a second construct comprising a cyclin A2 promoter and cyclin B1 D-box operably linked to blue fluorescent protein (BFP) will allow discrimination of cells in S phase (blue fluorescence) from cells in G2/M phase (blue and green fluorescence).
The cell cycle position nucleic acid reporter constructs and assay methods according to the present invention may be used in a variety of additional applications, for example:
i) Cells transfected with the cell cycle position reporter constructs of the present invention may be used to determine the effect of the cell cycle on the expression, translocation or subcellular distribution of a second marker in a multiplexed assay. For example, if the intracellular translocation of a fluorescent reporter to the plasma membrane is being studied and it is found that a test compound results in translocation in a percentage of the cells, then, using cells transfected with a construct according to the invention, it is possible to determine whether the translocation was cell cycle dependent.
Thus, in a seventh aspect of the invention there is provided a method of determining the effect of the mammalian cell cycle on the expression, translocation or sub-cellular distribution of a first detectable reporter which is known to vary in response to a test system, the method comprising:
a) expressing in the cell in the presence of the test system a second nucleic acid reporter construct comprising a nucleic acid sequence encoding a detectable live-cell reporter molecule operably linked to and under the control of:
i) a cell cycle phase-specific expression control element, and
ii) a destruction control element;
wherein the reporter construct is expressed in a cell at a predetermined point in the cell cycle;
b) determining the cell cycle position by monitoring signals emitted by the second reporter molecule; c) monitoring the signals emitted by the first detectable reporter,
wherein the relationship between cell cycle position determined by step b) and the signal emitted by the first detectable reporter is indicative of whether or not the expression, translocation or sub-cellular distribution of the first detectable reporter is cell cycle dependent. The term ‘test system’ is to be understood as hereinbefore described in relation to the fourth, fifth and sixth aspect of the present invention.
ii) Cell cycle position reporters of the present invention may be used in combination with analysis of endogenous cellular markers or phenomena that are cell cycle related, in order to gain further information on the cell cycle status of an individual cell or a cell population. For example, it is well known that the Golgi complex has a distinctive morphology in mammalian cells, comprising a ribbon like structure adjacent to the nucleus, and that distinctive changes occur in the structure of the Golgi as cells undergo mitosis as the ribbon structure is converted to clusters of vesicles and tubules dispersed throughout the mitotic cell. (Lowe et al., Trends Cell Biol., (1998), 8(1) 40–44). Analysis of the morphology of cell components, such as the Golgi apparatus, which vary in a known fashion with cell cycle progression, for example by use of specific fluorescent stains, may be used in combination with a cell cycle position reporter to enable more detailed analysis of cell cycle progression.
iii) The cell cycle position reporters according to the present invention may also be used for monitoring cell cycle status and progression in in-vivo applications. For example, the introduction of a DNA construct encoding a cell cycle reporter into living specimens such as Xenopus oocytes, and living organisms such as C. elegans and Drosophila , via transfection of individual cells or multiple cells can be achieved by microinjection (Krone P. H., and Heikkila J. J., Development, (1989), 106(2), 271–81), ballistic injection (Horard B. et al., Insect Mol. Biol., (1994), 3(4), 61–5), and other methods well known to the skilled person. Introduction of cell cycle reporter constructs into such specimens will enable investigation of cell cycle progression and control in cell progeny of transfected cells. Information from reporters is likely to be of significant value in study of growth and development in model organisms.
iv) The reporters of the present invention may be used in the generation of transgenic organisms, ie. where the DNA encoding the cell cycle position reporter is stably expressed in all cells of an organism or animal. Such transgenic organisms may be generated by microinjecting DNA into an early embryo, generally into one of the pronuclei of a newly fertilized egg. (Bishop J. O., Reprod. Nutr. Dev., (1996), 36(6), 607–18). Transgenic techniques may be used to engineer cell cycle position reporters into a range of host species from simple organisms such as C. elegans (Daniells, C. et al, Mutat. Res., (1998), 399(1), 55–64) to more complex organisms such as mice and rats (Sills, R. C., et al., Toxicol. Lett., (2001), 20(1–3), 187–98). Establishment of stable transgenic expression of a cell cycle position reporter in all cells of a transgenic organism will allow cell cycle status to be determined in any cell type within, or isolated from, the organism, including cultured cell lines derived from the organism. Accordingly, in an eighth aspect of the present invention there is provide a transgenic organism comprising a cell as hereinbefore described.
v) Cell lines that exhibit stable expression of a cell cycle position reporter may also be used in establishing xenografts of engineered cells in host animals using standard methods. (Krasagakis, K. J et al, Cell Physiol., (2001), 187(3), 386–91; Paris, S. et al, Clin. Exp. Metastasis, (1999), 17(10), 817–22). Thus, in a ninth aspect of the present invention, there is provided a cell line comprising a cell as hereinbefore described for use in establishing xenografts in a host organism. Xenografts of tumour cell lines engineered to express cell cycle position markers will enable establishment of model systems to study tumour cell division, stasis and metastasis and to screen new anticancer drugs.
vi) Use of engineered cell lines or transgenic tissues expressing a cell cycle position reporter as allografts in a host animal will permit study of mechanisms affecting tolerance or rejection of tissue transplants (Pye, D. and Watt, D. J., J. Anat., (2001), 198(Pt 2), 163–73; Brod, S. A. et al, Transplantation (2000), 69(10), 2162–6). Therefore, in a tenth aspect of the present invention there is provided a cell line comprising a cell as hereinbefore described for use in establishing allografts in a host organism.
In an eleventh aspect of the present invention there is provided a transgenic organism comprising a cell as hereinbefore described.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is further illustrated by reference to the following examples and figures in which:
FIG. 1 is a schematic diagram illustrating cyclin B1 regulation during cell cycle progression. The cell cycle proceeds in the direction of the arrow with cyclin B1 expression driven by a cell cycle phase-specific promoter which initiates expression at the end of the S phase and peaks during G2 (A). At the start of mitosis (B) cyclin B1 translocates from the cytoplasm to the nucleus and from metaphase onwards (C) the protein is specifically degraded.
FIG. 2 is a schematic diagram illustrating cell cycle position nucleic acid reporter constructs according to the present invention and in which, 2 A utilises a cell cycle phase-specific promoter and no IRES element, 2 B utilises an IRES element to facilitate mammalian selection, and 2 C contains a constituitive or inducible mammalian promoter and a cell cycle phase-specific IRES as the expression control element. In each case A represents a cell cycle phase-specific expression control (promoter), B represents a cell cycle phase specific destruction control element, C represents a cell cycle phase specific localisation control element, D represents a reporter gene, E represents a non-cell cycle specific IRES element, F represents a mammalian selectable marker, G represents a mammalian constitutive promoter and H represents a cell cycle specific IRES element.
FIG. 3 shows a DNA construct for determining the G2/M phase of the cell cycle, the construct containing a cyclin B1 promoter (A), cyclin B1 destruction box (D-box) (B), cyclin B1 CRS(C) and a GFP reporter (D).
FIG. 4 illustrates the expression of a nucleic acid construct expressing the G2/M cell cycle phase marker in a population of unsynchronised cells. Each cell exhibits cyclical expression and destruction of the fluorescent product from the construct, resulting in a continuous “blinking” pattern of fluorescence from all cells in the population. Analysis of the fluorescence intensity of each cell at times 1, 2, 3 and 4 yields dynamic information on the cell position status of each cell.
FIG. 5 is a bar chart showing the effect of cell cycle blocking agents on GFP fluorescence from a cell cycle phase marker according to the invention. A represents cells inhibited in mitosis by demecolchicine, B represents control cells and C represents cells inhibited at G1/S phase by mimosine;
FIG. 6 is a series of time lapse photographs showing a cell that has been microinjected with the construct described in Example 1 and undergoing mitosis according to Example 3. Differential interference contrast (DIC) images are shown on the left with the corresponding fluorescence image on the right. Frame A shows a cell (arrowed) in metaphase which shows bright fluorescence in the nucleus. Frames B and C show the same cell at later times in anaphase (B) and late anaphase (C). The DIC images of B and C show the division of the cell into two daughter cells (indicated by 2 arrows), the corresponding fluorescence images show the loss of fluorescence accompanying destruction of the fluorescent construct as the cell cycle progresses.
FIG. 7 is a series of time lapse photographs showing a U2-OS cell expressing the construct described in Example 1 undergoing mitosis according to Example 4. In panel A the cell on the left is in G2-phase of the cell cycle, in panel B the cell has entered prophase, in panel C the cell is in metaphase, in panel D the cell is in telophase and in panel E the two daughter cells are non-fluorescent and in G1 phase.
FIG. 8 is a graph showing the relative fluorescence of a U2-OS cell and its progeny that are stably expressing the construct described in Example 1 according to Example 4. The cell undergoes mitosis (A) after 4 hours and divides into two daughter cells (1,2). Daughter 1 then undergoes mitosis (B) at 34 hours dividing into two granddaughters (1.1 and 1.2) and Daughter 2 undergoes mitosis at 42 hours (C) dividing into granddaughters (2.1 and 2.2). The bold arrows show the increase in fluorescence of the daughter cells during G2-phase and prior to mitosis.
FIG. 9 is a FACS analysis showing the effect of cell cycle inhibitors upon the relative green fluorescence intensity of the stable cell line described in Example 5 according to Example 6. The histograms (on the left) show number of cells (Y-axis) against propidium iodide staining with FL3A (red fluorescence) and the dot-plots (on the right) show the same cells plotted with FL1H (green fluorescence, Y-axis) against FL3A (X-axis). The top two graphs show control cells that have not been treated with a cell cycle inhibitor. As can be seen these cells show the typical cell cycle profile (A) and have a diagonal pattern indicating that cells with more GFP are in the G2/M part of the cell cycle. The middle two graphs show cells that have been blocked in G2/M by colchicine (C). The majority of these cells have a relatively high green fluorescence (D). The bottom two graphs show cells that have been partially blocked in G1/S by mimosine (E). The majority of these cells have a relatively low green fluorescence (F).
DETAILED DESCRIPTION OF THE INVENTION
Examples
1. Preparation of DNA Construct
i) The N-terminal third of the cyclin B1 mRNA (amino acids 1–171), encoding the cyclin B1 destruction box and the NES was amplified with HindIII and BamHI ends using standard PCR techniques and the following primers:
SEQ ID NO:1: GGGAAGCTTAGGATGGCGCTCCGAGTCACCAGGAAC
SEQ ID NO:2: GCCGGATCCCACATATTCACTACAAAGGTT.
ii) The gene for wtGFP was amplified with primers designed to introduce restriction sites that would facilitate construction of fusion proteins. The PCR product was cloned into pTARGET (Promega) according to manufacturer's instructions and mutations (F64L/S175G/E222G) were introduced using the QuikChange site-directed mutagenesis kit (Stratagene). Constructs were verified by automated DNA sequencing. DNA encoding the mutant GFP was then cloned downstream of the cyclin B1 N-terminal region using BamHI and SalI restriction sites.
iii) The cell cycle dependent region of the cyclin B1 promoter (−150→+182) was amplified with SaclI and HindIII sites and cloned upstream of the Cyclin B1 N-terminal region and the GFP fusion protein.
iv) The promoter and recombinant protein encoding DNA was excised and cloned in place of the CMV promoter in a BglII/NheI cut pCl-Neo derived vector.
2. Effect of Cell Cycle Blocking Agents on GFP Fluorescence from Cell Cycle Phase Marker Using Transiently Transfected Cells.
U20S cells (ATCC HTB-96) were cultured in wells of a 96 well microtitre plate. Cells were transfected with a cell cycle reporter construct prepared according to Example 1, comprising a cyclin B1 promoter operably linked to sequences encoding the cyclin B1 D-box, the cyclin B1 CRS, and GFP in a pCORON4004 vector (Amersham Biosciences) using Fugene 6 (Roche) as the transfection agent.
Following 24 hours of culture, cells were exposed to the specific cell cycle blockers mimosine (blocks at G1/S phase boundary) or demecolcine (blocks in M phase). Control cells were exposed to culture media alone.
Cells were incubated for a further 24 hours and then analysed for nuclear GFP expression using a confocal scanning imager with automated image analysis (IN Cell Analysis System, Amersham Biosciences).
As shown in FIG. 5 , cells exposed to demecolcine showed increased fluorescence compared to control cells while cells exposed to mimosine showed decreased fluorescence compared to control cells. These results are consistent with the proposed use of the cell cycle phase reporter of the invention. Cells blocked in G1/S phase (mimosine treated), prior to the time of activation of the cyclin B1 promoter, show reduced fluorescence, while cells blocked in M phase (demecolcine treated), prior to the time of action of the cyclin B1 D-box, show increased fluorescence.
These results indicate that cell cycle phase reporters of the current invention are suitable for detecting agents which modulate cell cycle progression in a transient system and furthermore such reporters permit identification of the phase of the cell cycle in which cells are blocked.
3. Microinjection and Time-Lapse Photography of the Construct
HeLa cells were micro-injected with the construct prepared according to Example 1 and examined by time lapse microscopy, as shown in FIG. 6 . Differential interference contrast (DIC) images are shown on the left with the corresponding fluorescence image on the right. Frame A shows a cell (arrowed) in metaphase which shows bright fluorescence in the nucleus. Frames B and C show the same cell at later times in anaphase (B) and late anaphase (C). The DIC images of B and C show the division of the cell into two daughter cells (indicated by 2 arrows), the corresponding fluorescence images show the loss of fluorescence accompanying destruction of the fluorescent construct as the cell cycle progresses.
4. Stable Cell Line Production and Time Lapse Photography
U2-OS cells (ATCC HTB-96) were transfected with the construct described in example 1 and grown for several months in culture media containing 1 mg/ml geneticin to select for cells stably expressing the construct. A number of clones were picked by standard methods (e.g. described in Freshney, Chapter 11 in Culture of Animal Cells, (1994) Wiley-Liss Inc) and a clone containing fluorescent cells was isolated. This cell line was maintained at 37° C. in culture media containing 25 mM HEPES and a fluorescence and transmitted image of the cells taken every 15 minutes over a period of 24 hours using a standard xenon lamp at 488 nm. FIG. 7 shows 5 frames from a portion of the image that indicates that the cell line is behaving as expected. Cells in G2 exhibit green fluorescence in the cytoplasm, cells in early mitosis have fluorescence predominantly in the nucleus and following mitosis the reporter gene is degraded and the cells lose their fluorescence.
FIG. 8 shows the fate of a cell from the same clone that was monitored over 48 hours and that underwent two cell divisions to produce four granddaughter cells. For each time point the average intensity of each of the cells' progeny is measured and plotted against time. As can be seen the original cell enters mitosis at ˜4 hours, one of the daughters divides at 32 hours and the other at 42 hours into the experiment. As cells leave S-phase and enter G2 there is a steady increase in average intensity until the cell enters mitosis when the cell rounds up and the average intensity increases dramatically.
5. Preparation of a Brighter Stable Cell Line and Subsequent FACS Analysis
The green fluorescent protein reporter sequence in the vector described in example 1 was replaced with enhanced GFP (EGFP; Cormack, B. P. et al, Gene, (1996), 173, 33–38; BD Clontech) by standard methods. The EGFP gene is a brighter form of GFP containing the mutations F64L and S65T. In addition, EGFP contains codons that have been altered to optimise expression in mammalian cells. This new construct was transfected into U2-OS cells and a number of colonies were isolated by selection with geneticin followed by sorting of single cells using a fluorescence activated cell sorter. These clones showed brighter fluorescence than those generated in example 4 and as expected fluorescence intensity and location appeared to vary according to the cell cycle phase of the cell.
The cells were prepared for FACS analysis by standard methods. Briefly the cells were fixed and permeabilised using CytoFix/CytoPerm (Becton Dickinson) according to the manufacturers procedures. The cells were then treated with 50 μg/ml RNAse and 0.4% Triton X-100 and counterstained with 100 μg/ml propidium iodide. The degree of propidium iodide staining is proportional to the amount of DNA in the cell and therefore a measure of the cell cycle phase of the cell. As expected, the degree of red propidium iodide staining and the amount of green GFP fluorescence appear to be proportional in the cells.
6. The Effect of Cell Cycle Inhibiting Drugs on GFP Expression Levels
The cells prepared in Example 5 were grown in 25 cm 2 flasks and treated with either 100 ng/ml demecolcine (Sigma) or 1 mM mimosine (Sigma) for 24 hours. The cells were then fixed, permeabilised and stained with propidium iodide as described in example 5. FACS analysis revealed that, as expected, cells treated with the colchicine analogue arrested in G2/M and cells treated with mimosine arrested at the G1/S boundary. As is also expected the cells that had been arrested in G2/M were brighter than the cells that had been arrested at G1/S ( FIG. 9 ). | The invention provides a novel, non-destructive and dynamic process for determining the cell cycle position of living cells. The invention also provides DNA constructs, and cell lines containing such constructs, that exhibit activation and deactivation of a detectable reporter molecule in a cell cycle specific manner. The invention thus allows greater precision in determining cell cycle phase status than existing techniques and further provides a method for continuous monitoring of cell cycle progression in individual cells. | 2 |
[0001] The invention relates to suspended ceiling grid and, more particularly, to a clip for attaching grid tee ends to wall molding.
PRIOR ART
[0002] Suspended ceiling grid is normally made up of inverted tee shaped runners or tees that are arranged in a rectangular open grid pattern. Commonly, the ends of the tees, where they intersect with a wall, are simply laid onto the horizontal leg of a wall angle or wall molding. The vertical leg of the wall molding extends upwardly from the horizontal leg and is concealed by the horizontal leg and installed ceiling tiles. The vertical leg is nailed or screwed to the wall to support the wall molding and, in turn, the ends of the tees. Since the area of the vertical leg of the wall molding is concealed from view when the ceiling is completed, the fasteners used to secure it to the wall are unseen.
[0003] U.S. Pat. Nos. 4,715,161, 4,610,562 and 5,046,294 disclose types of clips that are used to attach ends of typical grid tees to wall moldings. U.S. Pat. Nos. 5,195,289 and 5,201,787 show a clip used to secure island trim to grid tees.
SUMMARY OF THE INVENTION
[0004] The invention provides a clip useful with suspended ceiling grid for attaching the ends of grid tees to wall angles or molding at selected or specified locations. The clip is arranged to be joined onto the end of the face or flange of a grid tee. The clip includes a formation, concealed in use, that interengages with the hem of a wall angle and to thereby lock the clip into position on the wall angle. In certain disclosed versions, the entire clip is concealed from view so as to yield an uninterrupted smooth finish on the visible portion of the wall angle and associated end of the tee.
[0005] In a reversal of roles, the clip can be used to mount the wall molding or its equivalent to the ends of the tees where the ceiling is constructed as an “island”. The clip can, additionally, be configured to telescopically support a tee end during seismic disturbances. Still further, the clip can be arranged to receive a grid tee that, by design, intersects the wall molding at an angle other than a right angle. This variable angle clip can be arranged, as mentioned before, to mount a wall molding or its equivalent in an island-like configuration even where the molding is free form or otherwise non-rectangular at the perimeter of the ceiling.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 is a fragmentary perspective view, looking from above, of a suspended ceiling grid employing the invention;
[0007] FIG. 2 is a fragmentary perspective view on an enlarged scale, of a first form of a clip for attaching the ends of grid tees to a wall molding;
[0008] FIG. 3 is a front elevational view of the clip of FIG. 2 ;
[0009] FIG. 4 is a side view of the clip of FIG. 2 ;
[0010] FIG. 5 is a perspective view of a modified form of the clip;
[0011] FIG. 6 is a perspective view of another modified form of the clip;
[0012] FIG. 7 is a perspective view of still another form of the clip specially suited for service in locales where seismic activity concerns exist;
[0013] FIG. 8 is a side elevational view of the clip of FIG. 7 ;
[0014] FIG. 9 is a plan view of the clip of FIG. 7 ;
[0015] FIG. 10 is a front elevational end view of the clip of FIG. 7 ;
[0016] FIG. 11 is a side view of a clip modified in form from that shown in FIGS. 7-10 ;
[0017] FIG. 12 is a fragmentary perspective view of a clip of modified form for use in instances where a tee intersects a wall molding at an angle other than 90°;
[0018] FIG. 13 is a plan view of the clip of FIG. 12 ;
[0019] FIG. 14 is a front end view of the clip of FIG. 12 ; and
[0020] FIG. 15 is a side elevational view of the clip of FIG. 12 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0021] Referring now to FIG. 1 , there is shown a portion of a suspended ceiling grid 10 including intersecting tees 11 and a wall angle or wall molding 12 . The tees 11 can be relatively long main tees and relatively short cross tees as is customary. The illustrated tees are of a customary cross-section ( FIG. 2 ) having a lower flange 13 , the underside of which forms the face of the tee visible from below in a room, a vertical stem or web 14 and an upper hollow reinforcing bulb 15 . The wall angle 12 illustrated in the figures has horizontal and vertical legs 17 and 25 of equal length (i.e. lateral width) and are each formed with a hem 16 . Customarily, the wall molding 12 is an elongated roll-formed sheet metal structure having a nominal standardized width.
[0022] As discussed hereinbelow, the ends of the tees 11 that overlie the horizontal leg 17 of the wall molding 12 are attached to the wall molding by individual clips 18 , as suggested in FIG. 2 . The clip 18 , preferably formed of sheet metal, has a generally horizontal leg 19 and an integral generally vertical leg 20 . At its end or edge remote from the vertical leg 20 , the horizontal leg 19 includes an integral tongue 21 . The tongue 21 extends substantially across the width of the clip, projects lengthwise a short distance from the horizontal leg, and is bent downwardly so that it forms an obtuse angle with the plane of the horizontal leg. The edges of the horizontal leg 19 are folded in the manner of a hem to form opposed channels 22 . The hems, designated 23 , are open sufficiently and their bight areas, designated 24 , are spaced apart sufficiently from one another to receive the flange 13 of the end of an associated tee 11 with sufficient room to enable the tee flange 13 to be received within the hem formed channels 22 without the application of excessive force. The hems 23 are short enough to permit free passage therebetween of the web 14 . For example, where the face of the flange is typically 15/16″ in width, the distance between the bights 24 can provide a lateral clearance of roughly 1/32″. The vertical distance between the hems 23 and main portion or body proper of the horizontal leg 19 can allow for minimal friction or a slight clearance with the thickness of the tee flange. The main portion of the horizontal leg 19 has a pair of laterally spaced holes 27 and the vertical leg 20 has a similar set of laterally spaced holes 28 .
[0023] Ideally, the clip 18 is proportioned so that it snaps in the space included between the two wall molding hems 16 . It can be difficult to precisely form the wall angle 12 so that the hems 16 are precisely open or precisely closed and/or to precisely position the free edges, designated 31 , of the hems 16 . The configuration and proportions of the clip 18 are intended to snap fit into the hem area of the wall molding 12 despite these variations. The tongue 21 , by virtue of its downward inclination is potentially capable of at least partially wedging under the hem 16 of the horizontal wall molding leg 17 . With reference to FIG. 4 , it will be seen that the generally vertical leg 20 is originally formed with a slightly obtuse angle α of say between about 91° and 101° to the plane of the main body portion of the horizontal leg 19 . The clip 18 is enabled to snap into the space occluded by the hem edges 31 by proportioning the clip 18 so that the distance between the free edge of its tongue 21 and a remote edge 36 of its vertical leg 20 , when the clip is in the free state illustrated in FIG. 4 is greater than the distance between the free edges 31 of the wall molding hem 16 . In this situation, when the clip 18 is pressed into the space bounded by the wall molding hem free edges 31 , the tongue 21 will lock against the free edge 31 of the horizontal wall molding leg 17 or will slip under its hem 16 . Similarly, the edge 36 will tightly abut the free edge 31 of the hem 16 on the vertical leg 25 or will snap under this hem 16 . Once the clip 18 is snapped in position so that it bears against the wall molding hem edges 31 or slips under one or both of them, the clip will be frictionally retained in its location. A moderate force can be applied to the clip manually to adjust it along the length of the wall angle 12 .
[0024] Ordinarily, the clip 18 can be slipped onto the end of a tee 11 before the clip is installed at a desired location on the wall molding 12 . The clip 18 is installed on the tee by simply slipping or telescoping the clip hems 23 and bights 24 over the lateral extremities of the tee flange 13 enabling these elements to grip the tee and prevent any significant relative movement between the clip and tee apart from telescoping motion along the longitudinal axis of the tee. Where desired, the tee 11 and clip 18 can be completely fixed relative to one another by assembling shallow head rivets or the like through the holes 27 in the main portion 26 of the horizontal clip leg 19 and through corresponding holes in the tee flange 13 , the location and making of which is ordinarily accomplished in the field by the installer. Shallow head fasteners assembled from the visible or face side of the flange 13 through the holes 27 allow these fasteners to exist between the horizontal clip leg 19 and horizontal wall molding leg 17 so that they are concealed from view of an observer looking upwards at a finished ceiling. The clip 18 can be fixed relative to the wall angle or molding 12 by screws, nails, or the like, through one or both of the vertical leg holes 28 and the vertical leg 25 of the wall angle. Fasteners in the clip vertical leg holes 28 , of course, cannot be seen from below the finished ceiling.
[0025] Various modified forms of the clip 18 are illustrated in FIGS. 5 through 15 . Elements serving the same or essentially same function as that described above in connection with the clip 18 are designated by the same previously used numerals. Elements having different or supplemental functions are ascribed with a third digit number designation.
[0026] FIG. 5 illustrated a clip 118 that is devoid of the vertical leg 20 of the previously described clip 18 . Here, in one approach the length of the clip 118 is such that the distance from the tongue free edge designated 34 to an opposite edge 119 is greater than the distance of a free edge 31 of a wall molding hem 16 (of a horizontal leg 17 ) to the vertical wall molding leg 25 . This extra length between these edges 34 and 119 assures that the tongue 21 will, at least, interfere with the wall molding horizontal leg hem edge 31 or will be caused to slide under it. In either case of interference or fitting below the hem 16 , the tongue 21 will lock the clip 118 in a selected position along the length of a wall molding 12 . The clip 118 is most easily installed by abutting the tongue edge 34 with the wall molding horizontal leg hem edge 31 and then forcing the clip from any inclination downwardly until the edge 119 is adjacent the corner between the horizontal and vertical wall molding legs 17 , 25 . Once the clip 118 is pressed so that its edge 119 is at or adjacent the corner between the wall molding legs 17 , 25 , the clip is frictionally locked in position. In an alternative approach, the distance between the free edge 31 of the tongue 21 and the opposite edge 119 can be the same or less than the distance between the inside edge 31 of the hem 16 of the horizontal wall molding leg 17 and the vertical leg 25 . The clip 118 is attached to a grid tee end with shallow head fasteners through holes 27 and aligned holes in the grid tee flange 13 . Where the holes 27 are not used or are omitted, the clip 118 (as well as other clips disclosed herein) can be locked to the grid tee flange 13 by crimping the hems 23 onto the flange.
[0027] Referring to FIG. 6 , a clip 218 differs from the 18 in that it is devoid of the vertical leg 20 , hems 23 , and bights 24 . The clip 218 has an edge 219 corresponding to the edge 119 of the clip 118 of FIG. 5 . The clip 218 is frictionally locked in position when the tongue edge 34 tightly abuts or slips under the wall molding horizontal leg hem free edge 31 and the edge 219 abuts or is adjacent the corner between the horizontal and vertical legs 17 , 25 of the wall molding 12 . Spaced holes 27 enable the clip 218 to be locked to the end of an associated tee 11 when screws, rivets or the like, are located in the holes and holes formed in the tee end.
[0028] FIGS. 7-10 illustrate a clip 250 suitable to be used, for instance, where seismic activity may be expected. The clip 250 has an elongated, e.g. 3″ long, horizontal leg 251 . The leg 251 includes a generally planar main body 252 with integral opposed hems 253 and bights 254 along its elongated edges. The hems 253 are open to enable the flange 13 of an end of a tee 11 to freely telescope therein along the longitudinal direction of the tee in the manner of a “trombone”. Like the hems 23 and bights 24 of the clip 18 , the hems 253 and bights 254 are proportioned to allow passage of the tee web 14 therebetween and limit relative motion between the clip 250 and tee 11 to longitudinal motion.
[0029] The clip 250 has the geometry of the tongue 21 and relative geometry between the plane of the horizontal leg 19 and vertical leg edge 36 as described in connection with the clip 18 of FIGS. 2 through 4 . Depending on where the end of the tee 11 is positioned, i.e. that dictated by the selected length of the tee, there can be about 1½″ in free telescoping movement in each longitudinal direction of a tee in the event of seismic movement.
[0030] FIG. 11 illustrates a side view of a clip 260 similar to the clip 250 of FIGS. 7-10 . The clip 260 differs from the clip 250 in that the tongue 21 is spaced farther from the vertical leg 20 of the subject clip. The clip 260 is provided to work with a seismic wall molding. The distance between the tongue edge 34 and remote edge 36 of the vertical leg 20 is increased to match the corresponding pseudo hypotenuse dimension between the free edges of the hems of the seismic molding.
[0031] FIGS. 12 through 15 illustrate another form of a clip 270 for attaching the ends of grid tees to wall angles or similar elements. The clip 270 is an assembly including a base 271 and an arm 272 pivotally joined to the base by a pin or rivet 273 which may be a separate element or integrally formed from one or both the base and arm. The rivet 273 enables the arm 272 to pivot about its axis in a horizontal plane when the clip 270 is in the orientation shown in FIG. 12 . The arm 272 from the rivet or pin 273 has a cross-section like that previously described in connection with the clip 18 of FIGS. 2 through 4 and the other modified clips, the arm including open hems 274 and bights 275 . The clip 270 allows a tee 11 to be attached to a wall molding 12 while intersecting it in the horizontal plane of a leg 276 at an angle other than 90°. It will be seen that the arm 272 can be pivoted about the center of the rivet 273 to permit the arm 272 to receive a tee 11 intersecting the wall molding at an angle from nearly 0° to nearly 180°.
[0032] While the clip of FIGS. 12 through 15 is proportioned to work with a wall molding with a horizontal leg of conventional width, this clip can be modified to lengthen the horizontal portion of the base 271 so as to move the tongue 21 further from the vertical leg 20 so as to mate with a relatively wide or seismic wall molding.
[0033] Various ones of the disclosed clips can be conveniently used to support a wall molding or a similar structure when the roles of the tees and wall molding are reversed such as in an island ceiling treatment where the perimeter of the ceiling does not abut a wall. The clip 270 permits a wall angle or a similar structure to be supported on tees which intersect at one or more angles other than 90°.
[0034] While the invention has been shown and described with respect to particular embodiments thereof, this is for the purpose of illustration rather than limitation, and other variations and modifications of the specific embodiments herein shown and described will be apparent to those skilled in the art all within the intended spirit and scope of the invention. Accordingly, the patent is not to be limited in scope and effect to the specific embodiments herein shown and described nor in any other way that is inconsistent with the extent to which the progress in the art has been advanced by the invention. | A clip for attaching the end of a grid tee to a wall angle. The clip, in various forms, is arranged to frictionally lock between the hem of the horizontal leg of the wall angle and the vertical leg. The clip, typically, has a pair of opposed open hems forming channels in which the flange of the tee end is received to join the tee to the clip. The clip can be elongated horizontally to accommodate movement of the grid during seismic activity. The clip can be used to trim the edges of a ceiling island and can be made to accommodate angular intersections of the grid with a wall or island edge. | 4 |
FIELD OF THE INVENTION
The present invention relates to a method of inducing targeted oriented fractures connecting two wells drilled in subterranean porous formations whether or not the connection of the two wells is oriented perpendicular to the in-situ minimum stress.
BACKGROUND
In many Earth engineering applications, wells are drilled into subterranean porous formations. It is desirable to create a fracture connecting two neighboring wells. In general, the fracture follows the plane perpendicular to the least resistance, i.e., perpendicular to the original in-situ minimum stress, Smin. Thus, normally, the two wells need to be drilled so that the line connecting them is aligned perpendicular to Smin. Otherwise, if the two wells are drilled substantially deviated from the preferred direction, a fracture may not be formed to connect the two wells. In Canada and many parts of the world, petrochemicals are found in heavy, viscous forms such as bitumen, which are difficult to extract. The bitumen-saturated oilsands reservoirs of Canada, Venezuela and California are just some examples of such subterranean formations. In these formations, it is not possible to simply drill wells and pump out the oil. Instead, the reservoirs are heated or otherwise stimulated to reduce viscosity and promote extraction.
The two most common and commercially-proven methods of stimulating oilsands reservoirs are (a) cyclic steam stimulation (CSS) and (b) steam assisted gravity drainage (SAGD). In both cases, steam is injected into the reservoir, to heat up the bitumen. Some variations of these processes may involve injecting solvent to aid the viscosity reduction or use electrical heating to replace the role of steam. In general, the initial injectivity into the reservoir, i.e., how much volume of the stimulant can be injected per unit of time, is relatively small. Fracturing of the reservoir is desired to provide channels for the stimulant travel and to access the reservoir. The fracture not only increases the injectivity, but also increases the contact area of the stimulant within the reservoir. For example, in CSS, the injection pressure goes above the reservoir's fracture pressure with the goal to form the fracture. It is desirable to be able to control the orientation, depth and length of fractures in the reservoir, in order to more effectively place stimulant in the targeted location, extent and/or time, all of which can help maximize petroleum extraction.
In the SAGD process, before the production can start, communication between the SAGD well pair must be established so that the bitumen can flow down to the production well. Conventionally, steam is circulated through the said two wells independently until the inter-well area is heated and the bitumen viscosity is reduced significantly so that it can flow to the production well and communication is established. This process normally takes up to 6 months to complete. Such a non-productive period wastes steam and manpower, ties up the capital used to build the infrastructure. If the SAGD wells can be hydraulically fractured, forming a high-mobility conduit connecting the two SAGD wells, the inter-well communication can occur much earlier and stronger.
The art of hydraulic fracturing as a stimulation method for hydrocarbon resource recovery has been practiced for a long time. In general, this method injects liquid at a high pressure into a well drilled through the target formation to be stimulated. The high pressure initiates a fracture from the injection well and propagates a sufficient distance into the formation. Then, the fracture is filled with proppants that are injected from the surface after the fracture is formed. The similar method is applied in vertical and horizontal wells and wells of any inclinations. However, the existing art of hydraulic fracturing is subject to limitations.
In hydraulic fracturing, there has historically been no proactive control of the orientation of the fracture formed. The fracture typically follows the plane perpendicular to the least resistance, i.e., perpendicular to the original in-situ minimum stress, S min . In many situations, SAGD wells may not be drilled in this optimal direction. For example, the azimuth of the SAGD wells being drilled might be dictated by the deposit channel of the oilsands resource. The well pair then tends to follow the channel direction which may or may not coincide with the S min direction. If a horizontal well is drilled in the direction of the minimum stress S min or substantially inclined towards it, the fracture being formed via the conventional hydraulic fracturing may be discrete in the vertical cross-section perpendicular or substantially perpendicular to the horizontal well. Such fractures may not be ideal for the petroleum production. For example, discrete fractures perpendicular to the SAGD wells do not contribute to uniform communication between the well pair.
There has been some work done in controlling the orientation of fractures including selective placement of hydraulically-driven fractures in the plane perpendicular to the original in-situ maximum stress, Smax. These practices in the past, however, typically require a sacrificial well which was fractured first along the direction perpendicular to Smin, i.e., the original in-situ stress condition dictates the fracture formed on this sacrificial well. For example, U.S. Pat. No. 3,613,785 by Closmann (1971) teaches creating a horizontal fracture from a first well by vertically fracturing the formation from a second well and then injecting hot fluid to heat the formation. Heating via the vertical fracture alters the original in-situ stress so that the vertical stresses become smaller than horizontal stresses, thus favouring a horizontal fracture being formed. This method requires a first sacrificial vertical fracture be formed and uses costly steam to heat the formation.
U.S. Pat. No. 3,709,295 by Braunlich and Bishop (1971) controlled the direction of hydraulic fractures by employing at least three wells and a natural fracture system. This method is only feasible in formations already having existing fractures.
U.S. Pat. No. 4,005,750 by Shuck (1975) teaches creating an oriented fracture in the direction of the minimum in-situ stress from a first well by first hydraulically fracturing another well to condition the formation. Again, additional wells and sacrificial fractures are required before the targeted fracture can be formed.
Canadian patent CA 1,323,561 by Kry (1985) teaches creating a horizontal fracture from a center well after cyclically steam-stimulating at least one peripheral well. At the peripheral well a vertical fracture is created. CSS operations coupled with fracturing at the peripheral well conditions the stress field so that a horizontal fracture can be formed. To create the horizontal fracture, a high-viscosity fluid is proposed to inject into the center well to limit the fluid from leaking into the formation.
Canadian patent CA 1,235,652 by Harding et al. (1988) first vertically-fractures the formation from peripheral wells to alter or condition the in-situ stress regime in the center region of the peripheral wells. The formation is then fractured through a central well to create and extend a horizontal fracture.
All of the above documents require either the existence of a natural fracture in the formation already or the formation of sacrificial fractures before a targeted fracture can be induced. This pre-condition adds cost to well drilling and completion.
The idea of forming a target fracture without initiating sacrificial fractures has been proposed in two presentation papers by Lessi, J., et al. . (“Underground Coal Gasification at Great Depth”; Technical Committee of Groupe d'Etude de la Gazefication Souterraine du Charbon and “Stress Changes Induced by Fluid Injection in a Porous Layer Around a Wellbore”; 24 th US Symposium on Rock Mechanics June 1983). These papers propose drilling two wells and forming a fracture connecting them even though their connection line may be not oriented perpendicular to Smin. According to the authors, this process relies on pressure diffusion and thus-associated poroelastic stress to create a fracture between the two wells. The two papers did not address interaction between the wells.
It is therefore of great interest to find a new method to over-come the original in-situ stress condition for selective placement of a fracture without drilling a sacrificial well or dictating presence of natural fractures.
SUMMARY OF THE INVENTION
A method is taught of creating one or more targeted fractures in a subterranean formation. The method comprises the steps of drilling and completing two wells in the formation, conditioning said wells to create a stress condition favorable for forming a fracture zone -connecting said two wells and initiating and propagating the fracture zone in said formation.
DESCRIPTION OF THE DRAWINGS
The invention will now be described in further detail with reference to the following drawings, in which:
FIG. 1 a illustrates a subterranean formation drilled with two wells of any inclinations in any azimuth with respect to the in-situ stress field;
FIGS. 1 bi to 1 biv each illustrate alternate orientations for pairs of wells that can be drilled and completed for the purposes of the present invention;
FIG. 1 c illustrates a well that that has been drilled and completed according one embodiment of the present invention;
FIG. 1 d illustrates a further well that has been drilled and completed according another embodiment of the present invention
FIG. 1 e illustrates a further well that has been drilled and completed according a further embodiment of the present invention;
FIG. 2 a illustrates a pair of wells as they are conditioned using a method of the present invention;
FIG. 2 b illustrates a pair of wells as they are conditioned using a method of the present invention;
FIG. 3 a illustrates a fracture zone in a subterranean formation as a result of a typical method of fracturing;
FIG. 3 b illustrates a fracture zone in a subterranean formation as a result of the method of the present invention; and
FIG. 4 is a schematic diagram of one embodiment of a method of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention provides a method of controlling the orientation of fractures in subterranean porous formations.
More specifically, the present invention provides a method of forming a fracture connecting two wells in subterranean geological formations even though the connection of the said wells is not oriented perpendicular to the original in-situ minimum stress. The said fracture(s) will facilitate the communication between the said wells. One direct application is to facilitate early and uniform start-up of the SAGD process in the in-situ recovery of heavy oil/oilsands reservoirs.
The orientation of the fracture(s) in subterranean formations is typically dependant on the in situ stresses at a particular location in the formation. Generally, fractures form in a direction perpendicular to the direction of the least stress.
However, the present inventors have found that the original in situ stress profile can be modified via interaction of said two wells in the pressure and/or temperature diffusion, and thereby change the orientation of induced fractures to the direction connecting the said two wells. The present method does not require one or more sacrificial fractures being formed a prior to preconditioning. Furthermore, it does not depend whether or not the original in-situ stress field favors the formation of the target fracture.
The process is well suited to oilsands reservoirs such as those in Alberta and Saskatchewan, Canada. However, the process can be applied to any formations and situations where the target fractures are sought. The steps of the present method are generally illustrated in FIG. 4 .
Two wells are first drilled and completed. The well drilling and completion follows the conventional petroleum engineering practices or difference can be sought, all of which depends on the specific applications. FIG. 1 a illustrates an example of well drilling applicable to the present invention although other methods and configurations of well drilling and completion would also be suitable for the present invention and would be obvious to a person of skill in the art. Some examples of further well orientations encompassed by the present invention are illustrated in FIGS. 1 bi to 1 biv.
An interval or zone 6 along each well is exposed along which injected fluid and thus pressure can enter into the target subterranean formation 2 . The two wells 4 are preferably in proximal to one another and have respective contacts with the formation 2 to be fractured.
For the purposes of the present invention, well-formation contact describes an interval 6 where the fluid can be injected into the formation 2 from the well. For open holes, any section of the wells 4 that is segmented for accepting the injected fluid is the contact.
The wells 4 may also be cased and cemented into place. The cement 8 is preferably perforated to penetrate the steel casing and the cement 8 to provide an interval 6 for the injected fluid to enter into the formation 2 . The perforated interval 6 can be of any length and the fracture can be initiated anywhere along the contact length. This is illustrated in FIG. 1 c . Alternatively, as illustrated in FIGS. 1 d and 1 e , a portion of the well can be cased and cemented 8 while another portion of well remains uncased, thus serving as the interval 6 through which injection fluid can enter the formation 2 .
The two wells 4 can be combined in different ways. Preferably, as illustrated in FIGS. 1 bi to 1 biv , two injection intervals 6 are formed from each of said two wells 4 . This allows exposed intervals 6 be close to each other so that pressure and/or temperature front can readily interact with each other.
Optimization of specific inter-well distance and/or orientation of their connection with respect to in-situ minimum stress component (S min ) depend on the in-situ condition, formation properties, operating condition, and production objectives among others. Simulations can be run to determine these well drilling and completion parameters for particular applications. For example, SAGD technology used in the in-situ oilsands development has the two horizontal wells 4 that are typically 5 m apart and 400 to 1000 m long which is open to the formation 2 .
In a second step, the area where said two wells 4 to be connected via a fracture is conditioned via controlled injection into one or the two of said two wells 4 . The increased pressure and/or temperature field alters the original in-situ stress condition via poroelastic and/or thermoelastic mechanisms. The new stress condition after the modification favors a fracture being formed to connect the exposed injection intervals 6 between said two wells 4 . These steps are illustrated in FIGS. 2 a and 2 b . FIG. 2 a illustrates the rather limited interaction between the two wells 4 at an early stage of conditioning and FIG. 2 b illustrates the more developed interaction between the two wells 4 near the end of conditioning.
The stress modification step involves pressure diffusion fronts from each of the said two wells 4 interacting with one another. The faster the pressure and/or temperature diffusion, the earlier the stress condition is modified. The larger the pressure and/or temperature change, the more significantly the stress condition is modified. The pressure diffusion depends on the effective fluid mobility in the formation 2 . Anything that can increase the mobility will help. Therefore, one or more of the following means can help the stress modification, although other means of stress modification are also possible and would be clearly understood by a person of skill in the art as being encompassed by the scope of the present invention:
(1) Dilation to increase the absolute permeability of the formation 2 . (2) Dilation with injected water to increase the relative permeability to water. (3) Injection of warm water to reduce the fluid viscosity in the formation 2 . Preferably, warm-up of the wells 4 via steam circulation prior to warm water injection can help to maintain the temperature of the injected warm water. (4) Injection of chemical solvents or solutions to reduce the fluid viscosity in the formation 2 . (5) Injection or circulation of steam.
The pressure diffusion increases the pore pressure inside the formation 2 , evoking the poroelastic stress buildup. Similarly, temperature diffusion increases the temperature inside the formation 2 , evoking the thermostatic stress buildup. Both poroelastic and thermoelastic stresses are similar in their benefits for the dilation promotion purpose. However, in general, the temperature diffusion is slower than the pore pressure diffusion. Thus, injection at a higher pressure is more efficient than injection at a high temperature. Simultaneous high pressure and high temperature injection is most preferred for the purposes of the present invention. For the purposes of the present invention, the phrase “high-pressure injection” is used and it should be understood that this phrase includes or applies to high-temperature injection as well.
The injection pressure should start below the original in-situ minimum stress (S min0 ). Preferably, known methods can be used, such as performing a mini-frac test to measure the original in-situ minimum stress. As the pore pressure increases in the formation 2 , the in-situ stresses increase due to the poroelastic mechanism. Thus, after the injection has undertaken for a certain period of time, it is possible to increase the injection pressure to somewhat above S min0 . Such an increased injection pressure will increase the magnitude of the stress modification. The increase is preferably gradual and monitored to prevent formation of a macroscopic tensile fracture before the formation 2 is fully conditioned. As illustrated in FIG. 3 a , if a fracture is initiated prior to full development of an interaction between two neighboring wells 4 , the fractures are not successful in connecting the two wells 4 .
Between the two wells 4 , many alterations can be pursued in the injection pressure, injection rates, injected materials and so on. Most preferably, injections are conducted in both wells 4 simultaneously to aid in accelerating interaction of the pressure diffusion between the wells 4 .
In other circumstances, injection into a single well may be preferred. For example, if a bottom layer of water is present in the reservoir, it may beneficial to reduce or eliminate injection into a lower of said wells 4 to avoid communication with the bottom water, although full elimination of injecting into the lower well is not necessarily required even in the presence of the bottom water layer.
In one preferred embodiment, a lower well injected or circulated with steam, to aid in viscosity reduction in an upwards direction, due to the tendency of steam to rise. A upper well can then be injected with a solvent or chemical solution, to promote viscosity reduction in a downwards direction, via gravity-driven fluid movement downwards.
In another embodiment, the injection can start with water such as water produced from water treatment plants typically in the vicinity of the wellbore operations. As dilation of the formation 2 induces more pore space, the injection material can be switched to steam or solvent that will have a good injectivity due to the pre-dilation by water. Advantageously in this arrangement, pore space is increased using more abundantly available water and more expensive steam or solvent is used to promote dilation and diffusion.
Furthermore, the temporal alterations described above can vary between said two wells 4 . In all cases, the materials, pressures, temperatures and rates of injection and injection coordination between the two wells 4 depend on specific geological situations, convenience and economics. Geomechanical simulations based on the specific circumstances can decide the optimum strategy.
Some examples of conditioning means include substantially simultaneous injection of stimulant into both wells 4 or substantially alternating injection of stimulant into one and then another of the well pair. Stimulant injection during the conditioning phase are preferably monitored and controlled to either maintain a constant injection rate and/or pressure or to vary the injection rate and/or pressure. Injection pressure can, in one embodiment of the present invention, be incrementally increased, or alternatively be raised and lowered to achieve formation 2 conditioning. Furthermore, the injection rate or injection pressure during conditioning can vary between the two wells 4 .
Stimulant injection rates should be lower than that required to fracture the formation 2 , but sufficiently high to create a desired rate of pressure increase. Preferably the injection rate is optimized to shorten operation time of the whole process.
Stimulant injection rate and time can be determined on-site based on the real-time monitored well injection pressure and rate. If the pressure increase is too slow, the rate can be increased. If the pressure rises too fast, the rate should be reduced. Site-based real-time pressure monitoring methods and devices are well known in the art and are included in the scope of the present invention. Preferably, stimulant injection rates are initially slower to probe and assess characteristics of the formation 2 , before a higher rate is used.
In some well completions, a well has two or more fluid injection or production points. For example, in SAGD operations, a long horizontal well interval is completed with two or more concentric tubulars. One leads to the front end, or toe, of the horizontal well and the others are placed to the intermittent points behind the toe one of which may be placed at the heel of the horizontal well. In these situations, the injection can proceed with injecting into one end such as toe while producing from the other end such as heel. The produced rate is smaller than the injected so that a net injection occurs into the formation. One advantage of such an injection scheme is to promote uniform distribution of pressure or temperature along the well length. Another advantage is an easy control on the injection rate or pressure.
The stimulant material to be injected can vary, so long as it serves to raise formation pressure and it does not harm the hydraulic conductivity of the formation 2 being fractured, any material can be injected. Ease to operate and economics dictates the material. For the purposes of the present invention, stimulant includes water of any temperatures, steam, solvent, solutions of suitable chemicals or their mixture in any portion.
Stimulant materials being injected into each of the two wells 4 can be different between them and/or alter over time. Furthermore, stimulant type and temperature to be injected during the stress modification phase can vary between the two wells 4 . For example, cold or warm water may be injected into a first well while the second well may be injected with steam. Alternatively a solvent, either warm or cold, may be injected in a first well, while the second well may be injected with steam. A skilled person in the art would understand that other combinations of stimulant type, temperature and pressure are also possible and encompassed by the scope of the present invention.
Some stimulant materials can increase the pressure diffusion and thus, should be encouraged. For example, in heavy oil or oilsands industry, solvent or certain chemical solutions can reduce the oil viscosity and thus increase the effective formation mobility. Warm water up to steam can reduce the viscosity and thus helps the stress modification.
Stimulants used for injection are not limited and can be anything from water produced from nearby water treatment facilities to high-temperature steam or anything between. The stimulant viscosity can also range from approximately 1 centipoise (cp), as in the case of water, to high-viscosity stimulants. Specific values of the viscosity can be designed by simulations when the in-situ condition and formation properties are known.
The stress modification stage serves to modify the in-situ stress field around the two wells 4 so that the target fracture can be formed along the connection of the said two horizontal wells 4 . The timing of the stress modification phase depends on the in-situ conditions, formation properties, stimulant material properties and injection conditions including rate, pressure and temperature of injection, and combinations of these conditions and properties. Preferably, geo-mechanical simulations can be run prior to conducting the methods of the present invention to estimate the conditioning timing and design the injection pressure or other condition. Further preferably, field pilot tests can be run in a particular location to fine-tune the timing. Moreover, end of the stress modification stage can be determined by pressure interference tests. Conventional interference test protocols in transient pressure analysis of petroleum engineering can be used. For example, one of the well pair is shut-in while the other well continues the injection. If the shut-in well sees pressure impact of certain degree from the injection well, the current dilation stage can end and the subsequent dilation promotion stage follows.
Following stress modification, the injection pressure is increased further at one or the two of said two wells 4 to break down the formation 2 and to propagate the fracture zone 12 which will connect the two wells 4 . This step is called fracture communication stage and is illustrated in FIG. 3 b.
In both FIGS. 3 a and 3 b it should be noted that compressive forces within the formation are represented as a positive increase in stress. While this may differ from typical solid mechanics notation, representing compression as a positive force is common in geomechanics, and is the correlation used for the purposes of the present invention.
For example, when the present method is applied to start up the SAGD process, injection of the stimulant serves to stimulate the area around the SAGD well pair so that a fracture zone 12 is formed between them.
In another example application, grout may need to be placed to seal a certain interval in the subsurface formation 2 . In this case, the fracture is first formed along the certain interval and then grout is injected into the fracture. In yet another example application, contaminants may need to be removed from subsurface. Leaching is normally used. The target fracture can be formed first to start the leaching process at the target locations. In a final example, THAI process has been tried as a potential in-situ oilsands recovery process. A target fracture can be formed between the injection well and producer well.
In geothermal applications, two wells are drilled with one well injecting cold water and the other producing the heated water. The present invention can be used to form a fracture between the wells.
The injection pressure is increased by increasing either the injection rate or injection pressure above the original in-situ minimum stress, S min , until a fracture zone is initiated. Initiation of the fracture zone can be observed by monitoring the injection pressure and/or rate. If fracturing injection is maintained at a constant rate, the increased injectivity is reflected by a decreasing pressure. If fracturing injection is maintained at a constant pressure, the increased injectivity is reflected by an increased demand of more volume per unit time to be injected in order to maintain the constant pressure. During initiation of the fracture, injection can be carried out at one or both of the two wells 4 .
Preferably, once the fracture has been initiated, one well is shut-in while the other well continues the injection. This enables detection of the inter-well communication. When pressure at the shut-in well increases, it means that the two wells 4 are in communication with each other.
The present method utilizes poroelastic and/or thermoelastic mechanisms to alter the original un-disturbed in-situ stress conditions so that the target fracture can be created. Poroelastic stress comes from the interaction between pore pressure and solid deformation. The general theory of poroelasticity was established by Biot (1941) although the particular case of poroelasticity relating to interaction between deformation and pressure diffusion was studied earlier by Terzaghi (1923) for soils. Poroelastic effects in rock mechanics related to petroleum engineering were first noted by Geertsma (1957, 1966). Thermoelastic stress comes from the interaction between temperature and solid deformation. Physically, an increase in the pore pressure (p) or temperature (T) causes rock to expand. Such expansion is constrained by the material outside the domain of p/T increase. The restriction introduces an additional stress component to the original undisturbed in-situ stress field in the formation 2 . Such induced stresses are called the poroelastic or thermoelastic stresses depending on if the causing mechanism is pore pressure increase or temperature increase.
Mathematically, the stress modification phase and subsequent fracture initiation and propagation stage can be simulated by a nonlinear coupled thermo-hydro-mechanical model.
This detailed description of the present processes and methods is used to illustrate certain embodiments of the present invention. It will be apparent to a person skilled in the art that various modifications can be made and various alternate embodiments can be utilized without departing from the scope of the present application, which is limited only by the appended claims. | A method is taught of creating one or more targeted fractures in a subterranean formation. The method comprises the steps of drilling and completing two wells in the formation, conditioning said wells to create a stress condition favorable for forming a fracture zone connecting said two wells and initiating and propagating the fracture zone in said formation. | 4 |
BACKGROUND OF THE INVENTION
[0001] During welding operations, it is often necessary to protect the root of the weld from oxidation as this can lead to weld defects and a reduction in corrosion resistance. This is particularly the case in creep resistant materials, alloy steels, stainless steels and its alloys, nickel and its alloys, and titanium and its alloys. The usual method of protecting the area to be welded is to purge it usually by passing a stream of an inert gas such as argon over the weld area. This limits the availability of oxygen at the weld root to cause oxidation.
[0002] However, there are a number of factors which may affect the efficiency of the process and the quality of the weld produced. These factors include the method of damming, the oxygen content of the purge gas and the purge flowrate, all of which can affect the service life of the welded component.
[0003] Purging is commonly required when gas tungsten arc welding (GTAW) or plasma processes are used, particularly when stainless steel and alloy steels, nimonics and reactive metals such as titanium or zirconium are being joined.
[0004] A common application area is for root runs in circumferential welds in pipe. For pipelines used in the production of electronic components, there is also a requirement to ensure the absence of particles, particularly oxides formed during welding operations.
[0005] For steel and nickel alloys, inadequate protection of the rear face of the weld will lead to heavy oxidation and poor penetration bead shape and low corrosion resistance as shown in FIG. 5 (Pitting corrosion potential graph). Further there will be discoloration in the reactive metals and embrittlement.
[0006] The problem to be solved is the extended length of time that is needed for oxygen concentration to be reduced from 200,000 ppm to about 10 ppm. The nature of the purging process follows a mathematical power curve of the form Y=AX −b . The nature of this curve is such that the tail of the curve is very long, leading to extended times for reducing the oxygen concentration from 200 ppm to 10 ppm. This time period is controlled by the diffusion mechanism and cannot appreciably be reduced significantly. This time period is dead time for fabricators and manufacturers as no production can continue until the 10 ppm level is reached.
[0007] The instant invention reduces this waiting time and utilizes the rapid expansion of liquid cryogenic gases from the liquid phase to the gas phase. The rapid expansion from the liquid to the gaseous state displaces air that is present inside a vessel or pipe to be purged, thereby replacing the air and oxygen present therein with the chosen inert cryogen gas.
SUMMARY OF THE INVENTION
[0008] In one embodiment of the invention, there is disclosed a method for purging air from a structure to be welded comprising feeding a liquid cryogen to said structure wherein said liquid cryogen will expand to a gaseous state and displace said air in said structure.
[0009] The structure that is to be welded is typically a pipe or vessel that is capable of entraining air. The liquid cryogen which is selected from the group consisting of argon, helium and nitrogen and mixtures thereof is added to the weld joint between the structure to be welded and the structure it is welded to. As the liquid cryogen warms up inside the structure, it will rapidly enter the gaseous phase and expand. This expansion will force air that is entrained in the structure to be welded out of the structure such as in the case of a pipe, the opposite end from the position that is being welded. This will reduce the oxygen content at the weld joint to about 10 ppm and will do so in a significantly shorter period of time than if traditional purging methods had been employed. The welding operation may commence at this point with the lower oxygen levels present.
[0010] The concentration of oxygen in the structure to be welded may be monitored by conventional means such as oxygen meters or oxygen concentration monitors. By measuring the level of reduction of oxygen in the structure to be welded, the welder/fabricator will know when to begin welding.
[0011] In another embodiment of the invention, there is disclosed a method for welding a structure comprising feeding a liquid cryogen to said structure and allowing said liquid cryogen to expand to the gaseous state thereby displacing air present in said structure.
[0012] The structure is typically a pipe or vessel that is capable of entraining air and having at least one open end to allow the escape of gas. The liquid cryogen which is selected from the group consisting of argon, helium and nitrogen and mixtures thereof is added to the weld joint between the structure to be welded and the structure it is welded to. Welding may begin when a lower level of oxygen present in the structure to be welded is measured.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a representation of a structure to be welded using liquid cryogen to displace air from the structure.
[0014] FIG. 2 is a graph showing oxygen amounts versus time for a traditional purging operation.
[0015] FIG. 3 . is a graph showing oxygen amounts versus time for the inventive purging operation.
[0016] FIG. 4 is a graph showing oxygen concentration versus time for a regular gas purge and the inventive method.
[0017] FIG. 5 is a graph showing the effects of oxygen levels versus pitting corrosion potential.
DETAILED DESCRIPTION OF THE INVENTION
[0018] In FIG. 1 , there is disclosed a structure to be welded according to the methods of the invention. This structure 10 can be a pipe or vessel that contains an empty space that is capable of entraining air. The structure 10 can be welded to an adjacent structure 40 which can be likewise in design (i.e., pipe to pipe fitting). The structure 10 to be welded can be any material that is capable of being welded, for example a material selected from the group consisting of creep resistant materials, alloy steels, stainless steel, nickel, titanium, zirconium and all their respective alloys.
[0019] The structure 10 to be joined with adjacent structure 40 can be joined by a variety of welding and joining means selected from the group consisting of GTAW (Gas Tungsten Arc Welding), PAW (Plasma Arc welding), GMAW (Gas Metal Arc Welding), Laser Welding and other suitable welding processes.
[0020] The weld joint 25 is the place where one end of structure 10 is joined with one end of structure 40 and is where the welding operation takes place. Liquid inlet 15 contacts the weld joint through a filling means 20 such as a funnel. The liquid inlet 15 will allow liquid cryogen selected from the group consisting of argon, helium, nitrogen and mixtures thereof to enter the structure 10 . The liquid cryogen will be fed to the structure 10 at typical ambient temperatures. As the liquid cryogen warms up inside the structure, it will convert to the gaseous phase and begin to expand. As the liquid cryogen expands to a gas, it will force the air that is already present in the structure 10 and the adjoining structure 40 out their ends 30 and 35 respectively. Typically this expansion of gas will result in oxygen content inside the structure 10 being reduced from around 200,000 ppm to about 10 ppm.
[0021] The amount of liquid cryogen employed depends upon the size and volume of the structure to be joined as well as the liquid cryogen itself. Typically this amount ranges from 0.25 of liquid litre to 5 litres depending on how large the pipe or vessel volume is and this amount is fed into the system for an amount of time necessary to allow the requisite amount of liquid cryogen to enter the structure.
[0022] Once the appropriate oxygen level has been reached, welding of the structure can commence. In order to maintain this level of oxygen, purging with a purge gas selected from the group consisting of Argon, Nitrogen, and Nitrogen and Hydrogen mixtures, should be performed at about 10 to 20 liters per minute of purge gas during the length of the welding operation.
[0023] FIG. 2 is a graph showing the concentration of oxygen versus time for a typical purging process. The structure to be purged was a 2205 Duplex Stainless Steel Vessel having a diameter of 460 mm and 1000 mm length. This normal gas purging utilized Argon as the purge gas and consisted of directing the purge gas through the pipe until the requisite oxygen concentration is reached. As noted earlier, the nature of the purging process follows a mathematical power curve of the form Y=AX −b . The nature of this curve is such that the tail of the curve is very long, leading to extended times for reducing the oxygen concentration from 200,000 ppm to about 10 ppm. As seen in FIG. 2 , the normal gas purging had a formula Y=2863.4X −1.3548 and took 65 minutes at a flow rate of 45 litres per minute to reach a 10 ppm oxygen level inside the vessel.
[0024] In FIG. 3 , the same vessel as in FIG. 2 was purged of gas using the inventive method and liquid argon. The power curve formula was Y=20.523X −1.148 and it can be seen that with the liquid argon being fed into the stainless steel vessel that it took 1 minute and 50 seconds to reach a 10 ppm oxygen level inside the vessel. This is a significant time savings versus the 65 minutes it took using the traditional purging method.
[0025] FIG. 4 is a graph showing the differences between the gas purging method as described in FIG. 2 and the inventive method using a liquid cryogen as described in FIG. 3 . The normal gas purging process took 65 minutes to reach 10 ppm oxygen level while the inventive process was able to reach this oxygen concentration in 1 minute and 50 seconds.
[0026] FIG. 5 is a graph showing the effect of purge gas oxygen levels on pitting corrosion potential in millivolts. As noted in FIG. 5 , the less oxygen present in a system, the higher the pitting corrosion potential is. Consequently, the higher pitting corrosion potential equates to higher corrosion resistance, therefore corrosion resistance is improved by purging oxygen from the vessel to be joined,
[0027] While this invention has been described with respect to particular embodiments thereof, it is apparent that numerous other forms and modifications of the invention will be obvious to those skilled in the art. The appended claims in this invention generally should be construed to cover all such obvious forms and modifications which are within the true spirit and scope of the invention. | A method for purging air from a structure to be joined by welding by feeding a liquid cryogen to the structure. The liquid cryogen will enter the structure, warm up and enter the gaseous phase very rapidly. The gaseous cryogen will displace the air that is present in the structure out of the structure and reduce the content of oxygen in the structure to about 10 parts per million when welding can begin. | 8 |
BACKGROUND OF THE INVENTION
[0001] I. Field of the Invention
[0002] The present invention relates generally to container handling equipment, including systems for accessing, grabbing, lifting and tipping a wide range of sizes and shapes of collection containers into charging hoppers or compartments of side loading collection vehicles, or other receptacles, and thereafter returning empty containers to their pickup locations. More particularly, the present invention relates to an automated container handling system including a container grabbing device, that is not only capable of lateral extension, but also capable of full lift and dump operation in very close quarters. A linearly-operating lift system is provided to lift and lower containers that cooperates with a pivoting, short-arm container grabbing device with hydraulic fingers. A rotary actuator pivots the grabbing device to adjust grabbing angle, tip containers and rotate it to and from a stowed position.
[0003] II. Related Art
[0004] Various vehicles dedicated to the collection of refuse or recyclables have included mechanized container handling devices that allow an operator to cause the device to access, lift, empty and return containers of interest without the need for any direct interaction by the operator so that the operator may remain in the vehicle. Such a holding or grabbing device is generally connected to an arm or extendable boom which is connected, in turn, to a base mounted on the vehicle. The arm or boom and grabbing device are operated in concert to access and engage a container of interest, lift and dump the container into a receiving hopper and return the empty container to the original location. One device of the class with an extensible boom is shown in U.S. Pat. No. 5,657,654 to Christenson and assigned to the same assignee as the present invention. Grabbing devices are also known which have opposed arms or fingers that converge around the girth of containers. Such devices generally have themselves been attached to extended arm members configured to pivot in a generally vertical plane to lift and invert a captured container and return it empty to an upright position. One such container grabbing device is illustrated and described in U.S. Pat. No. 5,769,592 to Christenson and also assigned to the same assignee as the present invention.
[0005] Systems also have been devised in which converging/diverging gripper arms are mounted on a carriage to reciprocate along a lift assembly using a chain drive or another mechanism. Such systems are disclosed in U.S. Pat. No. 5,230,393 and RE34,292. Another device is shown in U.S. Pat. No. 5,702,225 which depicts a pivoting linear lifting system operable along a pair of spaced rails. Curves in upper portions of the rails determine and control the tipping angle and radius for a captured container.
[0006] Mechanisms of known container handling devices generally have a large number of moving parts and articulated joints which are exposed to the extreme clogging and corrosive conditions of refuse collection, and, as such, tend to require frequent maintenance. It would thus be advantageous to provide a simplified mechanism to automatically operate the lift and dump arm function that reduces mechanism complexity and maintenance requirements. There is also a need to reduce the required lateral and/or vertical distance necessary for operation of such a lift and dump system so that an associated collection vehicle can successfully automate collection in narrower passages such as alleyways, or the like, in addition to emptying curb-side containers on wider streets.
SUMMARY OF THE INVENTION
[0007] By means of the present invention, there is provided a container handling or loading system, including a mechanism able to grab, lift and dump a relatively large range of sizes of refuse containers, which is particularly useful in loading refuse vehicles from the side in close quarters or narrow, confined spaces such as alleyways or the like. The container handling system of the present invention requires no more lateral distance to operate than that required for the truck to pass alongside a container of interest to be emptied. A container sandwiched between a passing truck and a wall, for example, can be automatically accessed, grabbed, lifted, dumped and returned to its original location where only minimum lateral clearance exists. The container handling mechanism of the invention also is one that can optionally move laterally with respect to a refuse truck for accessing, grabbing, lifting, dumping and returning a more laterally remote refuse container to its original location.
[0008] The system includes a pivoting lift frame assembly attachable to a refuse vehicle, a carriage device reciprocally operable along the lift frame assembly, a container grabbing and tipping system carried by the carriage device and further including a short radius rotational tipping mount and a pair of opening and converging opposed grabber arms or fingers. Operating or actuating systems operate the grabber arms and tipping mount to engage and tip a variety of sizes and shapes of containers. A carriage drive system is provided for operating the carriage device linearly along the lift assembly and a system of automatic controls is provided for controlling the operation of the container handling system.
[0009] The container lift frame assembly of the handling system as exemplified in the illustrative embodiment includes a top-pivoting, bottom-extending frame designed to be attached to a material receiving receptacle, in this case, a charging hopper of a side loading refuse vehicle. The frame includes a pair of spaced, generally parallel, side or lift support members spaced and connected by a common upper cross member. The cross member itself, in turn, spans, and is fixed to, a pair of generally vertically disposed telescoping support members designed to ride in vertical channels attached to, or integral with, the sidewall of an associated charging hopper or other receiving receptacle sought to be loaded by the container handling system of the invention.
[0010] The spaced lift support members are mounted so as to pivot in a generally vertical plane relative to the upper cross member and the lower portion of the lift support members are further pivotally attached to a bottom extending frame that includes a pair of spaced, generally parallel, laterally extendable members connected to advance and retract the lower portion of the lift support members thereby causing the upper ends of the lift support members to pivot and the vertical support members to telescope to accommodate the corresponding vertical displacement of frame members thereby accommodating the generally linear lateral displacement of the lower portions. In this manner, the associated container grabber can remain generally at the same height during lateral displacement.
[0011] A carriage system is mounted from the lift support members and carried by a drive system in a manner that enables it to traverse along the lift support members to accomplish a lifting function. The carriage system includes a rotary actuator having a double ended output including output shafts that carry and rotate spaced arm members of a yoke which, in turn, is fixed to a grabbing device for grabbing and releasing containers. The yoke mount enables the grabbing device to be pivoted or rotated generally vertically about a very short radius so as to rotate from a storage to a grabbing or deployed position in limited lateral space and also to adjust the posture of a grabbed container throughout a lift and dump cycle. The grabbing device is preferably one with opposed spaced fingers that close about a container during the grabbing function and open to release the container. The fingers are preferably operated by a compact, fully enclosed hydraulic actuating system that rotates spaced mounting shafts to open and close the fingers. The grabber fingers are designed to accommodate a wide range of container shapes and sizes.
[0012] The carriage is operated along the lift support members by a chain and cylinder mechanism that includes a pair of double-acting, double-ended hydraulic lift cylinders, each operating along a cylinder rod mounted along an associated lift support member in conjunction with a chain carried by sprockets mounted at the ends of each of the lift cylinders in coordinated fashion to operate the carriage and with it the grabber system along the lift support members to raise and lower a captured container. The rods are approximately twice the length of the cylinders. The carriage system is attached to mounts carried by the chains which are also fixed to the lift support members near the midpoints thereof in a manner that enables the carriage to travel the full length of the rods or lift support members or double the distance traveled by the lift cylinders as the chains also move the carriage a distance equal to that traveled by the cylinders.
BRIEF DESCRIPTION OF THE DRAWING
[0013] In the drawings, wherein like reference characters denote like parts throughout the same:
[0014] FIG. 1 is a rear elevational view partially in phantom of a side-loading vehicle equipped with the container handling system of the invention illustrating two steps in the lift and dump cycle including the accessing and dumping of a container in close quarters;
[0015] FIG. 2 is a view similar to that of FIG. 1 showing the container handling system of the invention in lateral extension demonstrating two positions including the accessing and dumping of a container of interest located a lateral distance from the side of the vehicle;
[0016] FIG. 3 is a view showing a chain and cylinder combination drive system associated with the raising and lowering of the carriage and grabber system along a side frame member in the equivalent of a fully lowered and fully raised position;
[0017] FIG. 4 is a greatly enlarged perspective view depicting a fully enclosed hydraulic actuating system for operating the fingers of a grabber suitable for use in the container handling system of the invention;
[0018] FIG. 5 is a fragmentary perspective view of a collection vehicle body with parts removed for clarity showing parts of a side loading receiving hopper equipped with a container handling system in accordance with the invention illustrating the container handling system in a fully retracted or stowed position;
[0019] FIG. 6 is a fragmentary perspective view of a collection vehicle body with parts removed for clarity equipped with a container handling system in accordance with the invention with the grabber lowered and rotated to a generally horizontal posture;
[0020] FIG. 7 is a view similar to FIG. 6 showing the container handling system addressing the remote container;
[0021] FIG. 8 is a view similar to FIGS. 6-7 showing the container being raised for emptying;
[0022] FIG. 9 is a view similar to FIGS. 6-8 showing the container being tipped; and
[0023] FIG. 10 is a schematic perspective representation of a side loading refuse vehicle employing an embodiment of the present invention.
DETAILED DESCRIPTION
[0024] The container handling system of the present invention represents advances in the automated lifting and emptying of containers, particularly with regard to manipulating containers in close quarters and addressing a wide variety of container sizes and weights. The system enables the lifting and tipping of containers with little or no lateral room in a manner which also enables the containers to remain generally upright throughout the grabbing and lifting process until the final tipping. The system greatly reduces the need for lateral and vertical space associated the lift and tip operations.
[0025] The container handling system is able to handle containers in a wide range of sizes and shapes including large, heavy containers. For example, such a system handles anything from normal 34 gallon (129 liter) residential curb-side containers to much larger containers such as 300 gallon (1136 liter) containers weighing 1200 pounds (544.2 kg) or more. The entire operation of the system may be automated and micro-processor controlled. The detailed embodiment shown here is meant to illustrate the concepts of the invention and not to limit the scope in any manner. Variations will occur to those skilled in the art.
[0026] FIG. 1 depicts a rear elevational view partially in phantom of a side loading refuse truck denoted generally by the reference character 20 which represents one of several types of vehicles for which the container handling system of the present invention is particularly well suited. The vehicle includes a truck body 22 mounted on a truck chassis generally at 24 . The truck body 22 is of a rear discharge type including tailgate 26 , top hinged by a pair of hinges as at 28 . A container handling mechanism, in accordance with the invention is depicted generally at 30 and includes a container grabber mechanism generally at 32 . The grabber mechanism is shown in one position having grabbed and retrieved a container 34 and in a tipping position, shown in phantom, emptying the container 34 into a forward charging hopper of the truck body 22 . In FIG. 1 , the container handling mechanism is depicted with the left frame in a fully upright or vertical posture, with the lower portion of the mechanism fully retracted. This enables operation in the narrowest of quarters, as it will be noted that a container as at 34 need simply be grabbed, lifted vertically and tipped.
[0027] FIG. 2 is a view similar to that of FIG. 1 showing the container handling system of the invention in lateral extension accessing, or replacing, and tipping container 34 located a distance laterally away from the vehicle 20 with the tipping position again being shown in phantom.
[0028] The details of the container handling system 30 are best depicted in FIGS. 3-9 . The system has a main frame that includes a pair of structural side or lift support members or structures 40 and 42 carried by an upper cross member in the form of a connecting bar 44 . As best seen in FIGS. 8 and 9 , the lower portions of members 40 and 42 are pivotally connected at 46 and 48 , respectively, to a bottom extending frame that includes link members 50 and 52 which, in turn, are pivotally connected at 54 and 56 to a pair of spaced, generally parallel retractable. Lateral support structural members 58 and 60 which are generally horizontally mounted and designed to move laterally, generally parallel to the bottom 62 of the truck body 22 and are attached to be operated by an outer connecting cross member 64 . The bottom extending frame is reciprocally operated laterally by a cylinder 66 ( FIGS. 1 and 2 ) and rod 68 attached to member 64 as by a clevis or the like 70 .
[0029] The upper cross member 44 connects a pair of spaced parallel members 72 and 74 ( FIG. 6 ) which are telescopically engaged in respective generally vertical hollow shapes 76 and 78 abutting the structural sidewall 79 of the forward charging hopper of truck body 22 . This allows the upper end of the main frame to move and adjust in a generally vertical direction as needed with the lateral displacement of the grabber as will be described.
[0030] The carriage and grabber system includes a carriage device 80 that is mounted to travel along the length of structural lift support members 40 and 42 and includes a pair of housings that include plate box structures 82 and 84 and structure members 86 and 88 which support a double-ended or double-output shaft rotary actuator 90 therebetween.
[0031] A lift operating system for raising and lowering the carriage system along the structural lift support members 40 and 42 is provided that includes a combination of two mechanisms, one carried by each support member, the details of which are best shown in FIG. 3 . A pair of lift chain segments each having a fixed end and a traveling end and a double-acting fluid cylinder are associated with each support member 40 , 42 . Thus, the mechanism includes a pair of double-acting, double-ended cylinders 92 and 94 mounted to travel along respective cylinder rods 96 and 98 which extend the length of structural lift support members 40 and 42 . As shown in FIG. 3 , the upper and lower ends of cylinder rod 96 are connected between suitable heavy structural plates or gussets 100 and 102 fixed as at 104 and 106 . The cylinder 92 is moved along the cylinder rod 96 by hydraulic fluid supplied and drained through the rod in a well known manner. A pair of chain sprockets including an upper sprocket 108 and a lower sprocket 110 are mounted on the ends of cylinder 92 . Both sprockets are idler or freewheeling sprockets, and chain segments 111 and 112 are engaged around the sprockets. The chain segments 111 and 112 are connected at one end to a fixed member 114 and at the other end to a moving member 116 . The member 114 is fixed to the lift support member 40 and the member 116 is fixed to plate 118 which is part of box 82 of the assembly that carries one side of the carriage 80 . As the cylinder 92 moves upward, or downward, this configuration produces an additional equidistant movement of the chain segments 111 and 112 and with them the plate 118 , along the cylinder, causing the plate at 118 to move a distance along the member 40 twice that moved by the cylinder as illustrated in FIG. 3 . With reference to both lift support members, of course, the carriage 80 will move double the distance moved by the cylinder.
[0032] The output shafts of the double-ended rotary actuator 90 of the carriage system 80 are connected to rotate relatively short, spaced arms of a heavy yoke device 120 ( FIGS. 6-9 ) which, in turn, is fixed to and carries grabber mechanism 122 which itself includes a totally enclosed, fluid-operated (preferably hydraulic) actuator 124 which operates a pair of opposed converging and diverging arms or grabber fingers 126 and 128 used to capture and release a container of interest. An enlarged view of the totally enclosed fluid-operated actuator 124 is shown in FIG. 4 and includes a central gear case or housing 130 and a pair of rotating output shafts 132 and 134 which, in turn, are keyed to rotate and operate a pair of connector devices 136 and 138 which, in turn, are connected, respectively, to operate the grabber fingers 126 and 128 in a manner familiar to those skilled in the art.
[0033] FIGS. 5-9 further illustrate steps in a typical sequence of operating the container handling system of the invention which illustrate accessing, grabbing, lifting and tipping a collection container. Thus, FIG. 5 depicts the illustrative embodiment of the container handling system of the invention in a fully stowed configuration with the gripper mechanism raised and rotated inward in a tipping posture. An alternate embodiment of the grabber fingers is shown at 126 a and 128 a. The bottom extending frame is fully retracted so that the system assumes a very narrow lateral profile abutting the side of the charging hopper of the truck body 22 . A container of interest 34 is shown at a lateral distance away from the container handling system in FIG. 6 . The grabber mechanism is shown rotated into a forward generally horizontal grabbing posture prior to any lateral extension of the system toward container 34 . FIG. 7 shows the bottom extending frame advanced with the grabber system having engaged and closed about the container 34 prior to raising of the container. FIG. 8 shows the system with the lift operation completed and the carriage 80 at the top of the lift support members 40 and 42 .
[0034] It will be appreciated that the container 34 has been maintained in an upright position throughout the grabbing and lifting sequence and is positioned for tipping. The carriage has simply moved up the incline of the frame. In FIG. 9 , the short-armed grabber yoke has been rotated to tip the container 34 and empty it into the charging hopper of the refuse truck.
[0035] Tipping having been completed, a simple reversal of the steps utilized to empty the container enables the container to be returned to the exact spot where it was picked up, because the bottom-extending frame has not moved from the pickup posture. The container handling system thereafter is returned to its stowed or traveling position. The design of the system of the invention, of course, results in a container handling system which, without the need for further motion or controls, at all times, returns a container being handled to its original spot. Of course, the system also works particularly well for close-in containers without the need to extend the bottom extending frame, as illustrated in FIG. 1 , enabling the emptying of containers of interest in very close quarters wherein the container is simply grabbed and lifted vertically and tipped.
[0036] An important aspect of the container handling system of the invention involves in the ability of the system to unload containers in a wide variety of sizes. Thus, the system is designed to grab, lift and dump any container size between about 34 gallons (129 liters)and up to even very large and heavy containers up to about 300 gallons (1136 liters) weighing #1200 lbs (544.2 kg) or more with the grabber fingers enabled to seize a container in such a wide range of sizes without slipping or crushing. This is because the need for elongated arms or other cantilevered parts has been eliminated. While the system is able to grab, lift and dump containers of this wide range of sizes in narrow spaces like alleys, it may also reach such containers where the distance from the side of the truck to the center of the container is up to 8 feet (2.44 meters) or more in one model. The cycle time can be quite rapid for the container handling system of the invention inasmuch as there is no need to retract an arm (or the access and lift frame) in order to lift and invert the container or re-extend the arm (or the access and left frame) to return the container to its original site.
[0037] FIG. 10 shows a schematic perspective representation of a side loading refuse vehicle including an embodiment of the present invention in full lateral extension. This represents the lowest vertical position for unloading.
[0038] This invention has been described herein in considerable detail in order to comply with the patent statutes and to provide those skilled in the art with the information needed to apply the novel principles and to construct and use such specialized components as are required. However, it is to be understood that the invention can be carried out by specifically different equipment and devices, and that various modifications, both as to the equipment and operating procedures, can be accomplished without departing from the scope of the invention itself. | A container handling mechanism suitable for mounting on the side of a refuse vehicle for loading material from refuse containers is disclosed that includes a lift assembly, having a pair of spaced, generally parallel lift support members, attachable to a refuse vehicle, a carriage device reciprocally operable along the lift support members of the lift assembly, a container grabbing system carried by the carriage device and further including a pair of opposed grabber fingers and an actuator system for closing and opening the grabber fingers to engage and release containers of interest, the container grabbing system being vertically pivotable on a short radius for adjusting the position of and tipping a container. A chain and cylinder drive system operates the carriage device along the lift assembly, and a control system controls operation of the container handling mechanism. | 1 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims priority to and the benefit of Korean Patent Application No. 10-2013-0046775 filed in the Korean Intellectual Property Office on Apr. 26, 2013, the entire contents of which are incorporated herein by reference.
BACKGROUND
[0002] (a) Field
[0003] The present disclosure relates to a deposition apparatus, a deposition system comprising the deposition apparatus and a method of manufacturing an organic light emitting diode display.
[0004] (b) Discussion of the Related Technology
[0005] An organic light emitting diode (OLED) display is a flat panel display which can be made lightweight and thin because it has a self-luminous characteristic and requires no separate light source. Particularly, the OLED display exhibits quality characteristics such as low power consumption, high luminance, high response speed, and as such, the OLED display receives much attention as a next-generation display device.
[0006] In general, an OLED display includes an organic light emitting element including an anode, an organic emission layer, and a cathode. Holes and electrons are injected from the anode and the cathode, respectively, to form excitons, and the excitons make a transition to a ground state, thereby causing the organic light emitting diode to emit light.
[0007] The anode and the cathode may be formed of a metal thin film or a transparent conductive thin film and the organic emission layer may be formed of at least one organic thin film. A vacuum deposition method may be used to form such an organic thin film, a metal thin film, and the like, on a substrate of the organic light emitting diode display. Generally, the vacuum deposition method is used for forming an organic thin film, a metal thin film, and the like. In a deposition device including a deposition source, a deposition material is inserted into a crucible and heated for deposition of the deposition material on the substrate such that a thin film is formed.
[0008] The above information disclosed in this Background section is only for enhancement of understanding of the background of the invention and therefore it may contain information that does not form the prior art.
SUMMARY
[0009] One aspect of the present invention provides a deposition apparatus that can process a plurality of substrates generally in parallel and minimize process standby time such as alignment of substrates and deposition masks and alignment time to achieve high productivity, and a deposition system including the same.
[0010] In addition, another aspect of the present invention provides a manufacturing method of an organic light emitting diode display using a deposition chamber and a deposition system.
[0011] A deposition apparatus according to an exemplary embodiment includes: a deposition chamber; a plurality of substrate holders comprising a first holder configured to maintain a substrate at a first substrate position in the deposition chamber and a second holder configured to maintain another substrate at a second substrate position in the deposition chamber, a deposition source disposed in the deposition chamber and configured to supply a deposition material to apply onto substrates placed at the first and second substrate positions, and a deposition source transfer mechanism configured to move the deposition source to be opposite to one of the first and second substrates in a first direction, a substrate transfer mechanism configured to transfer a substrate in a second direction to or from the first substrate position and further configured to transfer another substrate in the second direction to or from the second substrate position.
[0012] The deposition chamber may further include a mask transfer mechanism configured to transfer at least one deposition mask to a first mask position disposed between the first substrate position and the first source position and a second mask position disposed between the second substrate position and the second source position.
[0013] The deposition chamber may further include a mask storing chamber attached to the deposition chamber and configured to store at least a deposition mask, and the mask storing chamber is connected with the mask transfer mechanism.
[0014] The mask transfer mechanism may be provided in one side end of the deposition chamber along the first direction and is configured to move a mask along the first direction between the mask storing chamber and the deposition chamber.
[0015] The deposition chamber may further include a mask cleansing chamber connected with the mask storing chamber and the deposition chamber and cleansing the deposition mask.
[0016] The mask cleansing chamber may be provided between the deposition chamber and the mask storing chamber.
[0017] The deposition chamber may further include an alignment device configured to align the respective substrates and the deposition masks.
[0018] The mask transfer mechanism may include a pair of rails extending in the first direction, the deposition mask comprises a mask main body that a shielding portion and an opening are formed and a frame supported by the rails by fixing the mask main body, and the frame of the deposition mask may further include a protection plate surrounding the rails.
[0019] A deposition system according to an exemplary embodiment includes a plurality of the deposition apparatus each of which comprises the deposition chamber, and a plurality of transfer chambers provided between and connect two immediately neighboring deposition chambers.
[0020] The deposition system may a mask transfer mechanism configured to transfer at least one mask to a first mask position disposed between the first substrate position and the first source position and to a second mask position disposed between the second substrate position and the second source position.
[0021] The deposition system may be configured to coordinate the substrate transfer mechanism and the mask transfer mechanism such that when a substrate is provided into the deposition chamber from the transfer chamber, the substrate is transferred along the second direction, and a deposition mask is transferred along the first direction that crosses the second direction.
[0022] The transfer chamber may accommodate the substrate transfer mechanism.
[0023] The deposition chamber may further include a buffer chamber connected to the transfer chamber. In this case, the substrate transfer portion may include a robot arm structure.
[0024] A manufacturing method of an organic light emitting diode display according to an exemplary embodiment includes: providing the deposition apparatus, transferring a first substrate and a second substrate independently into the deposition chamber to place the first substrate at the first substrate position and the second substrate at the second substrate position, providing a first deposition mask and a second deposition mask into the deposition chamber, aligning the first substrate and the first deposition mask at a first alignment location, transferring the deposition source to the first alignment location, applying a deposition material to the first substrate, aligning the second substrate and the second deposition mask at a second alignment location, transferring the deposition source to the second alignment location; and applying the deposition material to the second substrate.
[0025] The alignment to the second alignment location may be performed while the deposition material is applied to the first substrate.
[0026] The manufacturing method of the organic light emitting diode display may further include, after the spraying of the deposition material to the first substrate, discharging the first substrate from the deposition chamber.
[0027] A manufacturing method of an organic light emitting diode display according to another exemplary embodiment includes: providing the deposition apparatus, transferring a first substrate and a second substrate independently into the deposition chamber to place the first substrate at the first substrate position and the second substrate at the second substrate position, providing a first deposition mask and a second deposition mask into the deposition chamber, aligning the first substrate and the first deposition mask at a first alignment location, transferring the deposition source to the first alignment location, applying a deposition material to the first substrate, aligning the second substrate and the second deposition mask at a second alignment location, transferring the deposition source to the second alignment location; and applying the deposition material to the second substrate. While the deposition material is applied to the first substrate, the second substrate and the second mask are transferred to be aligned at the second alignment location. After the deposition material is applied to the first substrate, the first substrate is discharged from the deposition chamber.
[0028] The plurality of the deposition apparatuses may comprise first and second deposition apparatus, wherein the deposition materials used in the first and second deposition apparatuses are substantially different from each other.
[0029] The plurality of the deposition apparatuses may comprise first and second deposition apparatus, wherein the deposition mask used in the first deposition apparatus and the deposition mask used in the second deposition apparatus are substantially different from each other.
[0030] According to the exemplary embodiments of the present invention, a thin film process can be sequentially performed in a plurality of process lines provided in each of a plurality of deposition chambers through a single deposition source provided in each of the deposition chamber so that cost can be saved and productivity can be improved.
[0031] Further, standby time can be shortened by performing substrate transferring and substrate and mask alignment with respect to a substrate in a process line while a thin film deposition process is performed on a substrate in another process line, thereby further improving productivity.
BRIEF DESCRIPTION OF THE DRAWINGS
[0032] FIG. 1 is a top plan view of a deposition system according to a first exemplary embodiment.
[0033] FIG. 2 is a schematic side view of a deposition chamber of the deposition system according to the first exemplary embodiment.
[0034] FIG. 3 is a partially enlarged view of the deposition chamber of the deposition system according to the first exemplary embodiment.
[0035] FIG. 4 is a partial enlarged view of the deposition system according to the first exemplary embodiment.
[0036] FIG. 5 and FIG. 6 are top plan views of a substrate transfer portion of the deposition system according to the first exemplary embodiment.
[0037] FIG. 7 is a top plan view of a deposition system according to a second exemplary embodiment.
[0038] FIG. 8 is a schematic side view of a deposition chamber of a deposition system according to a third exemplary embodiment.
[0039] FIG. 9A to FIG. 9C are schematic diagrams of a manufacturing method of an organic light emitting diode (OLED) display according to an exemplary embodiment.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0040] Hereinafter, a deposition chamber, a deposition system including the deposition chamber, and a manufacturing method of an organic light emitting diode display will be described in further detail with reference to the accompanying drawings. However, the present invention is not limited to the exemplary embodiments disclosed hereinafter but has many variations, and the exemplary embodiments described hereinafter are provided to make the disclosure of the present invention complete and to completely inform a person of ordinary skill in the art the scope of the present invention. In the drawings, like reference numerals refer to like elements.
[0041] In addition, unless explicitly described to the contrary, the word “comprise” and variations such as “comprises” or “comprising”, will be understood to imply the inclusion of stated elements but not the exclusion of any other elements. Further, the word “on” means positioning on or below the object portion, but does not essentially mean positioning on the upper side of the object portion based on a gravity direction.
[0042] In order to form an organic thin film, a metal thin film, and the like using the vacuum deposition method, a deposition system such as a cluster-type deposition system, an inline deposition system, and the like may be used. The inline deposition system is a deposition system in which a substrate loading chamber, a substrate unloading chamber, and a plurality of deposition chambers disposed between the substrate loading chamber and the substrate unloading chamber are arranged in a row, and has a merit of shortening a process time compared to the cluster-type deposition system.
[0043] FIG. 1 is a top plan view of a deposition system according to a first exemplary embodiment, FIG. 2 is a schematic side view of a deposition chamber according to the first exemplary embodiment, and FIG. 3 is a partial exploded perspective view of the deposition chamber according to the first exemplary embodiment.
[0044] Referring to FIG. 1 , a deposition system according to the first exemplary embodiment includes a plurality of deposition chambers 100 and a plurality of transfer chambers 300 .
[0045] The deposition chamber 100 is a means for forming a thin film of a substrate 122 , and is provided in plural corresponding to the number of thin films formed on the substrate 122 .
[0046] For example, when a display device formed on the substrate 122 is an organic light emitting diode (OLED) display, an emission layer ELM is formed, and a hole injection layer (HIL), a hole transport layer (HTL), an electron transporting layer ETL, and an electron injection layer may be further formed. In addition, a metal thin film functioning as a cathode or an anode or a transparent conductive thin film may be further formed on the substrate 122 . The thin films are formed in different deposition chambers 100 , and therefore the number of the deposition chambers 100 according the present exemplary embodiment corresponds to the number of an organic thin film, a metal thin film, and the like.
[0047] Referring to FIG. 2 , each of the deposition chambers 100 includes a chamber main body 110 , a substrate fixing portion 120 , a deposition source 130 , a deposition source transfer portion 140 , and a mask transfer portion 150 .
[0048] The chamber main body 110 defines an inner space formed therein, and performs a process for forming a thin film on the substrate 122 in the space. A vacuum pump (not shown) that decreases an internal pressure by discharging gas from the space and a venting means (not shown) that increases the internal pressure in the chamber main body by injecting a constant gas to the inner space of the chamber main body may further be provided.
[0049] The substrate 122 ( 122 a , 122 b ) is transferred into the inner space of the chamber main body 110 and fixed to be opposite to a spray nozzle of the deposition source 130 by the substrate fixing portion 120 ( 120 a and 120 b ). A process and structure for carrying the substrate 122 into the inner space of the chamber main body 110 and discharging the substrate 122 from the chamber main body 100 will be described later.
[0050] The substrate fixing portion or substrate holder 120 has a structure for easily attaching and detaching the substrate 112 so as to stably fix the substrate 122 while a thin film of a deposition material is formed and then discharge the substrate 122 from the inner space of the chamber main body 110 after termination of the treatment.
[0051] The substrate fixing portions 120 a and 120 b are provided in plural to treat a plurality of substrates in the deposition chamber 100 during one deposition process. The plurality of substrate fixing portions 120 a and 120 b respectively fix or hold the plurality of substrates 122 a and 122 b and can maintain the substrates at their deposition stations. In embodiments, the substrate holders 120 a and 120 b may be fixed in the deposition stations. In alternative embodiments, the substrate holders 120 a and 120 b may be movable to transfer substrates to the deposition stations and stop at the deposition stations to maintain the transferred substrates at the deposition stations.
[0052] In the present exemplary embodiment, the substrate fixing portion 120 is exemplarily formed of two fixing portions, i.e., the first substrate fixing portion 120 a and the second substrate fixing portion 120 b , but it is not restrictive. The first substrate fixing portion 120 a and the second substrate fixing portion 120 b fix the first substrate 122 a and the second substrate 122 b , respectively corresponding thereto. And the first substrate fixing portion 120 a and the second substrate fixing portion 120 b may be disposed generally in parallel with each other and arranged along a first direction (i.e., x-axis direction) for the respective substrates 122 a and 122 b to be opposite to the deposition source 130 .
[0053] In addition, during a deposition process with respect to the substrates 122 a and 122 b , the first substrate fixing portion 120 a and the second substrate fixing portion 120 b may be disposed at a distance from each other, interposing a gap therebetween along the first direction so as to prevent the deposition material from being attached to the second substrate that is waiting for deposition while depositing the first substrate.
[0054] Referring to FIG. 3 , as a means for discharging a deposition material for deposition to the substrate 122 , the deposition source 130 is provided with a space (not shown) for containing a deposition material such as an organic material, and spray nozzles 134 spraying the deposition material are formed in one side of the deposition source 130 , disposed opposite to the substrate 120 .
[0055] The deposition material containing space may be formed of a ceramic material having an excellent heat emission feature, such as alumina (Al2O3), aluminum nitride (AlN), and the like, and it is not restrictive. The deposition material receiving space may be formed of various materials having excellent heat emission feature and heat resistance.
[0056] Heater (not shown) may be formed to surround the external surface of the deposition material containing space in a closely attached manner, and the heater heats the received deposition material for vaporization of the deposition material.
[0057] As shown in FIG. 3 , the deposition source 130 may be provided as a linear deposition source extended in a second direction (i.e., y-axis direction) that crosses the first direction. In embodiments, the x-axis direction and the y-axis direction are generally perpendicular to each other. In this case, the linear deposition source may be extended corresponding to the length of the substrate opposite thereto.
[0058] An angle control member 136 that controls or limits a spray angle of the deposition material may be formed at the periphery area of the spray nozzles 134 . As shown in FIG. 3 , the angle control member 136 is extended along a length direction of the linear deposition source 130 to make the organic material uniformly sprayed on the substrate 30 by controlling a deposition angle of the deposition material sprayed from the spray nozzles 134 , and prevents the deposition material from being attached to other substrate that does not experience a deposition process during the deposition process.
[0059] As a means for transferring the deposition source 130 , the deposition source transfer portion or deposition source transfer mechanism 140 moves the deposition source 130 to be opposite to one of the substrates 122 a and 122 b . The deposition source transfer portion 140 enables a single deposition source 130 to be sequentially deposited to the plurality of substrates 122 a and 122 b.
[0060] When the deposition process is performed to the first substrate 122 a , the deposition source 130 is disposed at a location that is opposite to the first substrate 122 a through the deposition source transfer portion 140 . When the deposition process for the first substrate 122 a is finished, the deposition source 130 is disposed at a location that is opposite to the second substrate 122 b through the deposition source transfer portion 140 for performance of the deposition process.
[0061] A plurality of deposition masks 160 includes two deposition masks 160 a and 160 b , and is provided as a means for forming patterns of an organic thin film on the substrate 122 . In a deposition mask, openings are formed between shielding portions that block deposition of the organic material such that the organic material is deposited on the substrate 122 through the openings.
[0062] The deposition mask 160 is disposed under one surface of the substrate 122 , to which the pattern of the organic thin film is to be formed. In the present exemplary embodiment, the deposition process is performed with respect to two substrates 122 in one chamber, and therefore two deposition masks 160 a and 10 b are used.
[0063] The two deposition masks 160 a and 160 b are transferred and placed to correspond to the substrates 122 a and 122 b by the mask transfer portion or mask transfer mechanism 150 . As a means for arranging the deposition masks 160 a and 160 b at mask locations respectively corresponding to the substrates 122 a and 122 b , the mask transfer portion 150 may transfer the deposition masks 160 a and 160 b generally in parallel with the first direction (x-axis direction).
[0064] The mask transfer portion 150 includes a pair of rails 152 extending in the first direction (x-axis direction) as shown in FIG. 3 separated from a distance with a predetermined gap along the second direction (y-axis direction) and a plurality of rollers 154 arranged along a length direction of the pair of rails 152 and contacting the deposition mask.
[0065] When the deposition mask 160 is being transferred, friction between the deposition mask 160 and the rail 152 is reduced by the rollers 154 so that the deposition mask 160 can be smoothly transferred.
[0066] In this case, the deposition mask 160 is disposed between the pair of rails 152 . And the deposition mask 160 includes a mask main body 162 where the shielding portion and the openings are formed and a frame 164 fixing the mask main body 162 and supported by the rails 152 .
[0067] The deposition mask 160 may further include a protection plate 166 extending from one side of the frame 164 to prevent the deposition material from being attached to the rails 152 . That is, the protection plate 166 is extended from a side opposite to the spray nozzles 134 to cover the rail 152 .
[0068] In the present exemplary embodiment, the mask transfer portion 150 is illustrated as a rail, but it is not restrictive. The mask transfer portion 160 may have various shapes as long as the deposition mask 160 is transferred to one direction and arranged at a predetermined location. In addition, the deposition mask 160 may have various shapes as long as it is being supported by the mask transfer portion 150 and transferred along the mask transfer portion 150 .
[0069] Referring back to FIG. 2 , a mask storing chamber or mask storage 200 may further be included to store the deposition mask 160 at one side of the chamber main body 110 . The mask storing chamber 200 stores a required deposition mask 160 according to the type of an organic thin film, a metal thin, film, and the like formed in each deposition chamber 100 , and discharges the deposition mask 160 toward the inner space of the chamber main body 110 during the deposition process.
[0070] The mask storing chamber 200 is connected with the mask transfer portion 150 to mount the deposition mask 160 discharged from the mask storing chamber 200 to the mask transfer portion 150 .
[0071] In this case, the deposition mask 160 may be mounted to the mask transfer portion 150 using a mask transfer holder (not shown).
[0072] In order to arrange the substrates 122 a and 122 b and the deposition masks 160 a and 160 b at predetermined locations, respectively, a first alignment portion 170 a and a second alignment portion 170 b may be formed at one side of the chamber main body 110 . The first alignment portion 170 a aligns the first substrate 122 a and the first deposition mask 160 a , and the second alignment portion 170 b aligns the second substrate 122 b and the second deposition mask 160 b.
[0073] FIG. 4 is a partially exploded side view of the deposition chamber according to the first exemplary embodiment.
[0074] The mask storing chamber 200 is connected with the mask transfer portion 150 to make the deposition mask 160 transferred from the inner space of the chamber main body 110 into the mask storing chamber 200 through the mask transfer portion 150 after the deposition process is finished. In addition, the deposition mask 160 stored in the mask storing chamber 200 is carried into the deposition mask 160 again for a deposition process.
[0075] As shown in FIG. 1 , the deposition system according to the exemplary embodiment includes a plurality of deposition chambers 100 and a plurality of transfer chambers 300 disposed between the deposition chambers 100 to connect neighboring deposition chambers 100 .
[0076] In embodiments, the substrates 122 are provided by being transferred along a direction (for example, y-axis direction) to which the deposition chambers 100 and the transfer chambers 300 are connected, and the deposition mask 160 may be provided along another direction (for example, x-axis direction) that crosses the transfer direction of the substrate 122 .
[0077] As shown in FIG. 1 , when the deposition chamber 100 and the transfer chamber 300 are arranged in a row along the second direction (y-axis direction), the substrate 122 may be transferred along the alignment direction of the chambers. When the two substrates 122 a and 122 b are processed in a single deposition chamber 100 , the two substrates 122 a and 122 b may be provided generally in parallel with the chamber alignment direction (refer to AL and BL of FIG. 1 ).
[0078] FIG. 5 and FIG. 6 are top plan views illustrating exemplary variations of the substrate transfer portion according to the first exemplary embodiment.
[0079] The transfer chamber 300 includes a substrate transfer portion or substrate transfer mechanism 310 a that discharges the substrate 122 from an adjacent deposition chamber and carries the discharged substrate 122 into another deposition chamber. As shown in FIG. 5 , the substrate transfer portion 310 a may be formed in the shape of a robot arm. The robot arm is inserted in a deposition chamber 1001 where the deposition process is finished and grips the substrate 122 , and then mounts the gripped substrate 122 in a substrate fixing portion 120 in another adjacent deposition chamber 1002 where the next deposition process is going to be performed.
[0080] In addition, as shown in FIG. 6 , the substrate transfer portion 310 may be formed using a sliding method. And the substrate transfer portion 310 includes a substrate tray 312 on which the substrate 122 is mounted or placed and a sliding guide 314 along which the substrate tray 312 is slid. After the substrate tray 312 is inserted in the deposition chamber 1001 where the deposition process is finished and then the substrate 122 is mounted on the substrate tray 312 , the substrate 122 is mounted to a substrate fixing portion 120 in another adjacent deposition chamber 1002 where the next deposition process is going to be performed.
[0081] In addition, the deposition system according to the exemplary embodiment may further include a loading chamber 400 and a substrate unloading chamber 500 . The substrate 122 is loaded into the deposition system through the substrate loading chamber 400 , and a deposition material is deposited in each of the deposition chamber 100 to form an organic thin film on the substrate 122 , and then the substrate 122 is unloaded through the substrate unloading chamber 500 .
[0082] A gate valve may be provided between the substrate loading chamber 400 and the deposition chamber 100 , and another gate valve may be provided between the deposition chamber 100 and the substrate unloading chamber 500 . Each gate valves is provided between one of the deposition chambers 100 and the immediately neighboring transfer chamber 200 . Such a gate valve is opened while the substrate 122 is being transferred and closed while the organic material deposition process is performed such that the organic material deposition process can be performed in a vacuum state.
[0083] FIG. 7 is a top plan view of a deposition system according to a second exemplary embodiment.
[0084] Referring to FIG. 7 , a deposition system according to the present exemplary embodiment further includes a buffer chamber 320 connected with a transfer chamber 300 at one side of the transfer chamber 300 . When the substrate 122 is damaged or a problem occurs in a deposition chamber 100 or a transfer chamber 300 , the substrate 122 may be transferred into the buffer chamber 320 and then stored.
[0085] The buffer chamber 320 is provided in connection with the transfer chamber 300 at a location that is spaced apart from a transfer path of the substrate 122 in order not to interrupt transferring of the substrate 122 . When the substrate transfer portion 310 of the transfer chamber 300 is provided in the shape of a robot arm, the buffer chamber 320 is provided adjacent to the substrate transfer portion 310 formed in the shape of the robot arm to temporarily store the substrate, and accordingly, a time loss that may occur during mass production can be reduced.
[0086] In the deposition system according to the present exemplary embodiment, other configuration than the buffer chamber 320 may be the same as that of the first exemplary embodiment.
[0087] FIG. 8 is a schematic side view of a deposition chamber of a deposition system according to a third exemplary embodiment.
[0088] Referring to FIG. 8 , in a deposition system according to the present exemplary embodiment, a mask cleansing chamber 210 connected with a mask storing chamber 200 and the inside of a chamber main body 110 and cleaning a deposition mask 160 is formed in a lower end portion of the mask storing chamber 200 .
[0089] The mask cleaning chamber 210 is a device for cleaning a deposition material attached to a deposition mask after the deposition mask 160 repeats the deposition process several times, and may clean the deposition mask 160 using plasma or ultraviolet (UV) ray.
[0090] Gate values are respectively provided between the mask storing chamber 200 and the chamber main body 110 , between the mask cleaning chamber 210 and the chamber main body 110 , and between the mask storing chamber 200 and the mask cleaning chamber 210 , and the gate valves are opened when the deposition mask 160 is transferred along the mask transfer portion 150 and the gate valves are closed when the transferring of the deposition mask 160 is finished.
[0091] The mask cleaning chamber 210 is connected with the mask transfer portion 150 and thus the deposition mask 160 transferred from the inner space of the chamber main body 110 after the deposition process can be carried into the mask cleansing chamber 210 through the mask transfer portion 150 . In addition, the deposition mask 160 cleaned in the mask cleaning chamber 210 is carried back into the inner space of the chamber main body 110 for the next deposition process.
[0092] The mask transfer portion 150 may be moved so as to be connected with the mask storing chamber 200 or the mask cleaning chamber 210 . For example, in FIG. 8 , the mask transfer portion 150 is illustrated to be connected with the mask cleaning chamber 210 , but the mask transfer portion 150 may be connected with the mask storing chamber 200 by being transferred upward.
[0093] In the deposition system according to the present exemplary embodiment, a structure, excluding the structure related to the mask cleansing chamber 210 is the same as that of the first exemplary embodiment, and a buffer chamber may be provided as in the second exemplary embodiment.
[0094] Hereinafter, the operation and the manufacturing method will be described by illustrating the deposition system according to the first exemplary embodiment, but a deposition system according to the second or third exemplary embodiment or a deposition system according to the exemplary variations may also be applicable.
[0095] FIG. 9A to FIG. 9C are schematic diagrams sequentially illustrating a manufacturing method of an OLED display according to an exemplary embodiment.
[0096] Referring to the drawing, the manufacturing method of the OLED display according to the exemplary embodiment includes providing a deposition source, placing a mask, aligning a first substrate, transferring the deposition source, depositing the first substrate, aligning a second substrate, transferring the deposition source, and depositing the second substrate.
[0097] First, as shown in FIG. 9A , the deposition source 130 spraying the deposition material is provided in the deposition chamber 100 . The first substrate 122 a is inserted into the deposition chamber 100 . The second substrate 122 b is inserted into the deposition chamber 100 independently from the transfer of the first substrate 122 a . In embodiments, the second substrate 122 b can be inserted into the deposition chamber 100 while depositing the first substrate 122 a.
[0098] The first substrate 122 a and the second substrate 122 b are inserted generally in parallel along the second direction (y-axis direction) where the deposition chamber 100 and the transfer chamber 300 are arranged (refer to AL and BL of FIG. 1 ). The first substrate 122 a and the second substrate 122 b can be arranged generally in parallel with each other, interposing a gap therebetween along the first direction that crosses the transfer direction of the first substrate 122 a and the second substrate 122 b.
[0099] The first deposition mask 160 a and the second deposition mask 160 b are transferred into the deposition chamber 100 . The deposition masks 160 a and 160 b received in the mask storing chamber 200 are discharged and mounted on the mask transfer portion 150 , and then the deposition masks 160 a and 160 b are transferred to predetermined locations.
[0100] That is, the first deposition mask 160 a is transferred to a location corresponding to the first substrate 122 a , and the second deposition mask 160 b is transferred to a location corresponding to the second substrate 122 b . The first substrate 122 a and the first deposition mask 160 a are aligned in a predetermined first alignment location through a first alignment portion 170 a . In embodiments, the first deposition mask 160 a and the second deposition mask 160 b are transferred into the deposition chamber 100 before the first and second substrates are transferred into the chamber 100 , respectively. Alternatively, the first deposition mask 160 a and the second deposition mask 160 b are transferred into the deposition chamber 100 after the first and second substrates are transferred into the chamber 100 , respectively.
[0101] The deposition source 130 is transferred to the first alignment location, and then as shown in FIG. 9B , the deposition material received in the receiving space of the deposition source 130 is heated to be vaporized and then sprayed toward the first substrate 122 a.
[0102] The second substrate 122 b and the second deposition mask 160 b are aligned in a predetermined second alignment location through the second alignment portion 170 b . The aligning of the second substrate 122 b and the second deposition mask 160 b in the second alignment location may be performed while the deposition material is sprayed to the first substrate 122 a . Since the second substrate 122 b is aligned while the deposition material is sprayed to the first substrate 122 a , a process time can be shortened.
[0103] When the deposition process with respect to the first substrate 122 a is finished, as shown in FIG. 9 , the deposition source 130 is transferred to the second alignment location and then the deposition material is sprayed toward the second substrate 122 b.
[0104] After the deposition process with respect to the first substrate 122 a is finished and before a deposition process with respect to the second substrate 122 b starts, the first substrate 122 b may be discharged to the outside of the deposition chamber 100 . During the deposition process with respect to the second substrate 122 b , the first substrate 122 a may be prepared for the next deposition process by being transferred to the next deposition chamber through the transfer chamber 300 . Accordingly, a process time can be shortened.
[0105] After the deposition process with respect to the second substrate 122 b is finished, the second substrate 122 b may also be prepared for the next process by being transferred to the next deposition chamber. Through performing deposition steps of the above-stated deposition process in each deposition chamber, a multi-layered organic thin film may be formed in the substrates 122 a and 122 b.
[0106] While this invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. | A deposition apparatus includes a deposition chamber, a plurality of substrate holders comprising a first holder configured to maintain a substrate at a first substrate position in the deposition chamber and a second holder configured to maintain another substrate at a second substrate position in the deposition chamber, a deposition source disposed in the deposition chamber and configured to supply a deposition material to apply onto substrates placed at the first and second substrate positions, and a deposition source transfer mechanism configured to move the deposition source to be opposite to one of the first and second substrates in a first direction, a substrate transfer mechanism configured to transfer a substrate in a second direction to or from the first substrate position and further configured to transfer another substrate in the second direction to or from the second substrate position. | 2 |
CROSS-REFERENCE TO RELATED APPLICATION
This application claims the priority benefit of Taiwan application serial no. 91101230, filed Jan. 25, 2002.
SCENARIO OF THE INVENTION
1. Field of the Invention
The present invention relates in general to a watermark, and more particularly, to a watermark embedding and extracting method and a watermark embedding hardware structure used in an image compression system.
2. Description of the Related Art
In recent years, many corporations and enterprises have applied the Internet to commercial activities for business promotion. The activities include, for example, electronic shopping, on-line broadcast, on-line filming, and electronic document. A great convenience has been obtained for both the enterprises and the customers. However, problems regarding information security such as allonym transaction, embezzlement, abstraction and interpolation occur. Many of these problems can be resolved by encryption technique. However, copyright approval and inspection problems for the network transmission of valuable medium (such as image, film and music) have to be overcome. Lately, as digital cameras and scanners have become popular, the digitized photograph has become widely distributed over the network. Such a broad distribution results in interpolation and appropriation problems for the photographs, and copyright problems thus occur. The watermark is one of the methods to resolve such problems.
The hidden watermark is applied based on the distortability characteristic of the digital medium, that is, minor modification of digital data does not result in significant effect for sensory perception of human beings. The watermark technique is categorized into a spatial domain and a frequency domain. In the spatial domain, digital data value is directly changed to embed the watermark. Such a method has the advantage of fast operation speed, but it is difficult to resist damage caused by various type of signal process. In the frequency domain, the digital data is transformed into a frequency domain, using Fourier transformation, discrete cosine transformation (DCT), or wavelet transformation, for example. After transformation, the obtained coefficient is used to embed the watermark, which is then converted to the previous spatial domain. The method requires a huge operation, but has a better capability to resist noise processing damage.
The above conventional watermark embedding technique is achieved by software processing. As the watermark embedment requires a huge operation, a complex program is required. Thus, the load on the system is increased, and the performance thereof is affected.
SUMMARY OF THE INVENTION
The invention provides a watermark embedding and extracting method and a watermark embedding hardware structure used in an image compression system. By executing watermark embedment via the watermark embedding hardware structure, the image itself contains the watermark data after image compression, therefore, the performance of the whole system is enhanced.
The watermark embedding method used in the image compression system comprises partitioning an original image into several sub-image blocks. Each of the sub-image blocks B k (k=1, 2, 3, . . . , n, and n is a positive integer) has an 8×8 dimension. A discrete cosine transformation is performed on each of the sub-image blocks B k . A texture analysis and a luminance analysis are performed on each sub-image block by classification to generate analysis data each sub-image block is divided into three levels.
When number {intF k (u,v)/Q k (u,v))≠0}<T 2 and F k (0,0)<T 1 , the sub-image block B k is defined as level 1 that indicates darker luminance and insignificant texture characteristics.
When number {intF k (u,v)/Q k (u,v))≠0}>T 2 and F k (0,0)>T 1 , B k is defined as class 3 that indicates brighter luminance and significant texture characteristics.
When B k is neither class 1 nor class 3, it is defined as class 2 that indicates luminance and texture characteristics between levels 1 and 3.
In the above relationships, F k (0,0) indicates the low frequency value (DC) obtained by performing a discrete cosine transformation on each sub-image block B k , and F k (u,v) indicates the high frequency value (AC) obtained by performing discrete cosine transformation on each sub-image block B k , where u, v≠0. Q(u,v) is the quantized value, T 1 is the low frequency value, and T 2 is the non-zero number in high frequency. According to the analysis value, the image characteristic for each sub-image block is determined, and a corresponding weighted value α k is given. A multiplication for the weighted value and a watermark value is obtained. The data F k * of the watermark embedded into each sub-image block corresponding to a fixed position of the sub-image block is derived from the following equation (1).
F k * = { F k ( u , v ) + ( α k × x i ) , 3 k < i < ( 3 k + 1 ) , ( u , v ) ε { ( 0 , 1 ) , ( 1 , 0 ) , ( 1 , 1 ) } F k ( u , v ) , others ( 1 )
where x i is the embedded watermark value. The embedded watermark value is then quantized and encoded to generate a standard JPEG file.
The invention further provides a watermark extracting method used in an image compression system. The image to be tested X* is partitioned into several sub-image blocks with a dimension of 8×8. The discrete cosine transformation is performed on each sub-image block to obtain several data. A zigzag encoding process is performed to sort the data from low frequency to high frequency. A watermark signal energy W* is extracted at the position where the embedded watermark is. The relationship of Z=W×W*/M is applied to obtain the correlated value Z of the watermark contained in the image to be tested X*. Z is the correlated value of the watermark contained in the image to be tested X*, W is the value of the embedded watermark, and M is the quantity of the embedded watermark. When the correlated value Z is larger than a critical value S z , whether the image to be tested X* contains watermark is determined. The critical value S z can be expressed by
S z = α _ 3 M ∑ i = 1 M W i * ,
where {overscore (α)} is an average weighted value.
The invention further provides a watermark embedding hardware structure, having a discrete cosine transformation register, a quantization table ROM, a first and a second comparator, a first and a second register, a multiplier and an adder. The discrete cosine transformation register is used to store the data obtained by discrete cosine transformation. The quantization table ROM is used to store the quantized values. The first comparator coupled to the quantization table ROM receives and compares the data and the quantized values, and outputs the quantized values. The first register is used to store a first configuration value. The second register is used to store a second configuration value. The second comparator is coupled to the first comparator and the first and second registers to receive and compare the quantized data, the first and second configuration values, so as to output a weight value corresponding to each quantized value. The multiplier is coupled to the second comparator to receive the weighted values and the watermark values. The weighted values are multiplied by the watermark values to output the embedded watermark value. The adder is coupled to the discrete cosine transformation register and the multiplier to receive the embedded watermark values and the data to be embedded with the embedded watermark values. The data is added to the embedded watermark data to output the embedded watermark data. In addition, the embedded watermark data is stored in the discrete cosine transformation and output thereby.
The invention further comprises another watermark embedding hardware structure, comprising a discrete cosine transformation register, a classification detection system, and a watermark embedding apparatus. The discrete cosine transformation register is used to store the data obtained by discrete cosine transformation. The classification detection system is coupled to the discrete cosine transformation register to receive the data, and to output a weighted value, which is generated by a weighted value generator corresponding to each of the data. The watermark embedding apparatus is coupled to the classification detection system and the weighted value generator to receive the weighted values and the watermark values. The weighted values are then multiplied with the watermark values to obtain an embedded watermark value, which is then added with the data to obtain the embedded watermark data, output by the classification detection system. In addition, the embedded watermark data is stored in the discrete cosine transformation register and output thereby.
According to the above, the embedment of watermark executed by the watermark embedding hardware structure provided by the invention allows the image to contain the watermark data therein after image compression, so that the system performance is enhanced. In addition, the watermark embedding hardware structure can be combined with the joint photographic experts group (JPEG) system, and is applicable to image compression systems for digital cameras or scanners.
Both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows an embodiment of a watermark embedding hardware structure used in an image compression system in the invention;
FIG. 2 shows a watermark control process flow of an watermark embedding hardware structure used in an image compression system according to a preferred embodiment of the invention;
FIG. 3 shows an embodiment of a watermark embedding process flow applied to an image compression system;
FIG. 4 shows an embodiment of a watermark extracting process flow applied to an image compression system; and
FIG. 5 shows the correlation and peak signal noise ratio under different compression ratio for a watermark embedding hardware structure used in an image compression system in one embodiment of the invention.
FIG. 6 shows combining a JPEG file with a watermark embedding hardware structure used in an image compression system in one embodiment of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1 , a preferred embodiment of a watermark embedding hardware structure used in an image compression system according to the invention is shown. The embedding hardware structure comprises a discrete cosine transformation (DCT) register 102 , a classification detection system 104 , and a watermark embedding apparatus 106 . The functions for each of the above elements are described as follows.
The DCT register 102 is used to store several data obtained after the discrete cosine transformation. In this embodiment, the DCT register 102 has 64×12 bits.
The classification detection system 104 comprises a quantization table ROM 108 , a first comparator 110 , a first register 112 , a second register 114 , and a second comparator 116 . The quantization table ROM 108 is used to store several quantization values. The first comparator 110 is used to receive the data and the quantization values. The first register 112 is used to store a first configuration value. The second register 114 is used to store a second configuration value. The second comparator is used to receive and compare the quantization values, the first and second configuration values, and to output the weighted value α k corresponding to each of the quantization values. In addition, the weighted value α k is generated by a weighted value generator (not shown).
The watermark embedding apparatus 106 comprises a multiplier 118 and an adder 120 . The multiplier 118 receives the weighted values α k and a watermark value, so as to output an embedded watermark value obtained by multiplying the weighted values α k and the watermark value. The adder 120 receives the embedded watermark value and adds the data with the embedded watermark data to output embedded watermark data, which is then stored in and output by the DCT register 102 .
The whole control process for embedding watermark is completed using an internal control unit 122 as shown in FIG. 2 . The whole control process is divided into four states, that is, an idle state 202 , an S0 state 204 , an S1 state 206 and an S2 state 208 . The idle state 202 lasts until receiving a DCT complete signal. While receiving the DCT complete signal that indicates the completion of the discrete cosine transformation in the DCT module, the S0 state is entered. In S0 state, the data obtained by transformation is input and stored to the DCT register 102 , and the weighted values α k are obtained. The S1 state is then entered to execute the embedding function of the watermark. The S2 state is then entered to output the embedded watermark data obtained by the watermark embedding function. The system then enters the idle state 202 again and standby for the next DCT complete signal.
According the process flow for watermark embedment used in an image compression system in one embodiment of the invention as shown in FIG. 3 , an original image is partitioned into several sub-image blocks. Each sub-image block B k (k=1, 2, 3, . . . , n, where n is a positive integer) has an 8×8 dimension. A forward discrete cosine transformation (FDCT) is performed on each sub-image in step s 302 . Texture and luminance analysis is performed on each sub-image block to obtain an analysis value. According to the analysis value, each sub-image block can be divided into three levels.
When number {intF k (u,v)/Q k (u,v))≠0}<T 2 and F k (0,0)<T 1 , the sub-image block B k is defined as class 1 that indicates darker luminance and insignificant texture characteristics.
When number {intF k (u,v)/Q k (u,v))≠0}>T 2 and F k (0,0)>T 1 , B k is defined as class 3 that indicates brighter luminance and significant texture characteristics.
When B k is neither class 1 nor class 3, B k is defined as class 2 that indicates luminance and texture characteristics between class 1 and class 3.
In the above relationships, F k (0,0) indicates the low frequency value (DC) obtained by performing a discrete cosine transformation on each sub-image block B k , and F k (u,v) indicates the high frequency value (AC) obtained by performing a discrete cosine transformation on each sub-image block B k , where u, v≠0. Q(u,v) is the quantized value, T 1 is a value in low frequency, and T 2 is the non-zero number in high frequency (step s 304 ). According to the analysis value, the image characteristic for each sub-image block is determined, and a corresponding weighted value α k is given. Multiplication of the weighted value and a watermark value is performed. The data F k * of the watermark embedded into each sub-image block corresponding to a fixed position of the sub-image block is derived from the following equation (1).
F k * = { F k ( u , v ) + ( α k × x i ) , 3 k < i < ( 3 k + 1 ) , ( u , v ) ε { ( 0 , 1 ) , ( 1 , 0 ) , ( 1 , 1 ) } F k ( u , v ) , others ( 1 )
where x i is the embedded watermark value, which is a set of random variables ranged between +1 and −1 (as step s 306 ). An inverse DCT (IDCT) is performed on the resultant watermark data F k *, and the standard JPEG file generated by quantization and encoding is obtained (step s 308 ).
In addition, if each sub-image block belongs to class 1, the best image quality is obtained when the weighted value is 2 according to an empirical result. If each sub-image block belongs to class 2, the best image quality is obtained when the weighted value is 6 according to an empirical result. If each sub-image block belongs to class 3, the best image quality is obtained when the weighted value is 9 according to an empirical result. Further, the embedding method comprises a module added with a watermark and a module not added with a watermark, which results in the JPEG file with and without hidden watermark, respectively.
FIG. 4 shows a watermark extracting process flow used in an image compression system according to one embodiment of the invention. An image to be tested X* is partitioned into several sub-image blocks with a dimension of 8×8. The discrete cosine transformation is performed on each sub-image block to obtain several data. A zigzag encoding process is performed to sort the data from low frequency to high frequency (step s 402 ). A watermark signal energy W* is extracted at the position where the embedded watermark is (step s 404 ). The relationship of Z=W×W*/M is applied to obtain the correlated value Z of the watermark contained in the image to be tested X*. Z is the correlated value of the watermark contained in the image to be tested X*, W is the value of the embedded watermark, and M is the quantity of the embedded watermark (step s 406 ). When the correlated value Z is larger than a critical value S z , whether the image to be tested X* contains a watermark is determined. The critical value S z can be expressed by
S z = α _ 3 M ∑ i = 1 M W i * ,
where {overscore (α)} is an average weighted value.
When the correlated value Z is not larger than the critical value S z , the image to be tested X* does not contain the watermark (step s 408 ).
In addition,
W * = ∑ k = 1 n W k * , W k * = F * ( u , v ) , ( u , v ) ε { ( 0 , 1 ) , ( 1 , 0 ) , ( 1 , 1 ) }
where F k *(u,v) is the embedded watermark data.
W = ∑ i = 1 3 n x i ,
where x i is the embedded watermark value, and M=3n. In addition, the extracting method does not require the storage of the original figure, so that it can be applied to detection of watermark.
FIG. 5 shows a graph of correlation versus peak signal to noise ratio (PSNR) for an embedding hardware structure used in an image compression system under different compression ratios according to one embodiment of the invention. As shown in FIG. 5 , when the percentage of compression quality is low, the correlation and PSNR are low. In contrast, the correlation and PSNR are high when the compression quality percentage is high.
Another embodiment of the invention provides a watermark embedding hardware structure that can be incorporated in a JPEG system. The combination of the watermark embedding hardware structure and the JEPG system is shown as FIG. 6 . The watermark embedding structure 602 is a watermark embedding hardware structure used in an image compression system. The watermark value is stored in an watermark ROM. The JPEG system 606 comprises a low frequency table apparatus (DC — table) 608 , a low frequency variable length coding apparatus (DC — VLC) 610 , a difference program coding module (DPCM) 612 , a quantization apparatus 614 , a quantization table apparatus 616 , a zigzag code sequence apparatus 618 , an execution length converter (RLC) 620 , a high frequency table apparatus (AC — table) 622 , and a high frequency variable length coding apparatus (AC — VLC) 624 . The operation of the system structure is described as follows.
Through a color image domain converter (RGB2YUV) 626 , an image is sampled by a sampling apparatus 628 . The sampled image is partitioned into 8×8 image blocks by an image partitioning apparatus. Each image block is processed with FDCT by a DCT module 632 . The transformed image can select the watermark data provided by the watermark embedding apparatus 602 via a multiplexor 634 . The output data of the multiplexor are then quantized and coded by the JPEG system 606 . Through the transformation control apparatus 636 and the header 638 , the JPEG file with watermark data is generated. Therefore, the invention incorporates a combination of the watermark embedding hardware structure into a JPEG system, which is applicable to an image compression system such as a digital camera and a scanner. Thereby, while an image is intercepted by the digital camera or the scanner, the image itself contains the watermark data, and the system performance is enhanced.
According to the above, the invention has the following advantages.
1. A hardware structure is used for embedding the watermark, so that the performance of the whole system is enhanced.
2. After image compression, the image itself contains watermark data.
3. The watermark hardware structure can be combined with the JPEG system.
Other embodiments of the invention will appear to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. It is intended that the specification and examples to be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims. | A watermark and extracting method and a watermark hardware structure used in an image compression system. A series of data is generated by random variables, such that duplication is avoided. According to characteristics of the human vision system, weighted value of each block is analyzed by classification in the frequency domain. According to the specific weighted value for each block, a watermark intensity is embedded, such that the embedded watermark is not easily observed, while the robustness is retained. Therefore, the original figure is not required for extraction. In addition, the watermark embedding hardware structure can be incorporated in a joint photographic experts group (JPEG) system, so that the image itself contains the watermark data while being intercepted. | 6 |
BACKGROUND OF THE INVENTION
The present invention relates to a method of and an arrangement for designing of tubular round knitted articles produced on a flat knitting machine.
Due to constantly increasing personal costs, a trend for producing knitted articles for which after the production of the knitting machine no additional fabrication works are needed has been observed. These knitted articles are usually tubular round final products which are produced with the use of the possibilities of modern electronically controlled, fully automatic flat knitting machines. The sleeve and body trunk parts of such a tubular round final article are first formed as separate tubular round knitted articles, before the sleeves must be connected to the body trunk part. Starting from this position, three individual tubular round knitted articles are knitted further as a single tubular round knitted article. Then shoulder shapes, neck portions and in some cases collars are knitted to them. The knitted article is therefore completely formed by the flat knitting machine. After this no seams must be closed any longer, and as a rule only the initial and the end thread portions are cleaned manually.
In the tubular round final articles which are formed of several parts, in order to produce very complex knitted articles correspondingly large numbers of knitting data for controlling the flat knitting machine must be provided. This no longer can be done manually. The European patent document EP 0 763 615 B1 discloses a device and a method for designing a round knitted article for a flat knitting machine, in which first a pattern for the knitted article is placed. Subsequently, a contour of the knitted article is selected by selection of contour shapes stored on the device and dimensional data for the front and rear parts as well as the sleeves are provided. After this manually for each individual contour region a knitting process description is produced, which depends on the pattern structures available in the corresponding contour region. Then, based on the knitting process description, the device automatically generates the control data for the flat knitting machine.
This known method makes possible a high automation degree during designing of tubular round final knitted articles. However, it has some disadvantages. The knitted articles can not have any arbitrary contours, but they can have only those contours which are contained in the selection stored in the device. Since the knitting process descriptions depend on the contour and the pattern in the corresponding contour region, it is necessary for each pattern structure occurring inside the contour to provide its own knitting process description, which is very expensive. Manual changes which are performed after the manufacture of the design are not transferred automatically to the original pattern representation, so that no visual control of the performed changes is possible. Furthermore, with the known method after the manufacture of the total design a close to reality representation of the knitting device can be visualized, but not the intermediate stages of designing, for example during the pattern association to a sleeve or the like.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide method of and device for designing tubular round knitted articles produced on a flat knitting machine, which avoid the disadvantages of the prior art.
More particularly, it is an object of the present invention to provide a method of and device for designing a tubular round knitted articles, which are user-friendlier than the known solutions and allow a higher automation degree.
In keeping with these objects and with others which will become apparent hereinafter, one feature of the present invention resides, briefly stated, in a method of designing of tubular round knitted articles on a flat knitting machine with at least one front part and at least one rear part, which comprises the following steps:
preparation of a knitting pattern for each front part and each rear part as well as in some cases further knitted parts such as pockets, independently from the shape of the knitted piece by means of an inputting and indicating device and storing the pattern data,
describing the contour of each front part and each rear part by means of the inputting and indicating device and storing the contour data,
fixing the contour portion of the knitted parts on which a connection with another knitted part must be produced, and storing the data of this contour portion,
assembling the contours of the knitted parts to a total knitted piece and determining a sequence of knitting rows, with which the total knitted piece is producible,
for each knitted part indicating the knitting pattern and the contour on the indicating device, by means of the inputting device displacing the contour onto the knitting pattern until the knitting pattern fills the contour in a desired manner,
indicating the total knitted piece with the selected and stored knitting pattern-and contour data for the individual knitted part,
determining the knitting information for each knitting row for providing the total knitting piece in accordance with the pattern and contour data of the knitting parts.
The knitting information for each knitting row can be converted into knitting data for a flat knitting machine and thereby one or several flat knitting machines can be controlled for producing the tubular round knitting article.
With the inventive method only a few steps can be performed manually. They are limited to the perforation of a knitting pattern for each knitted part, the fixing of the contours of the knitted part as well as the connection portion of the individual knitted parts, and the introduction of the knitting pattern into the contour of the corresponding knitted part. When these data are provided, then automatically the required sequence of knitting rows is generated for production of the total knitting piece as well as the knitting information for each individual knitting row. Correction possibilities both of the pattern and the contour are possible in each designing stage. During a correction of the pattern or the contour of the total knitted piece, moreover the made changes can be provided automatically in the stored pattern and the contour data of the corresponding individual knitted part. Also, after a correction, the individual representations of the knitted parts and the representation of the total knitted piece coincide with one another.
The knitted patterns can be designed preferably in the loop formation representation or in the thread running representation. From the data for one individual representation type the data for another representation type can be calculated, so that the knitted pattern in each design stage of the knitted article is indicatable in both representation types. Further advantages are provided when in the case of the loop formation representation a reality-close approximately three-dimensional representation of all elements of the knitted piece, such as loops, tucks and floating is provided.
A tubular round knitted article is composed of at least three knitting plates, one for the front part and one for the rear part. With pocket-and/or special patterning, further knitting planes can be produced. In accordance with a preferable variant of the inventive method, the individual knitted parts are associated with one or several planes of the total knitted piece. It is advantageous when also each knitting element, such as loops, tucks, floatings of one knitted part are associated with one of the knitting planes. Thereby for the user it is clear, in which plane the corresponding knitting elements are formed.
For facilitating the designing of the knitting pattern for the knitted parts, portions from a knitting pattern can be stored as individual modules, which at different locations of the pattern or during designing of the knitting patterns of another knitted parts can be again utilized. A significant facilitation of this modular technique is moreover also possible when the modules with the new use at other locations can be joined with a loop technique correctly in the surrounding knitting pattern, and if necessary, an adaptation of the knitting article plane association to the individual knitting elements of the module can be performed.
The fixing of the contour portions of the knitted parts, on which a connection with another knitted part might be produced, can be performed so that the starting and end points of the portion and the type of the connection are determined for example with or without performing a longitudinal compensation between the knitted parts and can be stored.
The invention also deals with an arrangement for designing tubular round knitted articles produced on a flat knitting machine with at least one front part and at least one rear part, that has at least one storage device for the designing data, at least one indicating device for representation of design formations of the knitted article and at least one inputting device for producing and changing the design former, wherein in accordance with the present invention it has at least one device for assembling the contours of the at least one front part and the at least one rear part in accordance with a manually inputtable connection steps and for calculating the knitted rows required for production of the contour of the total knitted piece, as well as for calculating the knitting information for each knitting row of the total knitted article in accordance with the pattern-and contour data of the individual knitted parts.
The arrangement also has a device for converting the knitting information of each knitting row into a knitting data for a flat knitting machine. In accordance with a preferable embodiment, the indicating device can be formed so that simultaneously loop formation and thread running representations of the knitted article or the knitted article parts are reproducible.
Further decisive advantages, in particular during correction of the knitted product production, are produced when the arrangement during change of one or the both representation types simultaneously changes the other representation.
For facilitating the knitting pattern production, the arrangement can be provided with devices for combining several knitting elements of a thread running-or loop formation representation to modules and storing devices for storing the modules. Furthermore, the devices for loop-technically correct insertion of modules in an available knitting pattern, for reducing and increasing, for multiplying and for inverting of modules can be provided.
The novel features which are considered as characteristic for the present invention are set forth in particular in the appended claims. The invention itself, however, both as to its construction and its method of operation, together with additional objects and advantages thereof, will be best understood from the following description of specific embodiments when read in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a principle view of an inventive designing arrangement together with a flat knitting machine and a tubular round final knitted article;
FIGS. 2 a and 2 b are views showing a partial view of a front side of a tubular round knitted article in stitch formation representation and a thread running representation correspondingly;
FIGS. 3 a - 3 c are views showing two stitch formation representations and a thread running representation of a portion of a rear part of a tubular round knitted article;
FIGS. 4 a and 4 b are views showing a joint representation of the front and the rear parts from FIGS. 2 and 3 in a loop formation representation and a thread running representation;
FIGS. 5 a and 5 b are views showing representation of the front part of FIG. 2 in a loop formation representation and a thread running representation, which clearly show the knitting production;
FIGS. 6 a and 6 b are views showing a thread running representation of a pattern and a knitting module inserted in the pattern;
FIGS. 7 a - 7 c are views showing a loop formation representation of a braid pattern of the front and rear part of a tubular round knitted article;
FIG. 8 is a view showing a representation of contours of different knitted parts of a tubular round knitted article;
FIG. 9 is a principle view of the definition of connecting points of two knitted parts;
FIG. 10 is a view showing a representation of a knitting row sequence on an example of a sleeve and a body trunk part with a V-section on the front part;
FIG. 11 is a principle view showing the introduction of a pattern of a knitting pattern in different knitted parts;
FIGS. 12 a - 12 c are views showing different representations of a total knitted article composed of individual knitted parts.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a designing arrangement for producing a tubular round final knitted article 9 by means of a flat knitting machine 8 . The designing arrangement has a computing and storage device 1 , a keyboard 2 as a first inputting device, a graphic tablet 4 as a second inputting device, and an image screen 3 as an indicating device. A printer 5 and an external mass storage 6 are connected to the computing and storage device 1 .
FIGS. 2-7 show various pattern representation-and design possibilities of an inventive method and an inventive arrangement.
FIG. 2 a shows a loop formation representation of a section of the outer view of a front side of a right smooth tubular round knitted article. The loops 10 of the front part are right loops, and in FIG. 2 a are shown as in the final knitted article. FIG. 2 b shows the thread running representation corresponding to FIG. 2 a wherein the loops 10 here are formed on the front needle bed V.
FIG. 3 a shows the inner view of the rear part of a right smooth tubular round final knitted article. The loops 11 are left loops and formed, as in the thread running representation in FIG. 3 b , on the rear needle bed H. FIG. 3 shows the outer view of the rear part of the tubular round knitted article. Here the loops 11 are shown as right loops.
FIG. 4 a shows in the general view the front-end rear part from FIGS. 2 a and 3 a as a loop formation representation in a combined view. The right loops 10 of the front part belong to the first plane 100 of the total knitted product and the loops 11 to the second plane 200 . In this example a right smooth tubular round knitted article has only two knitting planes, the first knitting plane 100 for the front part and the second knitting plane 200 for the rear part. FIG. 2 b shows the thread running representation corresponding to FIG. 4 a . The loops 10 are formed on the front needle V and the loops 11 of the rear part are formed on the rear needle bed H.
FIG. 5 a shows a further type of the representation of the front part of FIG. 2 a in the loop formation representation, wherein the loops 10 are shown as they actually are suspended in the needles of the front needle bed. FIG. 5 b illustrates that the loops 10 are knitted only with each second needle of the front needle bed V. It can be seen that the loops 10 in FIG. 5 a are pulled further from one another than the loops 10 in the representation of FIG. 2 a , which is a reality-closed representation of the front part and does not consider the knitting-technical production of the knitted article.
FIGS. 6 a and 6 b illustrate the binding of a knitting module 25 in a knitting pattern 26 . The knitting pattern 26 in the rows 101 - 104 contains knitting instructions for the first plane of the knitted product and in the rows 201 - 205 contains data for the second plane of the knitted article. The module 25 contains knitting informations 101 ′- 104 ′ for a single knitting plane. FIG. 6 b illustrates how with insertion of the module 25 into the knitting pattern 26 automatically an adaptation of the module 25 in the both different knitting planes 100 and 200 is performed. Since the module 25 contains only data for the first plane of the knitted article, the rows of the second plane 201 - 205 remain unchanged. For the rows 101 - 104 , the module 25 contains data that in each its row left loops must be formed.
For enabling formation of mainly left loops in the row 101 , automatically the row 101 ′ generated, in which the fifth loop from left is transferred to the rear needle bed H. Also automatically a row 101 ″ is produced, in which the left loops are transferred back from the rear needle bed to the front needle bed. In an identical way, for the row 102 a row 102 ′ is generated. Also, the row 102 ″/ 102 ′ is automatically produced. Here the left loops are transferred back from the rear needle bed to the front needle bed, and the fourth loop is transferred from left to the rear needle bed, so that it can form a left loop in the rows 103 and 104 . In a similarly automatically produced row 104 ″ then the fourth loop is transferred back from left to the front needle bed V.
FIG. 7 a shows a 2×2 braid in the representation for a first knitting plane. The loop train 15 , 16 which raises to the right upwardly forms the intersecting visual side, and the loop train 17 raising to the left upwardly is covered. The illustrated knitting plane can be for example the outer front plane. FIG. 7 b shows the braid of FIG. 7 a in a representation for the second knitting plane of a tubular round knitted product, as seen from the front side of the knitted product. The second plane can be for example the inner side of the rear part. The braid train 15 ′, 16 ′ is now covered and raises to the left, and the loop train 17 ′, 18 ′ raises to the right and is not visible. In FIG. 7 c the knitted product is shown from the rear side. FIG. 7 c shows also the braid which is seen from the outer side of the rear part. The loop trains 15 ″, 16 ″ and 17 ″, 18 ″ are mirror inverted with respect to the orientation in FIG. 7 a.
FIG. 8 shows the contours of a front part 24 , a rear part 23 , as well as two sleeves 21 , 22 . The parts 21 - 24 can be selected completely arbitrarily by a designer.
FIG. 9 shows an example for fixing of contour portions on which a body trunk part 30 and a sleeve 31 must be connected with one another. This is performed by fixing the initial and end points 32 , 33 , 34 on the body trunk part 30 and corresponding initial and end points of the connecting portions 32 ′, 33 ′ and 34 ′ on the sleeve 31 . In the region between the points 32 / 32 ′ and 33 / 33 ′, the sleeve is suspended on the body trunk part and simultaneously production knitting rows for the sleeve are produced. Between the points 33 / 33 ′ and 34 / 34 ′ the sleeves are suspended only on the body trunk part and no loop rows for the sleeve 31 are produced any longer.
FIG. 10 shows example as an on the front part 30 and the sleeve 31 of FIG. 9, the sequence of criteria, in accordance with which a knitting row sequence is provided. 40 identifies the starting knitting row both of the body trunk part 30 and the sleeve 31 . At the knitting row 41 , the separate production of the body trunk part 30 and the sleeve 31 starts, and simultaneously the binding of the sleeve 31 to the body trunk part 30 starts. Both parts as well as the other not shown sleeves are further knitted from this position as a single tubular round knitted product. At the position 42 an interruption of the tubular knitted product is performed at the front part for the production of a V portion. On the position 43 the sleeve 31 comes to end in correspondence with a contour description. The position 44 identifies the last production knitting row of the sleeve 31 in correspondence with the knitting process. The row 45 is the last body trunk row, in which the sleeve 31 is bound to the body trunk part 30 . In the knitting row 46 an interruption of the tubular knitted product on the rear side of the body trunk part 30 is performed for producing a neck back section. Reference numeral 47 identifies the last produced knitting row.
In accordance with the sequence of knitting rows shown in FIG. 10, in the inventive method the introduction of the knitting pattern is performed, which were before generated for the knitting parts, in the contours of the sleeves 31 , 32 as well as the body trunk part 30 . The contours 30 - 32 are displaced on the pattern field 50 so long until the individual pattern elements 51 and 52 are arranged on the right position in the corresponding knitting part 30 - 32 as shown in FIG. 11 .
Subsequently the total knitted piece can be indicated in different representation types as shown in FIG. 12 . FIG. 12 a shows the standard representation of a total knitted piece 60 , wherein the knitting rows for the sleeves 62 and 63 are identified starting from the sleeve connection with the body trunk part 31 , 61 . When on a knitted part no loops are formed, while on the other knitted parts loops are formed, then in the corresponding knitted part a knitted row is identified with a definite color 65 which forms the background of the knitted article. In the shown example the non-formation of loops is identified with a white color. FIG. 12 b shows a variant of the illustration of FIG. 12 a , wherein the knitting rows for the sleeves 62 and 63 are released from the body trunk and indicated in a vertical direction parallel to the body trunk part 61 . FIG. 12 c corresponds to FIG. 12 b wherein however with the sleeves 62 and 63 the illustration of individual knitting rows in which no loops are formed for the sleeves 62 and 63 is dispensed with. It is to be understood that from the total knitted piece also a reality-close loop formation representation can be indicated, to test the design results based on purely optical criteria.
It will be understood that each of the elements described above, or two or more together, may also find a useful application in other types of methods and constructions differing from the types described above.
While the invention has been illustrated and described as embodied in method of and device for designing of tubular round knitted articles produced on a flat knitting machine, it is not intended to be limited to the details shown, since various modifications and structural changes may be made without departing in any way from the spirit of the present invention.
Without further analysis, the foregoing will so fully reveal the gist of the present invention that others can, by applying current knowledge, readily adapt it for various applications without omitting features that, from the standpoint of prior art, fairly constitute essential characteristics of the generic or specific aspects of this invention. | A method of and an arrangement for designing tubular round knitted products on a flat knitting machine operates with the fine automation degree and a plurality of representing, designing and correcting possibilities. | 3 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a division of U.S. application Ser. No. 14/418,034 filed on 28 Jan. 2015, which is a U.S. Nationalization of PCT International Application No. PCT/IL2013/050670 filed on 7 Aug. 2013, which claims priority to U.S. Provisional Application No. 61/680,322 filed on 7 Aug. 2012 and U.S. Provisional Application No. 61/736,015 filed on 12 Dec. 2012. The disclosure of each of the foregoing applications is incorporated herein, in its entirety, by this reference.
FIELD OF INVENTION
[0002] The present invention relates to a novel method for preparing amorphous calcium carbonate (ACC), based on stepwise addition of a stabilizing solution and an organic solvent. The ACC produced by the process of the present invention is characterized by increased stability both in solution/suspension and as a dry powder, and may be used, e.g., in the paper, dyes, plastics, inks, adhesives, marble restoration, medical device and pharmaceutical industries.
BACKGROUND OF THE INVENTION
[0003] Calcium carbonate (CaCO 3 ) is a calcium salt of carbonic acid, which is widely used in many industries today. It is mostly known as a calcium supplement, taken to increase daily calcium intake. Calcium carbonate has six known polymorphs, three of which are anhydrous crystalline, namely, calcite, aragonite and vaterite; two are crystalline hydrates, namely, monohydrocalcite and ikaite; and one is hydrated amorphous, namely amorphous calcium carbonate (ACC). ACC is a transient polymorph that precipitates out of a super-saturated solution following Ostwald's step rule. If not stabilized by any means, ACC will rapidly and completely crystallize into one of the five more stable polymorphs within seconds. The amorphous polymorph is characterized by distinctive 40-120 nm spherules, having no major XRD peaks but a broad low intensity peak between 20-30 2θ, and having a broad low intensity peak around 1082 cm −1 in Raman spectroscopy, in contrast to the 1-10 μm crystals typical of the other polymorphs, also having distinct major XRD peaks and significantly distinguishable Raman peaks.
[0004] Synthetic ACC is known for over 100 years, and today there are many methods for synthesizing ACC using various molecules for stabilizing the transient unstable amorphous phase. The three widely used methods all use supersaturated solution of calcium ions from either a soluble source such as calcium chloride or from dissolving a calcium insoluble salt such as calcium hydroxide using a hydrogen binding molecule, such as sucrose. This supersaturated solution of calcium ions is then reacted with a source of carbonate from either carbon dioxide gas, an alkaline metal salt of carbonate, such as sodium carbonate, from an organic salt of carbonate, from ammonium carbonate, or from the hydrolysis of dialkyl carbonate, such as dimethyl carbonate with hydroxide ions (see, for example, U.S. Pat. No. 4,237,147).
[0005] Since ACC is unstable in aqueous solution for more than two minutes, commercial production is impractical. Large scale production that includes hundreds or even thousands of liters being mixed and separated using liquid-solid phase separation techniques, such as filtration or centrifugation, in less than two minutes, is not applicable today. If the stability time in solution can be prolonged to several hours, therefore allowing for standard liquid-solid phase separation techniques, such as filtration or centrifugation to be used, commercial production can then become practical.
[0006] With the exception of Hyun et al. [ Materials Chemistry and Physics, 93 (2005) 376-382], that described a method to stabilize ACC in ethanolic medium for more than 24 hours, none of the above previous reports mention the period of time in which the ACC remains stable in solution. However, Hyun et al. can only produce stable ACC in the presence of toxic ammonia, which, as described by Hyun, is crucial to the stability. Also, the calcium carbonate concentrations used in the publication are relatively low, making them impractical for industrial use.
[0007] When attempting to reproduce other published procedures, the applicants of the present invention produced ACC that is only stable in solution for several minutes and crystallizes thereafter. In some cases, even though ACC was produced, it was impossible to isolate it from the solution. For instance, producing ACC using the procedure described in U.S. Pat. No. 4,237,147 at Example 2 yielded only a slurry that was impossible to filter and from which ACC could not be isolated. Also, should a powder be obtained from this slurry using spray drying, as suggested in this patent, it will only contain ˜2/15 of ACC, with the remaining 13/15 parts being sucrose.
[0008] In general, any attempts to duplicate the procedures described in U.S. Pat. No. 4,237,147 using calcium chloride, or some other soluble calcium salt did not yield ACC or any form of precipitated calcium carbonate.
[0009] It is well known that ACC will crystallize in the presence of water, however, to the applicant's best knowledge, there are no previous publications describing the production of ACC which remains stable in aqueous solution or suspension for extensive periods of time using only up to 10% by weight of stabilizers. Also, the carbonation step in all these methods is the last step of the synthesis, always followed by the liquid solid separation step.
[0010] There is an unmet need in the art for novel methods for producing ACC with increased stability, either as a suspension in aqueous phase, or as a dry powder, which can be adapted to production of ACC on commercial production scale.
SUMMARY OF THE INVENTION
[0011] The present invention relates to a manufacturing method for producing amorphous calcium carbonate (ACC) that exhibits specific XRD and Raman spectra typical of the amorphous form. The novel method of the invention utilizes hydrogen bonding molecules as stabilizers and an organic solvent, and results in ACC having increased stability when suspended in aqueous phase and in solid state as a dry powder. The method of the invention generally involves combining a solution comprising a soluble calcium salt and a first stabilizer with a solution comprising a soluble carbonate (e.g., a soluble alkali carbonate) to form an ACC suspension, and adding a water miscible organic solvent and a second stabilizer so as to form a stabilized ACC suspension from which stable ACC may be isolated. In some embodiments, the first and stable stabilizers may be the same or different.
[0012] Thus, in one embodiment, the present invention provides a method of preparing amorphous calcium carbonate (ACC), comprising the steps of combining a solution comprising a soluble calcium salt and a first stabilizer with a solution comprising a soluble carbonate so as to form an ACC suspension; and adding a water miscible organic solvent and a solution comprising a second stabilizer, simultaneously or sequentially in any order so long as the second stabilizer and organic solvent contact the ACC suspension within about 2 minutes of its formation, thereby obtaining a stabilized suspension of ACC, wherein the total amount of stabilizer constitutes up to about 12 wt % of the stabilized ACC suspension, and the water miscible organic solvent constitutes at least about 5 wt % of the stabilized ACC suspension. The first stabilizer and the second stabilizer may be the same or different, with each possibility representing a separate embodiment of the present invention.
[0013] In another embodiment, the present invention provides a method of preparing ACC, comprising the steps of i) preparing an aqueous solution comprising a soluble calcium salt and a first stabilizer; ii) preparing an aqueous solution comprising a soluble carbonate; iii) preparing an aqueous solution comprising a second stabilizer; iv) preparing a solution comprising a water miscible organic solvent; and v) combining the solution prepared in step ii) with the solution prepared in step i) so as to form an ACC suspension, followed by adding the solutions prepared in steps iii) and iv), simultaneously or sequentially in any order so long as these solutions contact the ACC suspension within about 2 minutes of its formation, thereby obtaining the stabilized suspension of ACC, wherein the total amount of stabilizer constitutes up to about 12 wt % of the stabilized ACC suspension, and the water miscible organic solvent constitutes at least about 5 wt % of the stabilized ACC suspension. The first stabilizer and the second stabilizer are the same or different, with each possibility representing a separate embodiment of the present invention.
[0014] In another embodiment, the present invention provides a method of preparing ACC, comprising the steps of i) preparing an aqueous solution comprising a soluble calcium salt and a first stabilizer; ii) preparing an aqueous solution comprising a soluble carbonate; iii) preparing a solution of a second stabilizer in a water miscible organic solvent; and iv) combining the solution prepared in step i) and ii) so as to obtain an ACC suspension, followed by adding the solution prepared in step iii) to the ACC suspension within about 2 minutes of its formation, so as to form a stabilized ACC suspension, wherein the total amount of stabilizer constitutes up to about 12 wt % of the stabilized ACC suspension, and the water miscible organic solvent constitutes at least about 5 wt % of the stabilized ACC suspension. The first stabilizer and the second stabilizer are the same or different, with each possibility representing a separate embodiment of the present invention.
[0015] In a currently preferred embodiment, the present invention provides a method for preparing stabilized ACC, comprising the steps of: i) preparing an aqueous solution comprising a soluble calcium salt and a first stabilizer; ii) preparing an aqueous solution comprising a soluble carbonate and combining it with the calcium salt of step i), thereby obtaining a suspension of ACC; iii) preparing an aqueous solution of a second stabilizer, thereby obtaining a stabilizing solution; iv) combining the stabilizing solution with the suspension of ACC; and v) adding a water-miscible organic solvent, wherein the stabilizing solution and the organic solvent are added to the suspension of ACC within about 2 minutes of its formation, so as to form a stabilized ACC suspension, wherein the total amount of stabilizer constitutes up to about 12 wt % of the stabilized ACC suspension, and the water miscible organic solvent constitutes at least about 5 wt % of the stabilized ACC suspension. The first stabilizer and the second stabilizer are the same or different, with each possibility representing a separate embodiment of the present invention.
[0016] In some embodiments, the method according to the invention may further comprise a step of separating the ACC from the suspension of stabilized ACC. The method may further comprise the step of drying the separated ACC, thereby obtaining a powder of stable ACC. The separating may comprise filtering or centrifugation, and the step of drying may comprise heating in vacuum or freeze-drying, with each possibility representing a separate embodiment of the present invention. Thus, in some embodiments, the method of the present invention provides a powder of stable ACC comprising less than about 15 wt % water preferably less than 8%, for example between about 1 and about 7 wt %, and calcium usually being between about 30 and about 33 wt %. Each possibility represents a separate embodiment of the present invention.
[0017] It is understood that, for each of the aforementioned embodiments, each of the terms “first stabilizer” and “second stabilizer” encompass a single stabilizing compound or a combination of more than one stabilizing compounds. Thus, in some embodiments, the aqueous calcium solution can contain one stabilizing compound or a combination of two or more stabilizing compounds (collectively referred to as “the first stabilizer”). In other embodiments, the solution comprising a second stabilizer can contain one stabilizing compound or a combination of two or more stabilizing compounds (collectively referred to as “the second stabilizer”). Regardless of the number of stabilizers used, the total amount of stabilizer constitutes up to about 12 wt % of the stabilized ACC suspension. In a currently preferred embodiment, the calcium salt is calcium chloride or nitrate. In other preferred embodiments, the soluble carbonate is an alkali carbonate (e.g., lithium, sodium or potassium carbonate), or an ammonium carbonate. Each possibility represents a separate embodiment of the present invention. In some embodiments, the calcium salt and the carbonate are present in a molar ratio of from about 0.5 to about 2.0.
[0018] In another embodiment, the water miscible organic solvent is preferably selected from lower alcohols and ketones (e.g., methanol, ethanol, propanol, isopropyl alcohol, acetone, diethyl ketone and cyclohexanone). A currently preferred water miscible organic solvent is ethanol. Each possibility represents a separate embodiment of the present invention.
[0019] In another embodiment, the soluble calcium salt solution comprises about from 4 mM to about 2 M soluble calcium salt, and the carbonate solution comprises from about 4 mM to about 2 M carbonate. Each possibility represents a separate embodiment of the present invention.
[0020] The first and secondary stabilizers used in the method of the present invention can be the same or not. In some embodiments, the first and second stabilizer are each independently selected from the group consisting of organic acids, phosphorylated organic acids, phosphoric esters of hydroxy carboxylic acids, sulfuric esters of hydroxyl carboxylic acids, phosphorylated amino acids and derivatives thereof, amino acid sulfate esters, and hydroxy bearing organic compounds combined with a base such as alkali hydroxides. The hydroxy bearing compounds, combined with the hydroxide, preferably also bear other functions like carboxyl, etc. but with the hydroxyl not being esterified. The organic acids may comprise, for example, ascorbic acid or acetic acid, and preferably they include carboxylic acids having at least two carboxylic groups and molecular weight not larger than 250 g/mol, such as citric acid, tartaric acid, malic acid, etc. The esters may include, for example, phosphoenolpyruvate. In another embodiment, the phosphoric or sulfuric esters of hydroxyl carboxylic acids comprise amino acids, examples of which include phosphoserine, phosphothreonine, sulfoserine, and sulfothreonine. In another embodiment, the stabilizing molecule is a phosphate ester derivative of an amino acid, such as phosphocreatine. The hydroxyl bearing compounds combined with hydroxide may comprise, for example, mono-, di- tri-, oligo-, and polysaccharides like sucrose or other polyols like glycerol. The hydroxyl bearing compounds may further comprise hydroxy acids like citric acid, tartaric acid, malic acid, etc., or hydroxyl-bearing amino acids such as serine or threonine. Each possibility represents a separate embodiment of the present invention.
[0021] In some embodiments, at least one of the first and second stabilizer is a polyol combined with an alkali metal hydroxide, or the stabilizer is a phosphorylated amino acid, wherein the total amount of polyols or phosphorylated amino acids in the suspension of stabilized ACC is from about 1 to about 1000 mM, for example from about 10 to about 100 mM. The polyols preferably comprise saccharides. In a preferred embodiment, the stabilizer is a phosphorylated amino acid, wherein its total concentration in the suspension of stabilized ACC is from about 2 to about 200 mM, for example from up to about 20 mM. In another preferred embodiment, the stabilizer is a dicarboxylic acid or a tricarboxylic acid (e.g., citric acid), wherein its total concentration in the suspension of stabilized ACC is from about 2 to about 200 mM, for example from up to about 20 mM. In another preferred embodiment, the stabilizer is a non-phosphorylated amino acid bearing a hydroxyl group (e.g., serine or threonine), in combination with an alkali metal hydroxide, wherein the total concentration of amino acid in the suspension of stabilized ACC is from about 2 to about 200 mM, for example from up to about 20 mM, and the hydroxide total concentration in the suspension of stabilized ACC is between about 1 mM and about 2000 mM, for example about 0.1 M. In another preferred embodiment, the stabilizer is a polyol combined with an alkali metal hydroxide, wherein the polyol total concentration in the suspension of stabilized ACC is from about 10 to about 1000 mM, for example up to about 100 mM and the hydroxide total concentration in the suspension of stabilized ACC is between about 1 mM and about 2000 mM, for example about 0.1 M. Each possibility represents a separate embodiment of the present invention.
[0022] In one embodiment of the present invention, the first and second stabilizers are different stabilizers. In a preferred embodiment of the invention, however, the first stabilizer and the second stabilizer are the same, and the stabilizer amounts used are in a ratio of from about 1:1 to about 10:1 (first stabilizer to second stabilizer), preferably a ratio of about 1:2 of first stabilizer to second stabilizer. Each possibility represents a separate embodiment of the present invention.
[0023] The step of combining the ACC suspension with the second stabilizer solution and the organic solvent is preferably performed at a temperature between about −10° C. and about 60° C., preferably between about −3° C. and ambient temperature (room temperature), and more preferably between about 0° C. and about 15° C. Each possibility represents a separate embodiment of the present invention.
[0024] In a currently preferred embodiment, the invention provides a method for preparing amorphous calcium carbonate (ACC) comprising the steps of i) preparing an aqueous solution of calcium chloride in a concentration of up to about 1 M and a stabilizer in an amount of between about 1 and 150 mmol, for example from about 4 to about 80 mmol per 1 mol of calcium chloride; ii) preparing an aqueous solution of sodium carbonate in the same molar concentration as calcium chloride in step i), and combining it with the calcium salt solution of step i), thereby obtaining a suspension of ACC; iii) preparing a stabilizing solution comprising about 350 g ethanol per one mol of calcium chloride in step i), and the same stabilizer as in step i) but in double amount; and iv) combining the stabilizing solution with the suspension of calcium carbonate, thereby obtaining stabilized suspension of ACC. In one embodiment, the stabilizer in steps i) and iii) is phosphoserine in amounts of from about 3 to about 9 mmol, and from about 8 to 16 mmol per one mol of calcium, for example about 6 mmol and about 12 mmol respectively, or about 4 mmol and about 8 mmol per one mol of calcium, respectively. In some embodiments, the method further comprises the step of filtering the stabilized suspension of ACC and optionally further drying in a vacuum at a temperature of between 40° C. and about 50° C. In another embodiment the stabilizer is sucrose with sodium hydroxide in amounts of about 20-100 mmol sucrose and about 50-200 mmol NaOH per 1 mol calcium, for example about 25-70 mmol sucrose and about 100 mmol NaOH, such as about 25 mmol sucrose and about 100 mmol NaOH per 1 mol calcium in step i), and about 40-200 mmol sucrose and about 100-400 mmol NaOH per 1 mol calcium, for example about 50-200 mmol sucrose and about 200 mmol NaOH, such as about 140 mmol sucrose and about 200 mmol NaOH per 1 mol calcium in step iii). In some embodiments, the method further comprises the step of centrifuging and freeze-drying the sediment. Each possibility represents a separate embodiment of the present invention.
[0025] In one currently preferred embodiment, the method according to the invention comprises combining in an aqueous mixture calcium chloride, an alkali carbonate, phosphorylated organic acid, and alcohol, thereby obtaining a suspension of stabilized ACC containing between about 2.5 and 5 wt % ACC, between about 0.001 and about 0.3 wt % e.g., between about 0.05 and about 0.2 wt % phosphorylated organic acid, and between about 8 and about 32 wt %, e.g., between about 10 and about 15 wt % ethanol.
[0026] Another preferred method according to the invention comprises combining in an aqueous mixture calcium chloride, an alkali carbonate, saccharide with sodium hydroxide, and alcohol, thereby obtaining a suspension of stabilized ACC containing between about 2.5 and about 5 wt % ACC, between about 1 and about 4 wt % saccharide, about 0.5 wt % hydroxide, and between about 10 and about 15 wt % ethanol.
[0027] Another preferred method according to the invention comprises combining in aqueous mixture calcium chloride, an alkali carbonate, a dicarboxylic acid, a tricarboxylic acid (e.g., citric acid), and alcohol, thereby obtaining a suspension of stabilized ACC containing between about 2.5 and about 5 wt % ACC, between about 0.001 and about 0.2 wt % dicarboxylic or tricarboxylic acid, and between about 8 and about 32 wt % ethanol. Another preferred method according to the invention comprises combining in aqueous mixture calcium chloride, an alkali carbonate, a dicarboxylic or tricarboxylic acid, a phosphorylated organic acid, and alcohol, thereby obtaining a suspension of stabilized ACC containing between about 2.5 and about 5 wt % ACC, between about 0.001 and about 0.2 wt % in total of dicarboxylic or tricarboxylic acid and phosphorylated organic acid, and between about 8 and about 32 wt % ethanol.
[0028] Another preferred method according to the invention comprises combining in aqueous mixture calcium chloride, an alkali carbonate, a non-phosphorylated hydroxyl-bearing amino acid (e.g., serine) with sodium hydroxide, and alcohol, thereby obtaining a suspension of stabilized ACC containing between about 2.5 and about 5 wt % ACC, between about 1 and about 4 wt % non-phosphorylated hydroxyl-bearing amino acid, about 0.5 wt % hydroxide, and between about 10 and about 15 wt % ethanol.
[0029] Another preferred method according to the invention comprises combining in aqueous mixture calcium chloride, sodium carbonate, a non-phosphorylated hydroxyl-bearing amino acid (e.g., serine), a saccharide and sodium hydroxide, and alcohol, thereby obtaining a suspension of stabilized ACC containing between about 2.5 and about 5 wt % ACC, between about 1 and about 4 wt % in total of non-phosphorylated hydroxyl-bearing amino acid and saccharide, about 0.5 wt % hydroxide, and between about 10 and about 15 wt % ethanol.
[0030] In another embodiment, the method of the invention further comprises separating ACC from the suspension and drying, thereby obtaining a powder of stable ACC comprising between about 75 and about 88 wt % CaCO 3 and less than about 10 wt % water.
[0031] In further embodiments, the present invention provides a stable ACC suspension and a stable ACC powder which result from the process as described herein. Thus, in one embodiment, the present invention provides a suspension of stabilized ACC produced by the process of the present invention. In one embodiment, the suspension of stabilized ACC contains between about 2.5 and about 5 wt % ACC, between about 0.05 and about 0.2 wt % phosphorylated organic acid, and between about 10 and about 15 wt % ethanol. In another embodiment, the suspension of stabilized ACC contains between about 2.5 and about 5 wt % ACC, between about 1 and about 4 wt % saccharide, about 0.5 wt % hydroxide, and between about 10 and about 15 wt % ethanol. In another embodiment, the suspension of stabilized ACC contains between about 2.5 and about 5 wt % ACC, between about 0.05 and about 0.2 wt % organic acid (e.g., a dicarboxylic acid or a tricarboxylic acid such as citric acid), and between about 10 and about 15 wt % ethanol. In another embodiment, the suspension of stabilized ACC contains between about 2.5 and about 5 wt % ACC, between about 0.05 and about 0.2 wt % organic acid (e.g., a non-phosphorylated hydroxyl-bearing amino acid), about 0.5 wt % hydroxide, and between about 10 and about 15 wt % ethanol. Suspensions comprising combinations of stabilizers are also contemplated. Each possibility represents a separate embodiment of the present invention.
[0032] In other embodiments, the present invention provides a powder of stable ACC produced by the process of the present invention. In one embodiment, the powder comprises between about 75 and about 88 wt % CaCO 3 , less than about 10 wt % water, and an organic acid (e.g., a phosphorylated organic acid, a non-phosphorylated organic acid, a dicarboxylic or tricarboxylic acid, an amino acid bearing a hydroxyl group, or any other organic acid described herein). In other embodiment, the powder of stable ACC comprises between about 75 and about 88 wt % CaCO 3 , less than about 10 wt % water, and between about 1 and about 5 wt % saccharide. Each possibility represents a separate embodiment of the present invention.
[0033] In other aspects, the present invention is further directed to the use of the above suspensions and powders in dyes, paper products, plastics, inks, adhesives, marble restoration products, medical devices, pharmaceuticals, food supplements, and/or food additives, with each possibility representing a separate embodiment of the present invention.
[0034] In some preferred embodiments, stabilized ACC was produced by mixing a supersaturated solution of calcium ions from a soluble calcium salt, such as calcium chloride, also containing a first stabilizing molecule, such as phosphoserine, with a super saturated solution of carbonate from a soluble carbonate salt, such as sodium carbonate. Without further stabilization the precipitated ACC rapidly crystallizes in solution in less than about 2 minutes to a mixture of calcite and vaterite. However, in the process of the invention, after allowing the precipitated ACC suspension in step 1 to mix for ˜10 seconds, the stabilizing solution containing the second stabilizing molecule, such as phosphoserine, is added. After allowing the precipitated ACC suspension and the stabilizing solution in step 2 to mix for ˜10 seconds, the organic solvent, such as ethanol, is added. After adding the organic solvent the ACC is stabilized and can be maintained in suspension for days, depending on the concentration of the first and second stabilizers as well as the ratio of the organic solvent. It was further found that reducing the reaction temperature can improve the stability time in solution. The order of addition of the secondary stabilizer and the alcohol may be reversed, or they may be added together in one solution comprising the secondary stabilizer in the alcohol.
[0035] The procedure can be performed in batches, where the solutions are added to each other in single additions, or as a continuous process, where the solutions are mixed, for example, in a continuous flow, using continuous flow technology apparatus.
[0036] Further embodiments and the full scope of applicability of the present invention will become apparent from the detailed description given hereinafter. However, it should be understood that the detailed description and specific examples, while indicating preferred embodiments of the invention, are given by way of illustration only, since various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0037] FIG. 1 : Raman spectra of several samples of calcium carbonate taken using a micro-Raman. The spectra are of the following samples A) ACC produced by the process of the present invention; B) ACC after crystallization; C) vaterite; and D) calcite. Vertical lines represent the Raman shift of the vaterite major peaks of the CO 2 vibration.
[0038] FIG. 2 : XRD spectrum of ACC produced by the process of the present invention. The ACC XRD spectrum is characterized by a broad, low intensity peak from ˜20-30 2θ.
[0039] FIG. 3 : XRD spectrum of vaterite. The vaterite XRD spectrum is characterized by three major peaks at 24, 27 and ˜33 θ.
[0040] FIG. 4 : XRD spectrum of calcite. The calcite XRD spectrum is characterized by multiple peaks with the most dominant one at ˜29 θ.
DETAILED DESCRIPTION OF THE INVENTION
[0041] The present invention provides the synthesis procedure for producing highly stable ACC using hydrogen bonding molecules as stabilizers and a water miscible organic solvent in a stepwise process. The stepwise procedure of the present invention was found to be far superior in terms of safety, yield and stability over previously described methods for producing stable ACC. It was found that performing this procedure in separate steps according to the embodiments described here is beneficial in order to produce highly stable ACC.
[0042] The surprising stability of the ACC prepared according to the process of invention is not fully understood. Without wishing to be bound by any particular mechanism or theory, it is contemplated that the addition of stabilizing molecules after ACC is produced allows for some external coating that increases the stability of the ACC, and the addition of an organic solvent both reduces the activity of the water and lowers the solubility of the stabilizing molecules in solution, ensuring they remain on the surface or inside the ACC particles thus promoting stabilization of the ACC. Loste et al. [ Journal of Crystal Growth, 254 (2003) 206-218], suggested that Mg increases ACC stability by incorporating into the amorphous lattice, and because the Mg radius is smaller than that of Ca it has stronger binding to the water molecules present inside the ACC structure, thus inhibiting crystallization. It is possible that the water binding molecules act through the same mechanism. By binding to both calcium ions and to water molecules they may act to inhibit water diffusion out of the amorphous lattice, thus inhibiting crystallization.
[0043] It was also found that when certain organic acids or phosphorylated amino acids were used there was no need to increase the solution pH with sodium hydroxide or another base. However, when sucrose or other sugars as well as non-phosphorylated, hydroxyl-bearing amino acids were used, the solution pH had to be raised using, e.g., alkali hydroxides such as sodium hydroxide, potassium hydroxide and the like, in order to obtain a stabilizing effect. Koga et al. [ Thermochimica Acta, 318 (1998) 239-244] previously suggested that high pH promotes ACC stabilization, however, Koga only used sodium hydroxide in his experiments which only allowed him to increase the pH to 13.5 before calcium hydroxide precipitated out of solution. When sucrose was introduced together with sodium hydroxide, it enabled to further increase the pH to >14 without precipitating calcium hydroxide. Without wishing to be bound by any particular mechanism or theory, it seems that this combination of sucrose with very high pH has an improved stabilizing effect.
[0044] U.S. Pat. No. 4,237,147 describes a method to produce ACC using calcium hydroxide and sucrose; however, the sucrose is being used in order to increase the solubility of the calcium hydroxide, which requires very large amount of sucrose relative the amounts described in the present invention. The high sucrose amounts described by U.S. Pat. No. 4,237,147 make the production of ACC impractical for two reasons: 1. The sucrose content is so high that the ACC is only partially precipitated making it almost impossible to isolate. 2. The high sucrose content is so high that it forms a viscous gel which is impossible to filter. In the present invention, because the sucrose is used sparingly as a stabilizer and not as a dissolving agent, far lower concentrations are required, which easily solves the two problems described above.
[0045] As used herein, the term “soluble calcium salt” means a calcium salt that is soluble in water, i.e., the calcium salt is capable of fully dissolving in water to obtain a clear solution. Generally speaking, a compound is deemed “soluble” in water if it dissolves to the extent of at least about 1 g/100 mL of water, such as for example at least about 5 g/100 mL, or at least about 10 g/100 mL, at a temperature of about 0° C. to about ambient temperature, which is defined herein as about 20° C. to 30° C. In a currently preferred embodiment, the soluble calcium salt is calcium chloride. In other embodiments, the soluble calcium salt may be calcium bromide, calcium iodide, calcium lactate, calcium gluconate, and the like. Each possibility represents a separate embodiment of the present invention.
[0046] As used herein, the term “soluble carbonate” means a carbonate (CO 3 2− ) that is soluble in water, i.e., the carbonate is capable of fully dissolving in water to obtain a clear solution. In a currently preferred embodiment, the soluble carbonate is an alkali carbonate such as lithium carbonate, sodium carbonate or potassium carbonate. In another preferred embodiment, the soluble carbonate is ammonium carbonate. Each possibility represents a separate embodiment of the present invention.
[0047] As used herein, the term “stabilized ACC suspension” or “stable ACC” means an ACC which can be maintained in suspension or as a dry solid (e.g., powder) for a period of time ranging from a few hours to several days, weeks or months, without substantial conversion to the crystalline form. The term “substantial conversion” generally means conversion of about 5% of more of the amorphous to a crystalline form. Thus, the method of the invention produces ACC which generally remains at least 95% or more in the amorphous form (preferably at least about 97% or even more preferably at least about 99%) when left in a suspension or as a solid powder, at temperatures up to room temperature (about 20-30° C.) or even at higher temperatures.
[0048] As contemplated herein, the present invention involves the use of stabilizers as described herein, and a water miscible organic solvent to form a stabilized suspension of ACC. The stabilizers used in the present invention are referred to herein as the “first stabilizer”, the “second stabilizer” respectively. Additional stabilizers may also be used, if needed. Preferably, the method of the invention involves the use of a first and secondary stabilizer, which may be the same or different from each other, with each possibility representing a separate embodiment of the present invention. Also, the term “first stabilizer” is meant to encompass a single stabilizing compound or a combination of more than one stabilizing compounds. In addition, the term “second stabilizer” is meant to encompass a single stabilizing compound or a combination of more than one stabilizing compounds. Thus, in some embodiments, the aqueous calcium solution can contain one stabilizer or a combination of stabilizers (collectively referred to as “the first stabilizer”). In other embodiments, the solution comprising a second stabilizer can contain one stabilizer or a combination of stabilizers (collectively referred to as “the second stabilizer”). In accordance with the present invention, the total amount of stabilizer used in the process of the invention constitutes up to about 12 wt % of the stabilized ACC suspension.
[0049] According to one aspect, the stabilizing molecules of the present invention are divided between the calcium ion containing solution and a second stabilizing solution, termed “stabilizing solution”. In one embodiment, the stabilizing solution is an aqueous solution comprising the second stabilizer and optionally the water miscible organic solvent. In another embodiment, the stabilizing molecule can directly be dissolved in the water miscible organic solvent.
[0050] In some embodiments, each of the first and second stabilizer is independently selected from the group consisting of organic acids, phosphorylated organic acids, phosphoric esters of hydroxy carboxylic acids, sulfuric esters of hydroxyl carboxylic acids, phosphorylated amino acids and derivatives thereof, amino acid sulfate esters, and hydroxy bearing organic compounds combined with alkali hydroxides. According to one aspect, the stabilizing molecules are selected from, but not limited to, organic acids, phosphorylated amino acids, a phosphate bearing molecule, such as, but not limited to, phosphoenolpyruvate or phosphocreatine, or a sulfate bearing molecule, such as, but not limited to an amino acid sulfate ester such as sulfoserine or sulfothreonine, or any combinations of the foregoing. According to another aspect, the stabilizing molecules comprise a hydroxyl bearing molecule, such as (i) mono, di, tri or polysaccharides, for example, sucrose, mannose, glucose etc.; or (ii) hydroxyl-bearing non-phosphorylated amino acids, in combination with an alkali metal hydroxide, such as, but not limited to, sodium hydroxide or potassium hydroxide.
[0051] In general, the stabilizing molecules can be divided into two groups: 1) Stabilizers that have strong stabilizing effect on their own. The stabilizing molecules in this group include organic acids, for example carboxylic acids having at least two carboxylic groups and molecular weight not larger than about 250 g/mol (e.g., citric acid, tartaric acid, malic acid, etc.), and phosphoric or sulfuric esters of hydroxy carboxylic acids (e.g., phosphoenolpyruvate, phosphoserine, phosphothreonine, sulfoserine or sulfothreonine). 2) Stabilizing molecules that require the addition of hydroxide in order to deprotonate the hydroxyl groups of the stabilizing molecules and improve their stabilization effect. The stabilizing molecules in this group include mono-, di-, tri-, oligo- or poly-saccharides (glucose, mannose, fructose, sucrose, etc.), non-phosphorylated hydroxyl bearing molecules including polyols and amino acids (e.g., glycerol, serine, threonine, etc.). The term “non-phosphorylated hydroxyl bearing amino acid” refers to an amino acid, which may be natural or unnatural, which bears at least one hydroxyl (OH) group on its side chain.
[0052] According to one aspect of the invention, the stabilizing molecule in the calcium solution and the stabilizing molecule in the stabilizing solution are the same molecules. According to another aspect of the invention, they are two different molecules. In a preferred embodiment of the invention, the first stabilizer and the second stabilizer are identical, and the stabilizer amounts used, e.g., in step i) and step iii) of the process are in a ratio of from about 1:1 to about 10:1, for example about 1:2, about 1:3, about 1:5, about 2:1, about 3:1 or about 5:1 (first stabilizer to second stabilizer ratio). Each possibility represents a separate embodiment of the present invention.
[0053] According to one aspect of the invention, the organic solvent is from but is not limited to, alcohols, such as, methanol, ethanol, propanol or isopropyl alcohol, ketones, such as, but not limited to, acetone, diethyl ketone, cyclohexanone etc., or other water miscible organic solvents. Other examples of water miscible organic solvents include, but are not limited to ethers such as tetrahydrofuran or dioxane, acetonitrile, dimethoxyethane, diethoxyethane, dimethylformamide (DMF), and dimethyl sulfoxide (DMSO). The term “water miscible organic solvent”, as used herein, refers to an organic solvent capable of mixing with water in all proportions, forming a homogeneous solution.
[0054] The total amount of stabilizer used in the methods of the present invention means the combined amount of stabilizer used, e.g., the total amount of first and second stabilizers as described herein. Generally, the total amount of stabilizer constitutes up to about 12 wt % of the stabilized ACC suspension, preferably up to about 10 wt % of the stabilized ACC suspension, and more preferably up to about 8 wt % or up to about 5 wt % or up to about 3 wt % of the stabilized ACC suspension. Each possibility represents a separate embodiment of the present invention.
[0055] The water miscible organic solvent constitutes at least about 5 wt % of the stabilized ACC suspension. Ethanol is a currently preferred organic solvent.
[0056] In some embodiments, the calcium concentration in the calcium ion solution may be varied from about 4 mM up to about 2 M. For practical reasons the calcium concentration should be maintained between about 0.5 M-1 M, for example between 0.5 M and 0.75 M, or between 0.75 and 1 M. Each possibility represents a separate embodiment of the present invention.
[0057] In other embodiments, the carbonate concentration in the carbonate solution may be varied from about 4 mM up to about 2 M. For practical reasons the carbonate concentration should be maintained between about 0.5 M-1 M, for example between 0.5 M and 0.75 M, or between 0.75 and 1 M. Each possibility represents a separate embodiment of the present invention.
[0058] In further embodiments, the calcium:carbonate molar ratio may be varied from about 2:1 to about 1:1.5, respectively. For practical reasons, it is preferred to work with equimolar ratios of 1:1, however various ratios may be employed as contemplated by a person of skill in the art.
[0059] In further embodiments, the stabilizing molecule concentration in the calcium ion solution is between about 0.0001% and about 10% by weight of the calcium ion solution. More preferably, the concentration is between about 0.01% and about 3%; however, it was found that each stabilizing molecule has its own optimum concentration which can be readily determined by a person of skill in the art.
[0060] In further embodiments, the stabilizing molecule concentration in the stabilizing solution is between about 0.0002% and about 20% by weight of the calcium ion solution. More preferably the concentration is between about 0.02% and about 6%; however, it was found that each stabilizing molecule has its own optimum concentration which can be readily determined by a person of skill in the art.
[0061] According to one aspect of the invention, when a hydroxyl, phosphate or sulfate bearing molecule is combined with hydroxide as the stabilizing molecule, the mole ratio between the hydroxyl, phosphate or sulfate bearing molecule to the hydroxide is between about 4:1 and about 0.5:1, for example about 3:1, 2:1, 1:1 or 0.75:1, with each possibility representing a separate embodiment of the present invention.
[0062] In further embodiments, the ratio between the amount of stabilizing molecule in the stabilizing solution and the stabilizing molecule quantity in the calcium solution is between about 1:1 and about 20:1, for example about 2:1, 5:1, 10:1 or 15:1, with each possibility representing a separate embodiment of the present invention. It was found that for each stabilizing molecule pair there is a different optimum ratio which can be readily determined by a person of skill in the art.
[0063] In further embodiments, the organic solvent used is at a weight ratio of about 15:1 up to about 1:3 (water:solvent) of the total aqueous solutions. Different organic solvents perform better at different ratios, for example, it was found that ethanol performs well at a weight ratio of ˜7:1 while acetone performs well at a ratio of ˜5:1. The optimal ratio of water to organic solvent can readily by determined by a person of skill in the art.
[0064] In further embodiments, the temperature of the reaction can be carried at a range of temperatures from about −10° C. to about 60° C. The temperature range of the reaction is preferably maintained between about −3° C. and ambient temperature (room temperature (RT)), more preferably between about 0° C. and about 15° C.
[0065] According to one aspect of the invention the moisture in the powder ACC should be maintained below 15% in order to maintain the product's stability as a dry powder. According to another aspect of the invention the moisture should be preferably maintained below 10%, even more preferably below 8%.
[0066] According to one aspect of the invention the dry, stable product can be maintained under ambient conditions. According to another aspect of the invention the dry, stable product should be maintained in a controlled humidity environment of preferably less than 20% relative humidity.
[0067] According to one aspect of the invention the calcium content in the produced ACC is between about 30% and about 33%. Preferably the calcium content in the ACC is between about 31.5% and about 32.5%.
[0068] The produced ACC can be filtered using standard liquid/solid separation methods such as, but not limited to, vacuum or pressure filtrations, centrifugation or decantation, and then dried using standard drying equipment such as, but not limited to, air dryers, vacuum or turbo ovens, spray dryers, flash dryers, freeze dryers or paddle dryers.
[0069] The following examples are presented in order to more fully illustrate certain embodiments of the invention. They should in no way, however, be construed as limiting the broad scope of the invention. One skilled in the art can readily devise many variations and modifications of the principles disclosed herein without departing from the scope of the invention.
Example 1
[0070] In a typical procedure, the calcium solution contained 1 liter of water, 88.8 g of calcium chloride and 888 mg of phosphoserine. The carbonate solution contained 1 liter of water and 84.8 g of sodium carbonate. The stabilizing solution contained 200 ml of water and 1.776 g of phosphoserine and 350 ml of ethanol was used as the organic solvent. The calcium and carbonate solutions were mixed together to precipitate non-stabilized ACC, the stabilizer solution was added to the ACC suspension after 20 seconds followed by the ethanol creating stabilized ACC suspension. The resulting stabilized ACC suspension stabilized ACC for at least 3 hours in solution at ˜20° C. and for at least 9 hours at 0° C. The ACC was then filtered during the time it was still stable in suspension, using a Buchner funnel, and the filtered cake was dried using a regular oven at 40-50° C.
Example 2
[0071] The calcium solution contained 1 liter of water, 88.8 g of calcium chloride and 700 mg of citric acid. The carbonate solution contained 1 liter of water and 84.8 g of sodium carbonate. The stabilizing solution contained 200 ml of water and 1.4 g of citric acid and 350 ml of ethanol was used as the organic solvent. The calcium and carbonate solutions were mixed together to precipitate non-stabilized ACC, the stabilizer solution was added to the ACC suspension after 20 seconds followed by the ethanol creating stabilized ACC suspension. The resulting stabilized ACC suspension stabilized ACC for at least 3 hours in solution at ˜20° C. and for at least 9 hours at 0° C. The ACC was then filtered during the time it was still stable in suspension, using a Buchner funnel, and the filtered cake was dried using a vacuum oven at 40-50° C., 400 mb under nitrogen atmosphere.
Example 3
[0072] The calcium solution contained 1 liter of water, 88.8 g of calcium chloride and 888 mg of phosphothreonine. The carbonate solution contained 1 liter of water and 84.8 g of sodium carbonate. 1.776 g of citric acid was dissolved in 350 ml of ethanol. The calcium and carbonate solutions were mixed together to precipitate non stabilized ACC and the ethanol-stabilizer solution was added to the ACC suspension after 20 seconds creating a stabilized ACC suspension. The resulting stabilized ACC suspension stabilized ACC for at least 5 hours in solution at ˜20° C. and for at least 9 hours at 0° C. The ACC was then filtered during the time it was still stable in suspension, using a Buchner funnel, and the filtered cake was dried using a regular oven at 40-50° C.
Example 4
[0073] The calcium solution contained 1 liter of water, 88.8 g of calcium chloride, 20 g of sucrose and 3.35 g of sodium hydroxide. The carbonate solution contained 1 liter of water and 84.8 g of sodium carbonate. The stabilizing solution contained 200 ml of water 40 g of sucrose and 6.67 g of sodium hydroxide and 350 ml of ethanol was used as the organic solvent. The calcium and carbonate solutions were mixed together to precipitate non stabilized ACC, the stabilizer solution was added to the ACC suspension after 20 seconds followed by the ethanol creating stabilized ACC suspension. The resulting stabilized ACC suspension comprised ACC stable for at least 10 hours at ˜20° C. and for at least 24 hours at 0° C. The ACC was then centrifuged using a bench top centrifuge at 4000 rpm for 5 minutes, the supernatant was discarded and the concentrated product was freeze-dried using a lyophilizer at −80° C. and high vacuum overnight.
Example 5
[0074] The calcium solution contained 1 liter of water, 88.8 g of calcium chloride, 10 g of serine and 3.8 g of sodium hydroxide. The carbonate solution contained 1 liter of water and 84.8 g of sodium carbonate. The stabilizing solution contained 200 ml of water, 20 g of serine and 7.62 g of sodium hydroxide and 350 ml of ethanol was used as the organic solvent. The calcium and carbonate solutions were mixed together to precipitate non stabilized ACC, the stabilizer solution was added to the ACC suspension after 20 seconds followed by the ethanol creating stabilized ACC suspension. The resulting stabilized ACC suspension comprised ACC stable for at least 2 hours at ˜20° C. and for at least 8 hours at 0° C. The ACC was then centrifuged using a bench top centrifuge at 4000 rpm for 5 minutes, the supernatant was discarded and the concentrated product was freeze-dried using a lyophilizer at −80° C. and high vacuum overnight.
Example 6
[0075] The calcium solution contained 1 liter of water, 88.8 g of calcium chloride, 10 g of serine and 3.8 g of sodium hydroxide. The carbonate solution contained 1 liter of water and 84.8 g of sodium carbonate. The stabilizing solution contained 200 ml of water 20 g of sucrose and 7.62 g of sodium hydroxide and 350 ml of ethanol was used as the organic solvent. The calcium and carbonate solutions were mixed together to precipitate non stabilized ACC, the stabilizer solution was added to the ACC suspension after 20 seconds followed by the ethanol creating stabilized ACC suspension. The resulting stabilized ACC suspension comprised ACC stable for at least 6 hours at ˜20° C. and for at least 24 hours at 0° C. The ACC was then centrifuged using a bench top centrifuge at 4000 rpm for 5 minutes, the supernatant was discarded and the concentrated product was freeze-dried using a lyophilizer at −80° C. and high vacuum over night.
[0076] FIGS. 1 and 2 show representative ACC Raman and XRD spectra of dry samples prepared according to above Examples 1 and 2. FIGS. 3 and 4 show the XRD spectra of vaterite and calcite, for comparison.
[0077] While the present invention has been particularly described, persons skilled in the art will appreciate that many variations and modifications can be made. Therefore, the invention is not to be construed as restricted to the particularly described embodiments, and the scope and concept of the invention will be more readily understood by reference to the claims, which follow. | Provided is a method for preparing a stable amorphous calcium carbonate (ACC), which can be obtained either in suspension or as a powder. The method comprises stepwise combination of a soluble calcium salt, a soluble carbonate, a first and second stabilizer, and a water miscible organic solvent as described herein. The present invention further relates to stable ACC suspensions and dry powders produced by the method of the present invention. | 2 |
CROSS-REFERENCE TO RELATED PATENT APPLICATIONS
This patent application is a continuation of U.S. application Ser. No. 12/992,702, now U.S. Pat. No. 9,220,892, filed Nov. 15, 2010, which is the National Stage of International Application No. PCT/EP2009/055984, filed May 18, 2009, which further claims the benefit of European Application No. 08171007.1, filed Dec. 8, 2008 and U.S. Provisional Application No. 61/053,788, filed May 16, 2008, the entire teachings and disclosure of which are incorporated herein by reference thereto.
FIELD OF INVENTION
The present invention relates to a method to remove a tumor comprising the use of a surgical instrument, in particular to a percutaneous surgical instrument, and relates also to an electrode guiding device for such surgical instruments.
PRIOR ART AND RELATED TECHNICAL BACKGROUND
Radiofrequency (RF) therapy, is a well known non-invasive and outpatient procedure that uses radio waves. Generally, it is used to treat cancer, more particularly for the ablation of tumors from different organs, e.g. breast, colon, lungs, pancreas, prostate, kidney.
In such procedure, electrodes are placed into contact with the tissue to treat and a current, from a RF generator, is applied to the tissue via the electrodes. As the current passes, the tissue between the electrodes heats, a lesion is created, and the corresponding tissue is destroyed.
RF surgical devices are well known. Generally they are monopolar devices.
The device described in U.S. Pat. No. 5,507,743 may be a monopolar or a bipolar device. In the bipolar form of the device, it comprises one straight and one helical (coiled) electrode, the straight electrode being inside the helix formed by the helical one. In U.S. Pat. No. 5,507,743, to increase the size of the lesion created, both electrodes are hollow with a plurality of fluid distribution ports to deliver, into or onto the tissue to be ablated, a conductive fluid, such as chemotherapeutic agent or as an isotonic or hypertonic saline solution.
One of the main disadvantages of such RF surgical devices is that no confinement of the lesion is achieved. Furthermore it is very difficult to predict how wide the lesion created will be.
In WO2004/100812, the bipolar RF device is a three elements device wherein at least two of the elements are “dry” electrodes, i.e. not hollow and not able to deliver a conductive fluid. In the bipolar RF device described, the electrodes may be either both helical (coiled) and parallel one to another, or one helical and one straight. The bipolar RF device works by a cage effect allowing some confinement of the lesion created.
One of the main disadvantages of such bipolar RF surgical devices working with a cage effect, is the imprecise confinement of the lesion created as the positioning of the RF electrodes, to effectively ablate the tissue, may be imprecise.
To ensure optimal performance, the axis of each electrode should be parallel; However, due to the piercing resistance of the skin, the tissue, or the organ to treat, and even if Radiofrequency electrodes are sharp and not deformable, the electrodes are prone to touch, or come close, one to another, leading to a misalignment of the electrodes and a reduced performance of RF devices.
In addition, a controlled widening of the confinement is not possible with such bipolar RF surgical devices.
AIMS OF THE INVENTION
The present invention aims to provide a method to remove a tumor comprising the use of a percutaneous surgical device which does not have the drawbacks of the prior art.
Particularly, the invention aims to provide a method to remove a tumor comprising the use of a RF surgical device with enhanced performance.
More particularly, the invention aims to provide a method to remove a tumor comprising the use of a RF surgical device which allow a defined confinement of the lesion created.
The present invention aims also to provide a method to remove a tumor comprising the use of a RF surgical device with stabilised electrodes.
The present invention aims also to provide a method to remove a tumor comprising the use of a device which ensure a dimensional stability of the electrodes of a RF surgical device.
SUMMARY OF THE INVENTION
The present invention relates to a method to remove a tumor comprising the use of a bipolar Radiofrequency surgical instrument comprising at least two dry electrodes, and a electrode guiding device comprising a main body, having a proximal end and a distal end, and at least two insertion holes guiding said electrodes, said insertion holes extending through the body.
The term “dry electrode” should be understood as “solid electrode”, solid electrode meaning that the electrode is not hollow and not able to deliver a conductive fluid.
According to particular embodiments, the bipolar Radiofrequency surgical instrument may comprise one or a combination of any of the following characteristics:
the at least two dry electrodes are helical; at least one dry electrode is helical, and at least one dry electrode is straight; the at least two dry electrodes are arranged in a concentric manner; the shape and the size of the holes correspond to the shape and the size of the corresponding dry electrodes; the diameter of the holes do not exceed 10% of the diameter of the electrodes; the bipolar Radiofrequency surgical instrument comprises a RF current generator, positioning means, controlling means, location means and imaging means.
The present invention relates also to a method to remove a tumor comprising the use of a device for guiding at least two Radiofrequency electrodes of a bipolar Radiofrequency surgical instrument, said guiding device comprising a main body, having a proximal end and a distal end, and at least two insertion holes guiding said electrodes, said insertion holes extending through the body.
According to particular embodiments, the guiding device may comprise one or a combination of any of the following characteristics:
the insertion holes are helical and arranged in a concentric manner at the proximal end of said body; the body comprises at least one helical insertion hole and one straight insertion holes, said holes being arranged in a concentric manner at the proximal end of said body; the diameter of the insertion holes do not exceed 10% of the diameter of the electrodes; the body further comprises at least a supplementary hole at the distal end of the body, said supplementary hole being straight; the body is circular, and a first series of supplementary holes are arranged, in a tangential manner, at the periphery of said body; the body further comprises a second series of supplementary holes arranged in a tangential manner in respect to the first series of supplementary holes; the at least one helical insertion hole is formed by engaging a threaded rod into a circular opening of the body; the guiding device comprises a fixing part to fasten the guiding device to the head of a laparoscopic surgical instrument or to positioning means of a percutaneous surgical instrument.
The present invention relates also to a kit of parts comprising the guiding device according to the invention, and at least two dry Radiofrequency electrodes.
The present invention relates also to a method to remove a tumor comprising the use of a Radiofrequency surgical instrument according to the invention.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic representation of the RF surgical device according to a first preferred embodiment.
FIG. 2 is a schematic representation of the RF surgical device according to a second preferred embodiment.
FIG. 3 is a schematic representation of the RF surgical device according to a third preferred embodiment.
FIG. 4 is a schematic representation of the cage effect whereby the RF surgical device treats the tissue.
FIG. 5 is a schematic representation of the guiding device according to a first embodiment of the invention.
FIG. 6 is a schematic representation of the guiding device according to a second embodiment of the invention.
FIG. 7 is a schematic representation of the guiding device according to a third embodiment of the invention.
FIG. 8 is a schematic representation of a two pieces embodiment of the guiding device according to the invention.
FIG. 9 is a schematic representation of a “X, Y” head of a preferred embodiment of the RF surgical device.
DETAILED DESCRIPTION OF THE INVENTION
The bipolar Radiofrequency surgical instrument according to the present invention comprises at least one helical electrode ( FIG. 1 ), preferably two helical electrodes 3 and 4 ( FIG. 2 ), or an helical electrode 3 and a straight electrode 5 ( FIG. 3 ) and a electrode guiding device 6 .
Preferably, the bipolar RF surgical instrument is of the type described in WO2004/100812 which is incorporated herein by reference. The RF surgical device comprise a main body 1 , stabilisation means 2 and at least a set of electrodes which can be helical, more preferably two helical electrodes, and even more preferably three helical electrodes. Optionally, it may further comprise a central member 5 , which may or may not be a straight electrode, and which is surrounded by the helical electrodes 3 or 4 . When the central member 5 is an electrode, it can be used with either a single helical electrode, or with two or more helical electrodes.
The RF electrodes 3 , 4 and/or the central member 5 are sharp, not deformable, and rigid electrodes. They are “dry electrodes”, i.e. not hollow and not able to deliver a conductive fluid. Preferably, they are made of metal, a biocompatible metal, preferably made of biocompatible stainless steel. It may be for example surgical stainless steel type 304 or type 316.
Preferably, the electrodes and/or the central member 5 are coated with an isolating polymeric compound, for example coated with TFE or polyester. More preferably, they are coated along their length but except on their tip, for example over around one turn for helical electrodes and around 1.5 cm for the central member.
The helical electrodes 3 and 4 may have the same diameter or a diameter different. Preferably, their diameter is between 1 and 2 mm, more preferably around 1.2 mm, or around 2 mm. Preferably, their length is of at least 15 turns, or a length of around 150 cm. The pitch is preferably a right-handed pitch, preferably of between 5 and 20 turns by cm. The helix formed by the helical electrodes 3 or 4 have preferably a diameter comprised between 8 to 24 mm. However, it is possible to adapt the diameter of the helix formed by the helical electrodes 3 or 4 according to the volume of the target tissue to treat.
The helical electrodes 3 , 4 are wounded parallel one to the other and have the same pitch. The helix formed by one of the electrode is arranged in a concentric manner in respect to the helix formed by the other, or others, electrodes.
Preferably, the central member 5 have diameter and length corresponding to those of the helical electrode 3 or 4 . More preferably, the diameter of the central member 5 is around 1.5 mm.
The central member 5 can be placed at the centre of the helix formed by the helical electrode 3 or 4 .
In a preferred embodiment, the helical electrodes 3 and 4 , and the central member 5 are fixed in the stabilisation means 2 by any suitable means.
In another preferred embodiment, the helical electrodes 3 and 4 are fixed in the stabilisation means 2 by any suitable means, while the central member 5 is removable.
Preferably, the helical electrodes 3 and 4 are glued in the stabilisation means 2 and are in contact with a connector which can be in electrical contact with a Radiofrequency generator.
As the central member 5 may be removable ( FIG. 3 ), it may comprise at one end a connector which can be in electrical contact with a Radiofrequency generator.
The stabilisation means 2 of the RF surgical instrument have a hollow cylindrical shape, made of a biocompatible polymeric material, for example poly-ether-ether-ketone (PEEK), polycarbonate or polyamide. It further may comprise a channel through which the central member 5 can pass.
Preferably, the stabilisation means 2 , comprising the helical electrodes 3 or 4 , is disposable. Preferably, the central member 5 is also disposable.
Each electrodes (electrodes 3 , 4 , and central member 5 ) can be activated independently one from the other to get a first pole (first electrode) and an second pole (second electrode), “activated” meaning that a current is applied into the electrode.
In on embodiment the first and the second pole are helical electrodes. In another embodiment, the first pole is a helical electrode 3 and the second pole is the central member 5 .
When applying a current to at least one electrode of the RF surgical instrument according to the present invention, the surgical instrument works by a cage effect ( FIG. 4 ). The heating created into the tissue goes from the closest electrode to the centre to the furthermost electrode. The tissue, which is in the cage formed by the electrodes, is thus destroyed, while the tissue outside the cage is safe.
The different combination between the type of electrodes (helical and/or straight), and the different diameter of the helix formed by helical electrodes, present the advantage of having a RF surgical instrument which can be easily adapted to the size of the tissue to treat. Furthermore, the use of the central member 5 presents the advantage of having the possibility to treat a smaller tissue volume, for example in combination with a smaller helical electrode (electrode 4 ). It may further present the advantage of modifying the shape of the treated zone, from a square like shape, in case of use of helical electrodes, to a sharper shape.
The electrode guiding device 6 according to the invention presents the advantage to maintain the dimensional stability of the electrodes by preventing their deformation during the perforation of the skin or the organ. Thus the confinement of the lesion created is precise and the tissue treated is as predicted. The precision of the treatment achieved is below 1 mm. It further enables an easier penetration of the helical electrodes 3 and 4 by making easier the penetration screw like movement.
The electrode guiding device 6 of the RF surgical instrument according to the invention comprises a main body 7 comprising at least two holes 8 and 81 ( FIG. 5 ) or 8 and 82 ( FIG. 6 ), or three holes 8 , 81 and 82 ( FIG. 7 ), extending through the body 7 .
The body 7 comprises a front side 71 , a back side 72 , a proximal end 73 and a distal end 74 .
The body 7 has any suitable shape, preferably it is substantially round, but may also have, for example, a polygonal or a square shape. It is made of any metal, or of polymeric material. Preferably, it is made of titanium or stainless steel, or of a poly-ether-ether-ketone (PEEK), polycarbonate, or polyamide.
The body 7 comprises at least two holes 8 and 81 , or 8 and 82 , extending through the body 7 from the front side 71 to the back side 72 . Preferably, the holes are arranged at the primal end 73 of the body 7 .
Through the body 7 , and on the surfaces defined by the front side 71 and the back side 72 , the holes 8 , 81 , and/or 82 have a shape and a diameter enabling the electrodes 3 , 4 , 5 to go through. Preferably, their shape and diameter correspond substantially to the shape and the diameter of the RF electrodes 3 , 4 , 5 to guide and which pass thought.
Through the body 7 , the hole for a straight electrode is substantially straight, and the hole for a helical electrode is substantially helical or substantially of a corkscrew shape, with either a left-handed or a right-handed pitch depending of the pitch of the helical electrodes. On the surfaces defined by the front side 71 and the back side 72 , the hole 82 may be round, square, oval, or octagonal.
The diameter of the holes 8 and 81 is substantially equal, or corresponding, to the diameter of the helix formed by the corresponding electrodes 3 and 4 . The size of the opening forming the holes 8 and 81 is substantially equal, or corresponding, to the diameter of the corresponding electrodes 3 and 4 , preferably the size of the opening do not exceed 10% of the diameter of the electrodes 3 or 4 .
The diameter of the hole 82 is substantially equal, or corresponding, to the diameter of the central member 5 , and preferably do not exceed 10% of the diameter of the central member 5 .
In a preferred embodiment, the body 7 of the guiding device comprises two helical holes 8 and 81 ( FIG. 5 ).
In another preferred embodiment, the body 7 of the guiding device comprises one helical 8 and one straight hole 82 ( FIG. 6 ).
In another preferred embodiment, the body 7 comprises two helical holes 8 , 81 and one straight hole 82 ( FIG. 7 ).
However, the number of holes and their shape are not limited to those disclosed here as examples. The guiding device may comprise as many holes, and as different, as RF electrodes are.
Preferably, the guiding device 6 according to the present invention cooperates with the RF electrodes as described. However, the electrode guiding device may be used with any RF surgical instrument having at least two RF electrodes, straight and/or helical, being either hollow to deliver a conductive fluid, or dry, and having any size and any length. Nevertheless, the electrode guiding device is well suited to devices comprising two helical electrodes wounded parallel one to the other.
The body 7 of the electrode guiding device has an overall size at least higher than the external diameter of the furthermost helical electrode from the centre of said body 7 (electrode 3 in FIGS. 1 to 3 ). Preferably, the body 7 has a size and a shape enabling his use with a catheter.
Preferably, the body 7 has a overall size of between 8 and 30 mm, a thickness of between 1 and 3 cm. The spacing between two helical holes is around 20 mm.
In another preferred embodiment of the electrode guiding device 6 according to the invention, the body 7 may comprise at least one supplementary hole 10 arranged at the distal end 74 of the body 7 . Preferably, the body 7 comprises several straight holes 10 laid in a tangential manner at its periphery. More preferably, the body 7 comprises two series of straight holes 10 , 11 , laid in a tangential manner at its periphery, the holes 10 of the first series being tangent to the periphery of the body 7 , and the holes 11 of the second series being tangent to the holes 10 of the first series of holes ( FIGS. 5 to 7 ).
The supplementary hole 10 and/or 11 guide any other electrode, an anchoring member, or a needle, for example a straight needle, to introduce a conductive fluid or chemotherapeutic agent into the tissue before, during, or after ablation, or a needle biopsy aspiration device or any sensor, for example temperature sensors, or any optical device, or illumination fibres.
In a preferred embodiment, the supplementary holes 10 and/or 11 guide a straight RF electrode. Preferably, the straight RF electrode is of the type of the central member 5 .
When the tissue to treat is bigger than the diameter of the biggest helix formed by the outermost helical electrode 3 , at least one straight RF electrode can be used, said straight RF electrode being guided precisely where wanted, thanks to the specific arrangement of the supplementary holes 10 and/or 11 into the guiding device 6 . To widen the volume of tissue to treat, the RF current is applied either between the helical electrode 3 and the supplementary straight electrode, or between the central member 5 and the supplementary straight electrode.
Optionally, the guiding device further comprises a fixing part 9 , to allow the guiding device 6 to be handheld, or to be fixed to a percutaneous surgical instrument or a laparoscopic surgical instrument.
The body 7 of the electrode guiding device may be made either of one piece, or made of the assembly a two elements, one corresponding to the front side 71 and the other corresponding to the back side 72 of the device, the two elements being assembled by any suitable method.
The one piece body 7 , or the two elements body 7 , may be produced by any suitable method, for example by extrusion, by moulding or by stereolytography.
In a preferred embodiment, the hole 8 , 81 , 82 and the supplementary hole 10 or 11 are formed during the process to manufacture the body 7 . In another embodiment, the hole 8 , 81 , 82 and the supplementary hole 10 or 11 are drilled, by any suitable means, into the mass of the one piece body 7 , or in the two elements corresponding to the front side 71 and the back side 72 of the body 7 , the holes being drilled before or after the assembly of the two elements of the body 7 .
In another embodiment, the holes 8 , 81 or 82 are not drilled but are formed by the assembly of a one piece body 12 , or a front side and back side elements assembly, having a circular opening 13 , and a threaded rod 14 engaged in said circular opening 13 ( FIG. 8 ). Preferably, the threaded rod 14 is engaged by force in the opening 13 and fixed to the body 7 , for example by heat welding or by mean of a biocompatible glue.
Preferably, the threaded rod 14 is made of the same material as the one of the body 7 , or as the one of the front side and back side elements, for example, made of PEEK.
The diameter of the opening 13 and the external diameter of the threaded rod 14 are chosen to fit the external diameter of the helical electrode to guide. Furthermore, the length of the threaded rod 14 substantially corresponds to the thickness of the body 7 , and its pitch substantially corresponds to the pitch of the helical electrode, in terms of dimension and type of pitch (either left-handed or right-handed thread).
Preferably, the threaded rod 14 further comprises a hole 82 , which may be an helical hole or a straight hole. The threaded rod 14 may comprise a helical and a straight hole. The hole 82 may be drill in the threaded rod 14 , or may be formed by the engagement a threaded rod in an opening at the centre of the threaded rod 14 .
The guiding device 6 may be fastened by any suitable means to a laparoscopic instrument, for example an endoscope, to a positioning head of a percutaneous surgical instrument, or to be held by hand. Preferably, this fastening is achieved by a fixing part 9 of the guiding device 6 .
Preferably, the electrode guiding device is disposable.
The RF surgical instrument, and the electrode guiding device, according to the invention, may be parts of a more complex surgical instrument.
In a preferred embodiment, the RF surgical instrument, and the electrode guiding device, according to the invention, may be parts of a laparoscopic surgical instrument, for example an endoscope device. Therefore, the electrode guiding device 6 may be fixed to the head of the endoscope by, for example, a fixing part 9 , which may have any suitable shape and size. The front side 71 of the guiding device 6 is place against the organ to treat and the electrodes extend out through the head of the endoscope device, engage, and extend out through, the electrode guiding device 6 , and penetrate into the organ in a screw-like movement for helical electrodes, or a straight movement for a straight electrode, as deep as necessary to reach the zone to treat.
The laparoscopic surgical instrument may further comprise a RF current generator, and optionally, spatial location means, optical means, biopsy aspiration means, sensors and/or computer means.
In a preferred embodiment, the RF surgical instrument, and the electrode guiding device, according to the invention, may be parts of a percutaneous surgical instrument. Therefore, the surgical instrument further comprises a RF current generator, and optionally, positioning means, controlling means, location means, imaging means, and computer means.
In percutaneous applications, the front side 71 of the guiding device 6 is place against the skin and is hand-held, for example by the fixing part 9 , said fixing part 9 having any suitable shape and size. Then, the electrodes 3 , 4 and/or 5 are engaged into the holes of the guiding device, and extend out through the guiding device 6 to penetrate through the skin in a screw-like movement for helical electrodes, or a straight movement for the straight electrode, as deep as necessary to reach the zone to treat. However, this operation may be more automated by using positioning means and controlling means. The RF surgical device may further comprise location means and imaging means.
Preferably, the positioning means comprise a “X, Y” head 12 ( FIG. 9 ), or a robot arm, to which the electrode guiding device 6 is fixed, for example by using the fixing part 9 of any suitable shape and size allowing its fastening to the “X, Y” head 12 or robot arm.
The location means, comprising for example a ultrasound probe coupled to imaging means, allow to get the exact position of the tissue to treat and give a reference point to insure the precise positioning of the electrodes using the “X, Y” head 12 , before and after the penetration of the electrodes 3 , 4 , 5 . Preferably, the location means are controlled by the computer means.
The front side 71 of the guiding device 6 , fastened to the “X, Y” head 12 , for example by the fixing part 9 , is place against the skin precisely at the point of entry determined by location means, at the level of the tissue to treat, or the area chosen for the treatment. Then, the electrodes 3 , 4 and/or 5 extend out through the electrode guiding device 6 , and penetrate through the skin as deep as necessary to reach the zone to treat.
The “X, Y” head 12 , and/or the movement of the electrodes 3 , 4 , 5 , may be hand-operated, for example by the operator of the surgical instrument, or automatically operated using the controlling means, which may comprise for example a stepper motor which may be controlled by the computer means.
Preferably, in either the laparoscopic or percutaneous embodiments, the treatment of the tissue or the organ may be followed by the location means coupled to the imaging means.
If necessary, to widen the volume of the area to treat, without being obliged to remove the electrodes and to readjust the position with the “X, Y” head 12 , one or more straight electrodes may be used. These supplementary electrodes are precisely positioned thanks to the supplementary hole 10 and/or 11 of the guiding device 6 . Thus, the area treated is widened while the skin perforation is reduced to a minimum.
The electrode guiding device 6 according to the invention presents the advantage of allowing thus a precise electrodes positioning in respect to the tissue to treat, as it is an alternate solution to the traditional grid used to guide straight electrodes of percutaneous surgical instrument.
It has also the advantage of giving the possibility to widen the treated area by guiding at precise locations supplementary electrodes.
The RF surgical instrument, according to the invention comprising the guiding device 6 , presents the advantage of having enhanced performances. It also has the advantage of being adaptable to any size or shape of tumours to treat. It also has the advantage of being minimally invasive.
The RF surgical instrument, according to the invention, may preferably been used to treat prostate, kidney or breast cancer. | The present invention relates to a method of removing a tumor by radiofrequency ablation, comprising providing a guiding device ( 6 ) having at least two first concentric through holes ( 8, 81, 82 ) and a plurality of second through holes ( 10, 11 ) at a periphery of the guiding device ( 6 ). The method further comprising placing the guiding device against the skin of a patient and inserting two first electrodes ( 3, 4, 5 ) into the first through holes ( 8, 81, 82 ) of the guiding device and into a patient's skin and then applying a first radiofrequency current between the two first electrodes ( 3, 4, 5 ). The method further comprising inserting a second electrode ( 5 ) through a second through hole ( 10, 11 ) and into the patient's skin and then applying a second radiofrequency current between a first electrode ( 3, 4 ) and the second electrode ( 5 ). | 0 |
RELATED APPLICATIONS
[0001] This application is a continuation-in-part application that claims the benefit under 35 U.S.C. §120 of U.S. application Ser. No. 12/724,025 filed on Mar. 15, 2010, entitled COVE BASE NOZZLE FOR DISPENSING APPLICATIONS, which in turn claims the benefit under 35 U.S.C. §119(e) of Provisional U.S. Application Ser. No. 61/160,853, filed on Mar. 17, 2009, also entitled COVE BASE NOZZLE FOR DISPENSING APPLICATIONS, all of whose entire disclosures are incorporated by reference herein.
BACKGROUND OF THE INVENTION
[0002] This invention relates generally to nozzles for handheld dispensing tools, and more specifically to nozzle for dispensing tools employed to dispense viscous materials such as gluing and sealing materials and the like.
[0003] Dispensing devices for the application of various viscous material products such as construction adhesives, caulking materials, grease, automotive windshield sealant, dual component reactive resins, sealants, and the like, are well known throughout many industries. Such dispensing devices ideally allow the viscous material to be applied in an accurate, mess-free, and waste-free manner.
[0004] Dispensing devices are often in the form of a dispensing gun, or caulking gun. Dispensing devices generally include a squeezable handle and trigger assembly which is operative for advancing the pistons of the dispensers and for maintaining the pistons in advanced positions when the trigger portions of the dispenser devices are released. The viscous materials can be packaged in a variety of forms; some of the most common are cartridge form, collapsible form, and bulk form.
[0005] Cartridges are most often designed with a nozzle through which a viscous material composition can be extruded. These cartridges were adapted to be loaded into dispensing devices equipped with mechanisms to push the sealant composition out of the cartridge package. Cartridges, depending on the kind of storage required for the viscous material composition, are generally made from paper, foiled lined paper, plastic, and various kinds of molded and laminated constructions.
[0006] The cartridges are typically tubes having a sealed dispensing outlet, such as a conical tip, disposed on one end, with the other end being open for receiving a plunger mechanism or the like from the dispensing device. Just inside the cartridge's open end is a slidably-sealed, axially-movable piston, disc, or the like. For use, the cartridge is placed in a retaining/dispensing section of the dispensing device, and the plunger is brought into contact with the piston. When a user desires to dispense product, the cartridge's dispensing outlet is unsealed, typically by cutting, and the plunger is forced against the piston. This forces the piston axially down the tube and against the product, which in turn is dispensed through the dispensing outlet.
[0007] Collapsible tubes are also popular containers for viscous materials. Collapsible packaging has been known in the trade for many years, and offers the benefits of providing good shelf stability for the contained chemicals, low package cost, and minimal packaging waste. Collapsible packages are generally known in the art as a “sausage” or “chub.” Collapsible packaging has a collapsible wall that is, typically, sealed at each end. While collapsible package can be used to contain non-reactive viscous material products, the collapsible package is typically moisture impervious, thus allowing the collapsible package to contain reactive viscous material products also (typically reactive viscous material products are ones that react when exposed to humidity in the air).
[0008] Bulk forms of the viscous material may be used with dispensing devices which have a dispensing chamber adapted to be filled directly with the bulk viscous material. All of these options (i.e., cartridge, bulk form, and collapsible form) can be employed in dual component dispensing devices as well as in single component dispensing devices. Moreover, the nozzles of the present invention can be employed with each of these options.
[0009] In many applications, multiple beads of adhesive are applied to the parts to be joined, where the surface area of the parts is large enough to require more than a single bead for adequate coverage and adhesion. A nozzle that emits multiple beads simultaneously increases application speed and provides a uniform separation distance between beads. Increased application speed ensures that, in the case of an adhesive, the amount of time that the adhesive is exposed to the air before the parts to be joined are affixed is reduced, thus improving adhesion and allowing for more uniform adhesion across large work areas. Nozzles with multiple dispensing outlets are known for this purpose. Not all applications, however, require as many beads of material as are available in presently available multi-tipped application nozzles, which typically have three or five outlets.
[0010] Therefore, there exists a need for a multi-tipped application nozzle for viscous materials wherein the user can select which tips are active and which do not eject material. Also, there exists a need for a multi-tipped application nozzle wherein the user can control the size of the nozzle opening to control the amount of the material to be dispensed. Also, there exists a need for an application nozzle which can be used in combination with a dispensing device regardless of the manner in which the viscous material is packaged, i.e., cartridge form, collapsible form, or bulk form. All references cited herein are incorporated by reference in their entireties.
BRIEF SUMMARY OF THE INVENTION
[0011] A nozzle is disclosed for dispensing viscous material comprising a plurality of dispensing tubes having dispensing tips and a single input cavity adapted to accept the viscous material. In an embodiment, at least one of the dispensing tips is manufactured closed and can be opened at the user's discretion.
[0012] In a further embodiment, the nozzle input cavity is adapted to accept a single nozzle from a material container, such as a cartridge. In a further embodiment, the nozzle includes a detachable locking plate enabling attachment of the nozzle to the front cap of a device for dispensing material in bulk form. In a further embodiment, the nozzle includes a detachable locking plate enabling attachment of the nozzle to the front cap of a device for dispensing material from a collapsible package, such as a sausage or chub.
[0013] In a further embodiment, the nozzle has a flange at the input tube end, and the flange holds the nozzle between a dispensing tool end-stop and a material container, such as the tip of a tube of adhesive or sealant. In an embodiment, the dispensing tubes are at an angle to the centerline of the material dispenser. In a further embodiment, the nozzle screws into a threaded socket on a dispensing tool by a thread on the outside of the input tube.
[0014] In a further embodiment, the nozzle has a flange at the input tube end, and the flange holds the nozzle between a dispensing tool end-stop and a material container, such as the tip of a tube of adhesive or sealant. In an embodiment, the dispensing tubes are at an angle to the centerline of the material dispenser. In a further embodiment, the nozzle screws into a threaded socket on a dispensing tool by a thread on the outside of the input tube.
BRIEF DESCRIPTION OF SEVERAL VIEWS OF THE DRAWINGS
[0015] The invention will be described in conjunction with the following drawings in which like reference numerals designate like elements and wherein:
[0016] FIG. 1 is a drawing of an exemplary multi-tip nozzle of the present invention in use;
[0017] FIG. 2 is a drawing of an exemplary multi-tip nozzle of the present invention with two tips cut open for dispensing material;
[0018] FIG. 3 is a sectional view taken along line 3 - 3 of FIG. 2 ;
[0019] FIG. 4 is a sectional view taken along line 4 - 4 of FIG. 2 ;
[0020] FIG. 5 is drawing of an alternate embodiment of a multi-tip nozzle;
[0021] FIG. 6 is a sectional view taken along line 6 - 6 of FIG. 5 ;
[0022] FIG. 7 is an exploded view of a second alternative embodiment of the multi-tip nozzle of the present invention having versatility to be mounted to the dispensing end of a dispenser, regardless of the manner in which the viscous material is packaged, i.e., cartridge form, collapsible form, or bulk form;
[0023] FIG. 8 is an enlarged view of the second alternative embodiment of FIG. 7 shown mounted to the dispensing end of a sausage type or bulk type dispensing device;
[0024] FIG. 9 is a sectional view taken along line 9 - 9 of FIG. 8 ;
[0025] FIG. 10 is an exploded view of a third alternative embodiment of the nozzle of the present invention wherein the flange and mounting plate are incorporated with a nozzle of conventional design and shape, e.g., a ribbon nozzle head, to provide versatility to enable mounting of the nozzle to the dispensing end of a dispenser, regardless of the manner in which the viscous material is packaged, i.e., cartridge form, collapsible form, or bulk form; and,
[0026] FIG. 11 is an enlarged view of the third alternative embodiment of FIG. 10 shown mounted to the dispensing end of a sausage type or bulk type dispensing device.
DETAILED DESCRIPTION OF THE INVENTION
[0027] FIG. 1 shows an exemplary multi-tipped nozzle 10 applying three beads of material 15 to a surface 20 to which a flexible covering 30 is to be affixed. A typical use of the multi-tipped nozzle 10 is application of material 15 , e.g., adhesive, for installing cove base molding 30 . Referring now to FIGS. 1-4 , the nozzle 10 is shown in use attached to a dispensing device, partially shown at 40 . A hard cartridge, partially shown at 50 , containing material 15 to be dispensed is shown housed within the dispensing device 40 . The hard cartridge 50 that is used in conjunction with such dispensing devices 40 is of a standard size and configuration and comprises a front wall 31 , a back wall (not shown), and tubular body portion containing material therein to be dispensed. A hard cup-shaped movable plunger (not shown) is located at the rearward end of the hard cartridge 50 . The hard cartridge 50 includes its own dispensing nozzle 33 located at the forward end thereof. As best shown in FIG. 3 , the dispensing nozzle 33 of the hard cartridge 50 extends through an opening located in an end plate 41 at the front end of the dispensing device 40 as it extends within the proximal base portion 8 of the nozzle 10 . The moveable plunger provides means for the dispensing device 40 to apply dispensing pressure to the material within the cartridge 50 . When the cartridge 50 is appropriately registered within the dispensing device 40 , the moveable plunger is arranged to be moved in a forward ejecting direction towards the cartridge dispensing nozzle 33 to expel material from the cartridge 50 .
[0028] While the invention has been described in detail and with reference to specific examples thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
[0029] As shown in FIG. 1 , three of the five tips of the multi-tipped nozzle 10 are open and emitting material, and two of the tips remain closed.
[0030] FIG. 2 shows a multi-tipped nozzle 10 similar to the one shown FIG. 1 . As shown in FIG. 2 , three nozzle tips 11 remain in place over nozzle tubes 13 to prevent material 15 from being dispensed through those nozzle tubes, while two nozzle tips 12 have been cut to open those two nozzle tips 12 to allow material 15 to be dispensed therefrom. In an exemplary embodiment, the multi-tipped nozzle 10 is blow-molded high density polyethylene and the nozzle tips 12 are easily removed with a knife. In alternate embodiments (not shown), the nozzle tips are threaded and can be removed and replaced for applications where, for instance, the multi-tipped nozzle 10 will be used more than once.
[0031] Referring now to FIG. 3 , each of the nozzle tubes 13 is bent, placing the centerline 14 of the tips 11 and 12 at an oblique angle θ to the centerline 36 of the hard cartridge 50 . While the invention encompasses both straight nozzle tubes and bent tubes 13 , the configuration shown in FIGS. 1-3 is especially useful in that it provides a more comfortable positioning of the dispensing device 40 relative to the surface 20 on which the material 15 is to be applied, e.g., a vertical wall surface. The bent tubes 13 also afford easier access to tight areas that might not be accessible with straight tubes.
[0032] FIG. 3 clearly shows how, in this exemplary embodiment, the multi-tipped nozzle 10 includes a flange 16 located at a proximal base portion 8 of the nozzle 10 . The flange 16 is sandwiched between the end plate 41 of the dispensing device 40 and the front wall 31 of the hard cartridge 50 . FIG. 3 also shows the nozzle 33 of the hard cartridge 50 extending through a front opening in the dispensing device 40 and into the proximal base portion 8 of the multi-tip nozzle 10 . The force of the plunger (not shown) that forces material through the hard cartridge 50 forces the front wall 31 of the hard cartridge 50 against the nozzle flange 16 , which is in turn forced against the end plate 41 of the dispensing device 40 , thus holding the nozzle 10 firmly in place with respect to both the dispensing device 40 and the hard cartridge 50 . FIG. 4 is a cross section view of the nozzle 10 taken at section lines labeled 4 in FIG. 2 .
[0033] In an alternate embodiment, shown in FIGS. 5 and 6 , the nozzle 100 has external threads 116 at the inlet end that mate with internal threads (not shown) on the dispensing device 140 . In this embodiment, the nozzle 100 is screwed into the end of the dispensing device 140 . One application where this is practical is for dispensing devices adapted to accept bulk material not contained in a separate tube with a nozzle or for so-called “sausage” containers of material that do not have nozzles and which are simply opened at one end and the material forced out of the dispensing device, which comprises a complete cylinder with a plunger at one end and a threaded hole to accept the nozzle at the other end. Other types of nozzle-to-dispenser attachment means are also possible within the scope of the invention, including snap fit and twist and lock type fits.
[0034] Referring now to FIGS. 7 through 9 , there is shown therein a second alternative embodiment of the multi-tipped nozzle 200 of the present invention. As with the prior embodiments described herein, a typical use of the multi-tipped nozzle 200 is application of a viscous material, e.g., adhesive, for installing cove base molding. Industrial quality guns such as that shown in FIGS. 7-9 of the drawings are filled generally in two different manners. The first is by unscrewing a front cap 204 and engaging the front of the barrel 208 with a bulk container (not shown) of a viscous material, such as an adhesive whereupon the piston assembly is retracted rearwardly to draw in a charge of adhesive from the bulk container (not shown).
[0035] As shown in FIGS. 7 through 9 , the front cap 204 includes an internal thread and is arranged for screwing onto the externally threaded dispensing end of the barrel 208 . The front cap 204 includes a central opening 206 and a pair of opposed cutouts 207 extending radially from the central opening 206 . Prior to replacing the front cap 204 onto the barrel 208 filled with bulk material, the nozzle 200 is secured to the front cap 204 using a locking plate 212 . The locking plate 212 includes a centrally-located externally threaded shank 216 and opposed locking tabs 220 that extend radially from the threaded shank 216 . The threaded shank 216 is arranged to extend through the central opening 206 of the front cap 204 and into the proximal base portion 224 of the nozzle 200 ( FIG. 9 ). As best shown in FIG. 9 , the proximal base portion 224 of the nozzle 200 is internally threaded and arranged to threadably receive the externally threaded shank 216 . As the threaded shank 216 of the locking plate 212 is placed through the central opening 206 of the front cap 204 , and screwed into the nozzle 200 , the opposed locking tabs 220 of the locking plate 212 seat into the opposed cutouts 207 of the front cap 204 to lock the nozzle 200 to the front cap 204 . Thereafter, the front cap 204 , with the nozzle 200 locked thereon, may be replaced onto the barrel 208 and the dispenser is ready for use. As best shown in FIGS. 7 and 9 , the threaded shank 216 is hollow along its length to enable the passage of bulk material from the barrel 208 , through the threaded shank 216 and into the nozzle 200 during dispensing.
[0036] A second and more recently available method of filling the barrel with adhesive is by the use of what are known as “sausage” packages (not shown). These “sausage” packages are tube-like members formed generally of a thin plastic material such as mylar which is generally in the range of 2 mils thickness. Such packages are filled and are approximately the length of the barrel 208 and are clamped on or tied off at their ends by an appropriate clamp or tie. In use, the front cap 204 is unscrewed and the “sausage” package is inserted into the barrel 208 after the piston (not shown) is retracted. Thereafter, the end of the package closest the front cap 204 is cut open. The nozzle 200 is attached to the front cap 204 using the locking plate 212 in the manner described above and the front cap 200 is threaded back onto the barrel 208 . The operation of the gun is as in the conventional manner in that the hand actuator (not shown) drives the piston rod and piston assembly forward compressing and extruding the compound within the package through the nozzle 200 of the gun.
[0037] The multi-tipped nozzle 200 also includes a flange 228 arranged for being sandwiched between the end plate of a dispensing device and the front wall of a hard cartridge as described in connection with the first embodiment above. In this manner, the multi-tipped nozzle 200 in combination with the locking plate 212 of this embodiment provides versatility. That is, when it is desired to use the multi-tipped nozzle 200 for dispensing material in bulk form or from a collapsible package or sausage, the locking plate 212 may be utilized for fastening the nozzle 200 to the barrel front cap 204 prior to screwing the front cap 204 to the dispensing end of the barrel 208 . Alternatively, when it is desired to use the multi-tipped nozzle 200 for dispensing material from a cartridge, utilizing the flange 228 , the nozzle 200 may be sandwiched between the dispensing device end plate and the hard cartridge front wall. In this manner, the locking plate 212 is not utilized.
[0038] While the invention has been described in detail and with reference to specific examples thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof. For example, FIGS. 7-9 illustrate the flange 228 and locking plate 212 features being utilized in combination with a multi-tipped nozzle 200 . However, it should be understood that these features, i.e., the flange and locking plate, can also be incorporated into any nozzle of conventional or standard design. For example, referring now to FIGS. 10 and 11 , there is shown therein a third alternative embodiment of the 300 of the present invention, wherein the flange and locking plate features have been incorporated into a conventional ribbon bead nozzle for providing ribbon or flat beads of adhesive or caulking material.
[0039] Referring now to FIGS. 10 and 11 , the third alternative embodiment 300 includes a ribbon nozzle head 302 of conventional design and shape. The nozzle head 302 is arranged for dispensing a ribbon or flat bead of adhesive or caulking material having predetermined dimensions, e.g., a ⅛″×4″ ribbon bead. The embodiment 300 includes a front cap 304 including an internal thread (not shown). The front cap 304 is arranged for screwing onto the externally threaded dispensing end of the barrel 308 . The front cap 304 includes a central opening 306 and a pair of opposed cutouts 307 extending radially from the central opening 306 . Prior to replacing the front cap 304 onto the barrel 308 filled with caulking material or adhesive, the nozzle 300 is secured to the front cap 304 using a locking plate 312 . The locking plate 312 includes a centrally-located externally threaded shank 316 and opposed locking tabs 320 that extend radially from the threaded shank 316 . The threaded shank 316 is arranged to extend through the central opening 306 of the front cap 304 and into the proximal base portion of the nozzle 300 .
[0040] The ribbon nozzle 300 is internally threaded and arranged to threadably receive the externally threaded shank 316 . As the threaded shank 316 of the locking plate 312 is placed through the central opening 306 of the front cap 304 , and screwed into the nozzle 300 , the opposed locking tabs 320 of the locking plate 312 seat into the opposed cutouts 307 of the front cap 304 to lock the nozzle 300 to the front cap 304 . Thereafter, the front cap 304 , with the nozzle 300 locked thereon, may be replaced onto the barrel 308 and the dispenser is ready for use. As best shown in FIG. 10 , the threaded shank 316 is hollow along its length to enable the passage of bulk material from the barrel 308 , through the threaded shank 316 and into the nozzle 300 during dispensing. The ribbon nozzle 300 also includes a flange 328 arranged for being sandwiched between the end plate of a dispensing device and the front wall of a hard cartridge as described in connection with the first embodiment above. In this manner, the ribbon nozzle 300 including the locking plate 312 and flange 328 of this embodiment provides versatility. That is, when it is desired to use the ribbon nozzle 300 for dispensing material in bulk form or from a collapsible package or sausage, the locking plate 312 may be utilized for fastening the nozzle 300 to the barrel front cap 304 prior to screwing the front cap 304 to the dispensing end of the barrel 308 . Alternatively, when it is desired to use the ribbon nozzle 300 for dispensing material from a cartridge, utilizing the flange 328 , the nozzle 300 may be sandwiched between the dispensing device end plate and the hard cartridge front wall. In this manner, the locking plate 312 is not utilized. | A nozzle assembly for dispensing viscous material is disclosed. The nozzle assembly is convertible from use with a device for dispensing bulk viscous material to use with a device for dispensing viscous material from a cartridge. Alternatively, the nozzle assembly is convertible from use with a device for dispensing viscous material from a sausage package to use with a device for dispensing from a cartridge. When dispensing viscous material from a cartridge, the base portion is arranged for receiving the cartridge conical tip and the flange is arranged for placement between an end plate of the dispenser and the cartridge to retain said nozzle within said dispenser for dispensing viscous material from the cartridge. When dispensing viscous material in bulk form or from a sausage package, a locking plate is provided for tightly retaining the nozzle to the end cap of the dispensing device. | 1 |
This application claims the benefit of U.S. Provisional Application No. 60/363,943, filed Mar. 12, 2002.
BACKGROUND OF THE INVENTION
Plasticized polyvinyl butyral (PVB) sheet is used in the manufacture of laminate structures such as, for example: windshields for vehicles including automobiles, motorcycles, boats and airplanes; homes and buildings; shelving in cabinets and display cases; and other articles where structural strength is desirable in a glass sheet. In many applications, it is desirable that the laminate be transparent and colorless, or at least have very low color. Undesired or unintended color in a glass laminate can be a result of impurities from various sources. In some cases, color can occur in the PVB interlayer. Color in a PVB sheet can result from several sources in the PVB resin, or from the manufacturing process. For example, color can result from instability of the PVB resin, from impurities, or from other additives present in the PVB composition. Color in a PVB sheet can develop during storage of the PVB, or be caused by process conditions to which the resin is subjected.
Conventional PVB sheet typically includes a plasticizer in order to increase the flexibility and processibility of the PVB sheet. Generally, the higher the concentration of plasticizer, the more flexible the sheet. Various plasticizers are conventional in the manufacture of PVB, and include such plasticizers as: diesters of polyethylene glycols such as triethylene glycol di(2-ethylhexanoate) (3GO) and tetraethylene glycol diheptanoate (4G7), for example. These examples are not all-inclusive of known plasticizers useful for preparing PVB sheeting. Typically, plasticizer is included in amounts of greater than 30 parts per hundred (pph), based on the total weight of the resin. Depending upon the application, as well as other factors, highly plasticized PVB typically can have as much as 60 pph of plasticizer.
In a conventional PVB sheet manufacturing process, additives are typically included to protect PVB from developing color, to improve the manufacturing process, or to impart desirable properties or characteristics to the sheet. Examples of such additives are: antioxidants, such as octyl phenol for example; light stabilizers; surfactants; and adhesion control additives.
Manufacturers are continually looking for opportunities to improve the process or the properties of the product. For example, combinations of light stabilizers can be required for optimum performance in conventional PVB compositions. Conventional PVB sheet compositions can include, for example, Tinuvin® P, Tinuvin® 123 in addition to Tinuvin® 326 to obtain satisfactory light stability in the sheet. However, using combinations of light stabilizers can add additional expense and complexity to the manufacturing process, which is not desirable.
One other problem faced by PVB manufacturers is that changing one component or additive in the polymer recipe can affect the performance of other additives, or change the quality or performance of the final sheet. There can be totally unexpected problems or benefits that result from a change in the composition of a polymer recipe. For example, Applicants have discovered that the effectiveness of a particular antioxidant can be dependent upon the plasticizer used. For example, the Applicants surprisingly have found that antioxidants that are effective in combination with 4G7 as plasticizer are not as effective when using 3GO plasticizer.
It can be desirable to have a process for preparing a plasticized PVB sheet composition, whereby the color of the PVB sheet can be improved with the proper selection of additives. It is a further object of the present invention to have a process for manufacturing PVB that utilizes a plasticizer and a compatible antioxidant/additive package.
SUMMARY OF THE INVENTION
In one aspect, the present invention is a plasticized PVB sheet composition consisting essentially of: polyvinylbutyral having a hydroxyl (OH) number of from about 15 to about 20; a plasticizer or plasticizer mixture present in an amount of from about 30 parts per hundred (pph) to about 50 pph, based on the dry weight of the PVB resin; a surfactant; and optionally including either (i) a PVB bleaching compound, or (ii) an antioxidant and an ultraviolet (UV) light stabilizer, or (iii) both (i) and (ii), wherein the sheet has a yellowness index (YID) color of less than 12.
In another aspect the present invention is a process for preparing a low color, PVB sheet comprising the steps: (I) admixing polyvinyl alcohol, butyraldehyde, an acid or mixture of acids, water, and a surfactant (II) stabilizing the mixture obtained in step (I) by (a) raising the pH of the mixture to at least pH 10 (b) isolating the resin by draining the liquid, (c) washing the resin with neutral pH water; (III) plasticizing the PVB resin composition with from about 30 to about 50 pph of plasticizer based on the dry weight of the PVB resin; (IV) optionally mixing (a) a PVB bleaching compound and/or (b) an antioxidant and a UV light stabilizer with the PVB resin composition; and (V) extruding the PVB resin composition at a temperature of from about 175° C. to about 225° C. to obtain a PVB sheet having a glass transition temperature (T g ) of greater than about 32° C. and a YID of less than about 12.
In still another aspect, the present invention is a laminate article comprising at least one layer of plasticized PVB sheet, wherein the PVB sheet consists essentially of: polyvinylbutyral having a hydroxyl (OH) number of from about 15 to about 20; a plasticizer or plasticizer mixture present in an amount of from about 30 parts per hundred (pph) to about 50 pph, based on the dry weight of the PVB resin; a surfactant; and optionally including either (i) a PVB bleaching compound, or (ii) an antioxidant and an ultraviolet (UV) light stabilizer, or (iii) both (i) and (ii), wherein the sheet has a yellowness index (YID) color of less than 12.
DETAILED DESCRIPTION
In one embodiment, the present invention is a plasticized PVB sheet composition comprising from about 30 to about 50 pph of a plasticizer. PVB can be manufactured according to known processes. For example, U.S. Pat. No. 3,153,009 describes a process for commercial manufacture of PVB. U.S. Pat. No. 4,696,971 also describes a process for manufacturing PVB wherein sodium dioctyl sulfosuccinate (DOSS) is used as a surfactant.
The term flake, as used in the present invention, describes a particular physical form of PVB resin material, that is, granular or particulate versus a film or a sheet. The physical form of the resin does not necessarily indicate a different PVB composition within the present application, even though sheets and/or films may include additives not found in the resin flake.
A PVB of the present invention includes a plasticizer. Plasticizers of the present invention can chosen from any that are known or used conventionally in the manufacture of plasticized PVB sheeting compositions. For example, a plasticizer suitable for use herein can be a plasticizer or a mixture of plasticizers selected from the group consisting of: diesters obtained from the chemical reaction of aliphatic diols with carboxylic acids, including diesters of polyether diols or polyether polyols; and, esters obtained from polyvalent carboxylic acids and aliphatic alcohols. For convenience, when describing the sheet compositions of the present invention, a mixture of plasticizers can be referred to herein as “plasticizer”. That is, the singular form of the word “plasticizer” as used herein can represent the use of either one plasticizer or the use of a mixture of two or more plasticizers in a given sheet composition. The intended use will be apparent to a reader skilled in the art. Preferred plasticizers for use herein are diesters obtained by the reaction of triethylene glycol or tetraethylene glycol with aliphatic carboxylic acids having from 6 to 10 carbon atoms; and diesters obtained from the reaction of sebacic acid with aliphatic alcohols having from 1 to 18 carbon atoms. More preferably the plasticizer is either 4G7, 3GO or dibutyl sebacate (DBS). Most preferably the plasticizer is 3GO.
The composition of the present invention optionally includes at least one PVB bleaching compound. A PVB bleaching compound (bleaching compound) of the present invention is any compound that can reduce or eliminate color from a PVB sheet relative to the color of an otherwise identical composition, treated using an identical or similar process, with the exception that a bleaching compound is not present. The mode of the bleaching action demonstrated by the bleaching compound is not critical to the present invention. For example, a bleaching compound useful in the practice of the present invention can be a compound that reacts directly with color-forming compounds (color bodies) present in a PVB sheet composition, or a compound that is capable of yielding a compound that reacts directly with color-bodies. A bleaching compound can be a compound that can decompose in situ to yield decomposition products capable of reacting with color bodies present in a PVB sheet composition. A bleaching compound in the practice of the present invention can be a compound that inhibits the formation of color bodies. Bleaching compounds of the present invention include, for example, inorganic bisulfites such as sodium or potassium bisulfite; organic bisulfites such as tetramethylammonium bisulfite; and compounds similar in structure or function. Bleaching compounds also include sulfosuccinates such as dialkyl sulfosuccinates. For example, the present invention can include DOSS as a bleaching compound.
A bleaching compound of the present invention can be included in any effective finite amount. An effective amount for the purposes of the present invention is any amount that reduces the color of a PVB sheet relative to the color of an identical or substantially similar PVB sheet composition without the bleaching compound. Color measurement can be done according to any conventional standard practice. Alternatively, in the absence of comparative data, an effective amount is any amount that reduces the color of a PVB sheet to a yellowness index (YID) of less than about 12 YID. Preferably the YID is less than about 10, more preferably less than about 8, and most preferably less than about 6.
A bleaching compound can be included in an amount of from about 0.01 to about 0.85 pph, based on the weight of polyvinyl alcohol (PVA) used in the preparation of PVB. Preferably, the bleaching compound is present in an amount of from about 0.05 to about 0.80 pph, more preferably in an amount of from about 0.10 to about 0.75 pph, and most preferably in an amount of from about 0.15 to about 0.70 pph. While color reduction in a PVB sheet is an important consideration, the amount of bleaching compound included will also be a function of the cost of production and the other properties that may be affected by including the additive.
The present invention includes a surfactant. A surfactant suitable for use herein can be any that is known to be useful in the art of polyvinylbutyral manufacture. For example, surfactants suitable for use herein include: sodium lauryl sulfate; ammonium lauryl sulfate; sodium dioctyl sulfosuccinate; ammonium perfluorocarboxylates having from 6 to 12 carbon atoms; sodium aryl sulfonates, adducts of chlorinated cyclopentadiene and maleic anhydride; partially neutralized polymethacrylic acid; alkylaryl sulfonates; sodium N-oleyl-N-methyl taurate; sodium alkylaryl polyether sulfonates; triethanolamine lauryl sulfate; diethyl dicyclohexyl ammonium lauryl sulfate; sodium secondary-alkyl sulfates; sulfated fatty acid esters; sulfated aryl alcohols; and the like. Preferable surfactants include sodium lauryl sulfate, sodium dioctyl sulfosuccinate, sodium cocomethyl tauride, and decyl(sulfophenoxy)benzenesulfonic acid disodium salt.
The surfactant can be included in any effective amount for the particular set of process conditions practiced. The surfactant can be included in an amount of from about 0.01 to about 0.85 pph by weight, based on the weight of PVA used to prepare PVB. Preferably the surfactant is included in an amount of from about 0.10 to about 0.80 pph. More preferably, the surfactant is included in an amount of from about 0.15 to about 0.75 pph. Most preferably, the surfactant is included in an amount of from about 0.15 to about 0.70 pph.
The surfactant and the bleaching compound can be the same compound, or can perform both functions. The bleaching compound is optional only in the event that the surfactant can also perform the function of a bleaching compound. Otherwise the bleaching compound is considered to be essential in the practice of the present invention. For example, DOSS can be used in the practice of the present invention as a surfactant. DOSS can also be a bleaching compound in the practice of the present invention. In one particularly preferred embodiment, DOSS can be included as both a surfactant and as a bleaching compound. In this embodiment, the use of a bleaching compound other than DOSS is optional.
Antioxidants can be optionally included in a PVB resin composition of the present invention during sheet preparation to inhibit the oxidation of the PVB resin and/or components. Preferred antioxidants are known conventionally and available commercially. Most preferred are bis-phenolic antioxidants, which are surprisingly more suitable for preparing low color PVB sheeting, particularly when 3GO is used as plasticizer. Bis-phenolic antioxidants are available and can be obtained commercially. Suitable bis-phenolic antioxidants include 2,2′-ethylidenebis(4,6-di-t-butylphenol); 4,4′-butylidenebis(2-t-butyl-5-methylphenol); 2,2′-isobutylidenebis(4,6-dimethylphenol); and 2,2′-methylenebis(6-t-butyl-4-methylphenol), for example. Bis-phenolic anti-oxidants are commercially available under the tradename of ANOX™ 29, LOWINOX® 22M46, LOWINOX® 44B25, and LOWINOX® 22IB46, for example.
An antioxidant can be included in any effective finite amount. Preferably, the antioxidant is included in an amount of from about 0.01 to about 0.6%, based on the total weight of the sheet. More preferably, the antioxidant is present in amount of from about 0.03 to about 0.3%, most preferably in an amount of from about 0.05 to about 0.25%.
Other additives are known conventionally to be useful, and can be included in a resin composition of the present invention. Such additives include: light stabilizers, particularly UV light stabilizers, such as Tinuvin® P; Tinuvin® 326, and Tinuvin® 123. UV light stabilizers can stabilize the PVB composition by absorbing ultraviolet light and preventing unwanted effects by the UV light on the PVB. Adhesion control agents such as alkali and alkaline earth metal salts of carboxylic acids, alkaline earth metal salts of inorganic acids, or a combination of such salts can be added. Surface tension controlling agents such as Trans® 290 or Trans® 296 available from Trans-Chemco; or Q2-3183A® available from Dow Chemical can be used in the practice of the present invention. The use of Trans® 290 or Trans® 296 is preferred.
A PVB resin of the present invention can be obtained by processes known in the art of PVB manufacture. PVB resins used in the practice of the present invention can be prepared by mixing PVA with butyraldehyde in an aqueous medium in the presence of an acid or mixture of acids, at a temperature of from 5° C. to 100° C.
Typically, the ratio of PVA to butyraldehyde can be chosen such that the PVB has residual hydroxyl functionality, conventionally reported as OH number. Residual hydroxyl functionality can vary according to what properties are desirable in the PVB. The relative amounts of butyraldehyde and PVA required to obtain the desired OH number in the PVB resin will be readily apparent to those skilled in the art of PVB manufacture. In the practice of the present invention residual hydroxyl can be in the range of from about 14 to about 30. Preferably, the OH number is from about 15 to about 25. More preferably, the OH number is from about 15 to about 20, and most preferred in the practice of the present invention is PVB resin having an OH number in the range of from about 17 to about 19. The OH number can be determined according to standard methods such as ASTM D1396-92.
In a preferred embodiment, a low color PVB resin of the present invention can be obtained by a process comprising the steps: (I) admixing polyvinyl alcohol, butyraldehyde, an acid or mixture of acids, water, and a surfactant (II) stabilizing the mixture obtained in step (I) by (a) raising the pH of the mixture to at least pH 10 (b) isolating the resin by draining the liquid, (c) washing the resin with neutral pH water; (III) plasticizing the PVB resin composition with from about 30 to about 50 pph of plasticizer based on the dry weight of the PVB resin; (IV) optionally mixing (a) a PVB bleaching compound and/or (b) an antioxidant and a UV light stabilizer with the PVB resin composition; and (V) extruding the PVB resin composition at a temperature of from about 175° C. to about 225° C. to obtain a PVB sheet having a T g of greater than about 32° C. and a YID of less than about 12.
The steps of the process described herein can be carried out in varied order. For example, while it can be necessary to carry out step (I) before step (II) it is not essential, for the purpose of obtaining a low color sheet of the present invention, that steps (III) or (IV) be carried out in any particular order. Although it may be preferable to implement these steps just prior to, or simultaneous with, step (V). Also, the order of addition of components is not critical in the practice of the present invention, although a skilled artisan will recognize that there may be other benefits of carrying out the process in a consistent and ordered manner. For example, plasticizer can be mixed with the PVB either before or during the extrusion of the PVB composition, as described in U.S. Pat. No. 5,886,075.
Plasticizer can be added in any amount desirable to obtain a plasticized PVB sheet. Plasticizer can be added in an amount of from about 30 to about 50 pph, based upon the total dry weight of the resin. The “dry weight” as used herein refers to the weight of the dry resin, that is, after water has been removed from the resin. Preferably the plasticizer is present in an amount of from about 30 to about 45 pph, and most preferably in an amount of from about 32 to about 45 pph.
Plasticization can be carried out using either a “wet” process or a “dry” process. The wet process, as the term is used herein, is a process whereby the plasticizer is mixed with a PVB resin aqueous slurry, together with other additives, prior to, or as, the mixture is fed into an extruder. A residence time of from 2 to 24 hours for the plasticizer/PVB mixture can be preferred prior to sending the mixture to an extruder. A wet process suitable for use herein is described in U.S. Pat. No. 3,153,009, for example. A dry process, as the term is used herein, is a process whereby the plasticizer is mixed with the dry PVB resin flake prior to, or as, the mixture is fed into an extruder. A dry process suitable for use herein is described in U.S. Pat. No. 5,886,075, for example.
The T g of a PVB sheet of the present invention, as measured by Dynamic Mechanical Analysis (DMA) is dependent upon the concentration of plasticizer included in the composition. In the practice of the present invention, a sheet has a T g of from about 32° C. to about 50° C. Preferably, the T g is from about 33° C. to about 47° C., and more preferably from about 35° C. to about 45° C.
A low color PVB resin sheet suitable for the purposes herein can be obtained by a process that comprises the steps of: (1) isolating PVB flake from a PVA/butyraldehyde reaction mixture previously described herein; (2) optionally admixing an antioxidant and a UV light stabilizer with the plasticizer to obtain a plasticizer/additive mixture (plasticizer mixture); and (3) co-extruding the flake, plasticizer, antioxidant, and UV light stabilizer, or alternatively co-extruding the flake and the plasticizer mixture at a feed ratio of plasticizer mixture to dry of flake from about 30:100 (wt:wt) to about 50:100 (wt:wt) at a temperature of from about 175° C. to about 225° C. to obtain a low-color PVB resin having a YID of less than about 12. It is preferable to admix the antioxidant/UV light stabilizer with the plasticizer prior to extrusion of the resin.
EXAMPLES
The following Examples and comparative examples are presented to further illustrate the present invention. The Examples are not intended to limit the scope of the invention in any manner, nor should they be used to define the claims or specification in any manner that is inconsistent with the invention as claimed and/or as described herein.
The following tests were used in the examples and comparative examples below.
Hydroxyl number: ASTM D 1396-92.
Sheet yellowness index (YID): A chip is made with 21.0 grams of sheet, and heat pressed into a 10.0 mm thick disk of 50.8 mm diameter. Chip preparation involves preheating a stack of 50.8 mm disks cut from the sheet in a mold for one minute at 2200 N force and 185° C., then increasing the pressing force to 32,000 N at 185° C. for two minutes, and cooling under the same force for 7.5 minutes. No residual surface pattern that was on the extruded sheet is visible in the chip. Yellowness index was determined per ASTM D1925-70 on the 10.0 mm thick chip.
Flake Yellowness Index (YID)
A “chip” specimen is made from 21.0 grams of dried PVB resin (aka flake). Flake moisture should be less than 0.2% prior to chip preparation. The dried flake is heat pressed into a 1-cm thick, 5.08-cm diameter circular chip. Chip preparation involves hot pressing a the 21.0 grams of dried PVB resin as follows:
Press Cycle Time (min) Temp. ° C. Force (N) a. Pre-heat 1.5 180 2220 b. Cure 2. 180 86700 c. Cool 8.0 86700
The thickness of the chip is measured and recorded and the yellowness index (YID) is then determined per ASTM D1925.
Glass Transition Temperature—T g is determined by DMA using the procedure of ASTM D4065, using the tangent delta at 1 Hz.
Example 1
Poly(vinyl butyral) sheet was prepared as follows: at 90° C., a mixture comprising 32 parts by weight of poly(vinyl alcohol) of average degree of polymerization 618 and 99.5% hydrolyzed and 68 parts by weight of PVA of average degree of polymerization 1005 and 99.5% hydrolyzed was dissolved in 615 parts by weight of demineralized water. To this solution was added 1 part by weight of 88% para-toluene sulfonic acid and enough sulfuric acid to bring the dissolved PVA solution to a pH of 2. Using the procedure described in U.S. Pat. No. 3,153,009, 62 parts by weight of n-butyraldehyde and 0.47 parts by weight of 70% DOSS and the PVA solution were charged into a vessel maintained at 90° C. After a one hour hold time, a Blurry was obtained and the slurry was stabilized with a sodium hydroxide solution to raise the pH to 11. Concurrent with the stabilization, 0.07 parts by weight Trans® 290 surface tension stabilizing agent was added. The slurry was then washed and cooled with demineralized water. A granular, white PVB resin with residual hydroxyl number of 18.6 and flake YID of 8.8 was obtained. The flake was mixed with 3GO plasticizer containing 4 grams per liter of Tinuvin® P and 8 grams per liter of Lowinox® 44B25 antioxidant and was extruded so that the residence time in the extrusion system was about 15 to 25 minutes. The feed rate ratio of plasticizer to dry flake was 35:100 (wt:wt). Potassium formate solution was injected so as to deliver a potassium concentration of 10 parts per million (ppm) in the sheet. Melt temperature measured at the slot die was between 210 and 215° C. Sheet YID was 5.85.
Comparative Example C1
PVB flake was prepared as in Example 1 except that 0.4 parts by weight of sodium lauryl sulfate was used in the place of DOSS as the surfactant, and no other surface tension modifiers were added. A granular, white PVB resin with residual hydroxyl number of 18.6 was obtained. Using the flake made with sodium lauryl sulfate as described here, sheet was prepared as in Example 1. Melt temperature measured at the slot die was between 210 and 213° C. Sheet yellowness was 25.05.
Comparative Example C2
Flake and sheet were made as in Example C1, except that 4 grams per liter of octylphenol was used in the place of Lowinox® 44 B25 as antioxidant in the plasticizer, and the potassium level was 300 parts per million (ppm). Sheet yellowness index was 13.57. | The present invention is a low-color plasticized PVB sheet and a process for preparing the same. The sheet of the present invention yields a YID measurement of less than 12. A sheet of the present invention is useful for making glass laminates that are useful in cars, boats, trains, buildings, and display cases, for example. | 2 |
This application is related to application Ser. No. 845,590, filed Oct. 25, 1977, now abandoned, and to the continuation-in-part thereof, Ser. No. 888,625, filed Mar. 21, 1978, now U.S. Pat. No. 4,165,657.
BACKGROUND OF THE INVENTION
This invention relates to a multistage automatic planetary transmission gearing suitable for motor cars, particularly passenger cars, with the changing of gear stages being effected by centrifugal multiple plate disk clutches.
Known multistage automatic transmission gearings in which gear stages are changed by means of centrifugal clutches are simple, but their operating properties are not fully satisfactory, particularly at the beginning of gear stage changing at uniform speed of the vehicle without regard to load, and also the mutual dependence of the first phase of gear changing between the speed v 1 to v 2 (v 1 being the speed at which a forceless contact of friction parts of the clutch occurs, and v 2 being the speed at which the gear change clutch transmits a part of the torque) and in the second phase of gear stage changing within the range of speeds v 2 to v 3 (v 3 being the speed at which a rigid coupling of the gear change coupling takes place) the second phase of changing taking place at a reduction of the revolutions of the engine from n 2 to n 3 . The steepness of the function n 2 -n 3 in dependence on time must not jeopardize the continuity of changing; wherein the range of speeds v 1 to v 3 , where the efficiency of transmission of power is reduced due to slippage of the gear change clutch, inefficiency should not increase proportionally. These prior transmission gears are not suitable for more than two speed stages.
In automatic planetary transmission gearing in which the gear changing is accomplished by oil controlled clutches in the first and second phase of changing on the continuity of changing within a chosen narrow speed range v 1 to v 3 are eliminated by a hydrodynamic starting clutch, or by a hydrodynamic torque converter, at the price of a reduced efficiency of power transmission within the whole speed range of the vehicle except for the highest speed stage if the hydrodynamic element is at the highest speed stage, and at the price of higher costs and complexity of the transmission gear if the hydrodynamic element is connected to the highest speed stage. In the latter case fuel consumption is affected unfavorably and the operating properties are secured by rather hydraulic complicated and in recent times also electronic control means, the parts of which are costly and demanding as to technology and service.
SUMMARY OF THE INVENTION
It is an object of this invention to provide an automatic multistage planetary transmission gearing, wherein the said drawbacks in the course of gear changes are for the major part eliminated, and which is less expensive and more easily manufactured than actually used in prior transmission gearings of the same general type.
According to this invention the drum of the gear change clutch in each stage containing a planetary transmission gearing unit, such drum being firmly connected to the output gear of the planetary gearing, is provided with a mechanism for feedback coupling, comprising an output part, a regulating part and a rest stop. The output part comprises carrier arms, firmly connected to the input gear of the following planetary gear unit or to the output shaft of the transmission gearing, and an output arm of swinging carriers, suspended on bolts fixed to the drum of the gear change clutch. The contact faces on the output arms of said swinging carriers engage carrier arms so, that due to the force transmitted via the output arms to the carrier arms according to the magnitude of the torque at the output of the planetary gear unit in question, or of following planetary gear units, the effect of the centrifugal force of centrifugal weights and of guiding arms of the swinging carrier is reduced, thus controlling the regulating part so that increased slippage through the gear change clutch then takes place. The regulating part comprises centrifugal weights guided by guiding arms of swinging carriers, a controlled disk, and a return spring, by the action of which the centrifugal weights are clamped between an inclined surface of the controlled disk and the drum of the gear change clutch.
Among the advantages of the multistage automatic planetary transmission gearing according to this invention are its simplicity and low manufacturing costs, as well as advantageous operating characteristics.
DESCRIPTION OF THE DRAWINGS
The attached drawings illustrate a preferred embodiment of the invention together with a diagram indicating its properties in operation.
FIG. 1 shows the course of transmitted driving forces P H , of the driving resistances P f +P w , of the speed of revolution n of the motor and of the efficiency in dependence on the speed v of the vehicle for a four-stage transmission gearing;
FIG. 2 is a view in longitudinal axial section of an embodiment of the gearing of this invention for a two-stage automatic planetary transmission gearing; and
FIG. 3 is a view in cross section of the gearing showing in elevation the feedback coupling, the section being taken generally along line 3--3 in FIG. 2.
DESCRIPTION OF PREFERRED EMBODIMENT
FIG. 1 shows the resultant courses of the driving forces for different throttling of the engine fuel for a narrow range of speeds of the transmitted power at reduced efficiency, where the efficiency η (eta) is reduced from the value η=1 on the curve P pk to the value η=i k /[i (k-1)] on the curve P IIk at a speed of v 2 , whereby the driving forces shown on curve P IIk cannot equalize the driving resistances at an efficiency other than η=1, as the course of P IIk increases with a higher speed of the vehicle more steeply than the course of the driving resistances P o =(P f +P w )+P z , where P z is an increase of driving resistances due to wind or upgrade driving. At the lowest efficiency η, (for instance for driving resistances P o1 at full load of the motor at a speed v 24 ) driving is possible only theoretically, as substantially increased driving resistances P o1 at a high speed v 24 =128.6 km/h of the vehicle could be overcome solely on a long straight road with a uniform incline; at higher efficiency a slight reduction of driving resistances, on the other hand, would cause an equalization of driving resistances with driving forces at a higher speed, namely v o , where the efficiency of transmission of power η=1, and the vehicle has in the fourth transmission stage at the reduced speed v 34 a reserve of driving power for overcoming increased driving resistances P O2 . Thus the range of speeds of the vehicle v 24 to v 34 for a constant opening of the throttle is not stable, and a constant speed can be achieved within this range only by a reduction of the supply of fuel to the engine and at an efficiency of 100%.
Theoretically a heating of the gear change clutch and a reduction of the coefficient of friction takes place in case of a longer drive at the speed v 24 , in consequence thereof the constant of the gear change clutch is reduced to k s4z and the coefficient of feedback coupling is reduced to x 4z -(k s4z ,/k s3 ) so that with changed courses of forces of the I phase P Iz4 and of the II phase P IIz4 , the driving resistances equalize with the driving force P Iz4 at a slightly increased speed v z and with an increased efficiency η. In addition, the mutual independence of the courses of the I and II transmission phases do not require any solution of the continuity of gear change by the introduction of a hydrodynamic element in front of the transmission gearing, a simple centrifugal starting clutch being sufficient. Such starting clutch slips solely within the narrow range of speeds from o to v s , whereby for a reduced load the speed v s drops along the curve P s . At a speed higher than v s the starting clutch is rigidly connected, which equally contributes to a reduction of fuel consumption and, with the exception of the speed range in the course of gear change at load, where the efficiency of transmission of power is automatically reduced, the multistage automatic planetary transmission gearing does not worsen the dynamic properties of the vehicle. The courses of P pk and P IIk secure the so-called "kick-down effect" (an automatic gear change to a lower speed stage at sudden actuation of the gas pedal, for instance, in case of overtaking) within an arbitrary speed range, limited solely by the courses of P vk , as it is, for instance, possible to select the speed v p14 so that a sudden actuation of the gas pedal causes a gear change from the fourth to the first speed stage. Another advantage is, that in case of a selection of ##EQU1## any value of the torque is transmitted from the transmission gearing at a speed surpassing v p14 via the fourth speed stage; for a suitable selection of v p14 this is advantageous for an emergency starting of the motor by towing the vehicle, or possibly in going down-slope without any other arrangement, since the driven part of the starting clutch is provided with centrifugal weights. These in addition reduce the speed of the vehicle, the starting clutch being rigidly connected without reduction of the achievable force in the course of starting, resulting in a reduction of fuel consumption, particularly when driving in a town.
FIG. 1 shows only the part of the course of the efficiency where it drops in the course of gear change due to slipping of the gear change clutch. The transmission ratios i k of individual stages have been chosen as follows:
i 1 =3.52
i 2 =2.23
i 3 =1.4
i 4 =1
The courses of driving forces P H and of the speed of revolution n of the motor are shown in full lines for a fully open throttle condition, by a dash line for a partly open throttle condition, and by a dot-dash line for a minimum opening of the throttle, in which, in the case of a drive at level without a wind a gear change from the third to the fourth speed stage takes place. The course of the driving force P Ik in dependence on the speed of the vehicle at gear change to the k th transmission stage in the I phase of gear change is determined by the equation: ##EQU2## where: P v (k-1) is the course of the driving force to the (k-1) st speed stage from the torque of the motor in dependence on the speed v of the vehicle,
k sk is the constant of the clutch of the k th stage,
P 2K is the driving force of the k th transmission stage at the speed v 2K at the end of the I phase of gear change and at a speed of revolution n 2 of the motor, and
x k is the coefficient of feedback coupling characterizing the change ΔP s of the driving force transmitted by the gear change clutch at a change ΔP of the driving force at the output of the planetary transmission gear, so that
ΔP.sub.s =ΔP·x.sub.k
The course of the driving force P IIk in the course of the II phase of gear change in dependence on the speed v of the vehicle is: ##EQU3##
The course of the driving force P pk , where the I phase of gear change starts at a speed v is: ##EQU4## where v pk is the speed at which the I phase of gear change starts at zero load.
The physical significance of the constant k sk of the gear change clutch follows from the equation: ##EQU5## v Itk is the speed of the vehicle, where the I phase of gear change would proceed at k sk , P 2k and v 2k without action of the feedback coupling. The constant of the clutch is determined by the equation: ##EQU6##
The efficiency of transmission of power in the I phase of gear change is: ##EQU7##
The efficiency of transmission of power in the II phase of gear change is ##EQU8##
For a better determination of the courses of P pk , P Ik and P IIk the following parameters have been chosen:
2. speed stage v 22 =51.2 km/h v p2 =23 km/h x 2 =0.65
3. speed stage v 23 =80.6 km/h v p3 =36 km/h x 3 =0.65
4. speed stage v 24 =128.6 km/h v p4 =50 km/h x 4 =0.65
Turning now to FIGS. 2 and 3, there is there shown a two-stage automatic transmission gearing in accordance with the invention. Such gearing which is shown as constituting one assembly unit, is interposed between the crankshaft 13 of an automobile engine and an output shaft 9, the transmission gearing shown in FIG. 2 having two similar stages A and B connected in series. The same reference characters are employed for designating corresponding parts in the two stages.
Driving power is transmitted from the crankshaft 13 via a conventional starting centrifugal friction clutch 14, clutch 14 being interposed between fly wheel 15 secured to the crankshaft 13 and a driven disc 16, coaxial of the fly wheel. The disc 16 is mounted for rotation with respect to a free shaft 35 which is mounted in the transmission gearing housing coaxial of the crankshaft 13. The disc 16 has a sleeve-like hub which extends to the right in FIG. 2, such hub having affixed thereto the input gear 7 of the planetary transmission gearing unit 4 of stage A. Gear 7 is in constant mesh with the left-hand gear of the composite planetary gearing unit 4, unit 4 being mounted for rotation upon a stub shaft 40 which is fixedly secured at its left-hand end to a carrier 19 which is mounted for rotation in one direction only about the shaft 35. The carrier 19 is locked against reverse rotation by a free-wheeling or one-way clutch 20. Extensions 30 of the fixed part 31 of the one-way clutch 20 are engaged in longitudinally extending recesses 32 of the housing 33 of the transmission gearing. The fixed part 31 of the one-way clutch 20 is guided in the radial direction by a circular cylindrical surface 34 of the clutch 20.
A drum 1 is supported coaxial of the shaft 35 for rotation thereabout on a disc 39. Within the drum 1 there is disposed a multi-plate gear change clutch 2 which has a plurality of alternating carrier discs 21 and driven discs 22. The carrier discs 21 rotate with carrier 19, being axially slidable with respect to a part 19' of the support 19 and being rotatable therewith about the shaft 35. The driven discs 22 are drivingly connected to the drum 1, the torque transmitted through clutch 2 between support 19 and the drum 1 being controlled by axial adjustment of a controlled disc 27 which is constantly urged in a clutch-disengaging direction to the right by a dished spring 26.
A mechanism 23 is provided in each of stages A and B to furnish power feedback coupling between such stage and the succeeding stage or the output shaft 9 of the transmission, as the case may be. Mechanism 23 comprises an output part 24 having three radially outwardly erected equally angularly spaced arms 10, as shown in FIG. 3. Mechanism 23 also comprises a plurality of regulation parts 5 (three shown), and a rest stop 28 for each of parts 5. Each part 5 is pivotally mounted by a pivot pin 12 upon the disc-like member 39 to the outer edge of which the drum 1 is integrally connected. The rest stops 29 are also mounted on the member 39. The output part 24 of stage A is fixedly connected to the input gear 7 of stage B; the output part 24 of stage B is connected to the output shaft 9 by a suitable coupling, as shown.
Each of the regulation parts 5, which is in the form of a bell crank, has a first, short generally radially directed arm 36 having a recess with opposed surfaces 11, such recess receiving the rounded end 25 of the respective arm 10 of output part 24. As shown in FIG. 2, the outer ends of arms 10 extend through windows 38 in the member 39. The other arm 37 of the regulation member 5 extends generally circumferentially of the member 39 and within the drum 1, adjacent the outer end of the arm 37 of each of members 5 there is a seat within which is rotatably mounted a centrifugal weight in form of a ball 6. When the apparatus shown in FIGS. 2 and 3 is at rest, the outer ends of the arms 37 of members 5 is in engagement with its respective rest stop 28.
As shown in FIG. 2 each ball 6 is interposed between a radially elongated annular seat 41 in the inner surface of the member 39, and a seat 29 in the right-hand end of the controlled disc 27. The seat 29 is inclined to the right in a radially outward direction, so that as the balls 6 swing outwardly under the influence of centrifugal force when the mechanism is in operation, an increased speed of rotation of the part 10 causes the balls 6 mounted thereon to travel radially outwardly, thereby further compressing the stack of discs 21, 22 of the clutch 2, and thus decreasing the slippage through the clutch between the support 19 and the drum 1.
In accordance with the present invention, not only is the radial position of the balls 6 responsive to changes in speed of rotation of the drum 1, but it is also responsive to the opposing force exerted upon each respective swinging carrier 5 by engagement between the outer end 25 of the respective arm 10 and the surfaces 11 on the arm 36 of carrier 5. It will be seen that such two forces, centrifugal force on the one hand and the torque exerted upon each swinging carrier 5 by the respective arm 10 of the output part 24, oppose each other. It will also be seen that the return spring 26 tends to urge the balls 6 radially inwardly with respect to the shaft 35 by reason of the direction of inclination of the seat 29 in the controlled disc 27. Thus, due to the force transmitted by the output arm 36 to the carrier arms 10 according to the magnitude of the torque at the output of the planetary gearing or of following planetary gearings of following stages, the effect of centrifugal force upon the weights 6 and thus of guiding arms 37 of the swinging carriers 5 is reduced as such torque increases, thereby controlling the regulating parts 5.
Although the invention is illustrated and described with reference to one preferred embodiment thereof, it is to be expressly understood that it is in no way limited to the disclosure of such a preferred embodiment, but is capable of numerous modifications within the scope of the appended claims. | Multistage automatic planetary transmission gearing, particularly suitable for passenger cars, using for improvement of conditions in the course of gear changes a mechanism of feedback coupling, comprising an output part, a regulating part and a rest stop. | 5 |
FIELD OF THE INVENTION
The present invention is directed to a cam guided corneal trephine used to cut a circular or non-circular (or other than round) portion of the cornea.
BACKGROUND OF THE INVENTION
Corneal trephines have been used in lamellar and penetrating keratoplasty. Originally, such trephines have been in the form of a honed cylinder as developed by Castroviejo. Many surgeons have attempted to improve the techniques as developed by Castroviejo, see U.S. Pat. No. 4,423,728. Many surgical companies have attempted to make holders for such cylinders in order to improve the visualization of the cutting edge but such attempts have generally been insufficient due to lack of proper centering, obscuration of the cutting edge at sometime during the procedure, independent eye and trephine movements, and lack of ability to cut other than round windows in the corneal tissue.
An improved corneal trephine was developed by David M. Lieberman, M.D., as described in the American Journal of Ophthalmology, May, 1976, pages 684-685. As described therein, the surgical instrument was comprised of inner and outer cones, the inner cone revolving within the outer cone. The outer cone included an upper ridge held by the non-dominant hand of the surgeon, stabilizing the instrument on the eye, and a lower ridge containing an annular suction device which firmly held the eye with a pressure of from 10-15 mm Hg to assure centration of the device over the cornea. The inner cone revolved within the outer cone and carried a slide mechanism with an attached disposable razor blade. To perform the incision, the inner cone which carried the blade was rotated about the cornea. After each rotation, the blade was lowered a few thousandths of an inch by turning a screw and the inner cone was rotated again. The incision could be viewed through an operating microscope. The slide mechanism upon which the blade was mounted was controlled by an adjustment screw for varying the radial position of the blade. Two interchangeable cutters could be used, one at a time. The first provided the razor blade at a 20° angle. The second cutter mechanism held the blade vertically and was suitable for keratoplasty in which a donor cornea had been punched for reinsertion onto a patient's cornea.
Although the single trephine described above represented a significant advance in the art, the device could only provide a round cut and, consequently, could not be employed whenever an other than round incision was required.
A second improved corneal trephine was developed by David M. Lieberman, M.D., and is disclosed and claimed in U.S. Pat. No. 4,423,728 which disclosure is hereby incorporated herein by reference. The advantages of this trephine include the use of a circular or non-circular cam which guides the path of the cutting blade to provide either a circular or other than round cut of the cornea. As described therein, the surgical trephine comprises a base, a non-circular cam guide operatively connected to the base, and a rotation cone adapted to be disposed and rotated on the base, the rotation cone having a blade mounting means provided thereon. The blade mounting means includes a slide mechanism with an attached disposable razor blade and is further provided with a slave wheel which rides on the non-circular cam guide such that upon rotation of the circular rotation cone the blade means provides a cut of the cornea following the pattern of the annular cam guide. The razor blade is connected to the blade mounting means through a vertical adjustment screw such that upon adjustment of the screw, the blade could be moved vertically to control the depth of cut of the blade into the corneal tissue.
The above device was also provided with an angled blade mounting means which operated similarly to the vertical blade means to provide a cut within the corneal tissue in an other than vertical manner.
And, while the cam-guided trephine device described above and in U.S. Pat. No. 4,423,728 represented a significant advance in the art over the single point trephine described in the David M. Lieberman article, the cam guided trephine could still be improved. Specifically, the razor blade had a tendency to wobble during rotation of the blade, and the depth of cut of the cornea was difficult to accurately control. Further, since the complete cutting action of the corneal tissue was interrupted after each rotation of the blade means to incrementally lower the cutting blades, the cornea lamella is allowed to spread providing an uneven incision or "hour-glass" effect. Further, the process of making a complete cut through the corneal tissue was very slow. And, further, the sudden incremental lowering of the cutting blade for each new rotation of the blade means tended to displace the corneal tissue and thereby producing an uneven cut.
SUMMARY OF THE INVENTION
It is therefore an object of the invention to provide a cam-guided corneal trephine which overcomes the disadvantages of the prior art trephines.
It is a further object to provide a cam-guided corneal trephine having an interchangeable blade means providing either a vertical or angled cut with respect to the corneal surface of the eye.
It is a further object of the invention to provide a cam-guided corneal trephine which includes a blade which can provide either a "round" or "other than round" cut of the cornea.
It is a further object of the invention to provide a cam-guided corneal trephine which includes a cutting blade and roller cage assembly that will decrease any wobble during rotation of the roller cage assembly within an interchangeable cam. The cams can have either an inner round cam guiding surface or an inner non-round cam guiding surface to allow the cutting blade to cut either a round or other than round hole in the corneal tissue.
It is a further object of the invention to provide a cam-guided corneal trephine which includes an inner adjusting ring which supports the roller cage assembly and cutting blade to provide a course blade height adjustment relative to the surface of the corneal tissue.
It is a further object of the invention to provide a cam-guided corneal trephine which includes a roller cage assembly supporting a cutting blade which provides a continuous cutting action during rotation of the roller cage assembly to provide a smooth, uninterrupted cut of the corneal tissue.
And, it is a further object of the invention to provide a cam-guided corneal trephine which includes a blade holding means supporting a cutting blade which continuously advances the cutting blade towards the corneal tissue of the eye during rotation of the blade holding means to provide a smooth uninterrupted cut of the corneal tissue without wobble or deflection of the cutting blade.
In accordance with the above objects, a novel cam-guided corneal trephine device is provided herein The cam-guided corneal trephine comprises a base, a course adjusting ring, interchangeable annular cams operatively supported by the adjusting ring, the annular cams having various inner round diameters or other than round dimensions, and a roller cage assembly adapted to be disposed and rotated within the annular cam, the roller cage assembly having a blade mounting means disposed therein for providing a cut of the corneal tissue corresponding to the inner shape of the selected cam upon rotation of the roller cage assembly.
The blade mounting means provides a continuous adjustment of the blade height or blade advancement upon rotation of the roller cage assembly while grasping the end of the blade mounting means. This continuous blade advancement is accomplished by use of a differential thread arrangement provided within the blade mounting means to allow the tip of the blade to advance downwardly 0.096 mm per revolution of the roller cage assembly and blade mounting means as is further described below.
More specifically, the roller cage assembly includes a generally circular cage having three rollers provided therein. A first roller is fixed within the cage and has the blade mounting means secured through its diameter. The other two rollers are affixed to the cage in radial slots and are biased outwardly from the cage to allow the roller assembly to be rotated about the inner cam surface. In this fashion the roller cage assembly can be rotated within a cam having an other than round inside dimension.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be described in detail with reference to a preferred embodiment thereof, which is an ophthalmic cam-guided corneal trephine for performing a penetrating keratoplasty surgical operation. In the drawings:
FIG. 1 is a cross-sectional view of the cam-guided corneal trephine taken through section 1--1 of FIG. 2;
FIG. 2 is a top view of the cam-guided corneal trephine illustrated in FIG. 1;
FIG. 3 is a side view of the cam-guided corneal trephine illustrated in FIG. 1;
FIG. 4 is a top view of an other than round cam having a circular outer diameter and an annular or oval inside dimension; and
FIG. 5 is a top view of a totally round cam having both circular outer and inner diameters.
DETAILED DESCRIPTION OF THE INVENTION
The cam-guided corneal trephine according to the present invention is shown in FIGS. 1-5. Specifically referring to FIG. 1, the cam-guided corneal trephine 10 as shown includes a suction ring 12 for conforming and securing the patient's eye E and trephine 10, an annular base 14 integral with the suction ring 12, a course adjustment ring 16, an interchangeable cam 18, a roller cage assembly 20 and a blade mounting means 22 mounted within roller cage assembly 20 for rotational movement relative to the annular base 14 integral with the suction ring 12. A locking or retaining ring 24 is secured into the top of the adjustment ring 16 to secure the cam 18 and roller cage assembly 20 within the adjustment ring 16. The base 14 includes a pair of finger grips 26. In the device shown in the Figures, suction ring 12 and base 14 are connected by an outer cone 28, and elements 12, 14 and 28 are formed from a single integral piece. The blade mounting means 22 includes a moveable diamond tipped cutting blade 30 for cutting the corneal tissue.
The course adjustment ring 16 is provided with an external thread 32 which is received within a mating internal thread 34 provided in the annular base 14. The course adjustment ring 16 provides for a 6 millimeter (mm) adjustment of the blade mounting means 22 relative to the corneal surface of the eye E. The top surface of the adjustment ring 16 is provided with a plurality of number indicators 1 through 6 positioned about the periphery of the ring and the base is marked with a "V" as shown at 36 to provide a reference point for marking the position of the adjustment ring 16. The adjustment ring 16 is provided with a locking screw 38. The locking screw 38 is tipped with a nylon insert (not shown). When the course adjustment ring 16 is threaded into the base 14 such that the cutting blade 30 is positioned immediately adjacent the patient's cornea, the locking screw 38 is threaded through the ring 16 until the nylon tip is in contact with the external threads 32 of ring 16 to hold the ring in position relative to the annular base 14. In one embodiment of the invention by way of example and not to be construed in a limiting manner, the external thread 32 of ring 16 and internal thread 34 of base 14 are of a truncated metric thread design having a diameter of 47 mm and a pitch of 6.35.
The adjustment ring 16 is provided with an inner circular surface 40 and a bottom bearing surface 42. The interchangeable cam 18 as shown in FIGS. 4 and 5 is positioned within the adjustment ring 16. The outer generally circular surface 44 of the cam 18 is configured to fit snugly against the inner surface 40 and is supported on the bottom bearing surface 42 of ring 16. The cam 18 is further held in position within ring 16 by use of a set screw (not shown). The inner surface of the cam 18 can either be configured in either a generally circular or round shape as shown at 46 in FIG. 5 or an other than round shape as shown at 48 in FIGS. 2 and 4.
The roller cage assembly 20 includes a cylindrical cage member 52 for supporting the blade mounting means 22 for rotational movement within the annular base 14 and ring 16. The cage member 52 includes a top member 53 with three depending cylindrical side members 57 and a bottom member 55 which can be affixed to the depending side members 57 to form an integral cage member 52. The cage assembly is provided with three (3) rollers positioned about the periphery of cage member 52 at approximately 120° from one another. Two of the rollers 54 and 56 are spring loaded and are received in radial slots 58 and 60, respectively provided in top and bottom surfaces 53 and 55, respectively on cage member 52. The spring loaded rollers 54 and 56 are biased radially outwardly from the cage member 52 by springs 62 and 64, respectively. A third roller 66 is provided in a fixed position about the cage and is configured to receive the blade mounting means 22 through the center of its diameter. This blade roller 66 has a larger diameter than rollers 54 and 56 to provide the necessary clearance for receiving the blade holding means 22. The rollers 54 and 56 and blade roller 66 extend outside the periphery of cage 52 so that such rollers contact the inner cam surface 48 and bottom bearing ring surface 42, thereby allowing the roller cage assembly 20 to rotate freely within cam 18.
The roller cage assembly is held in place within the ring 16 by use of a locking ring 24 which is threadably received within the top portion of ring 16. The locking ring 24 is provided with two indentations 70 in its top surface which can receive a spanner tool (not shown) for installing and removing the locking ring 24 from the adjustment ring 16.
The blade mounting means 22 includes a body 74 having an externally threaded portion 76 extending up through a spacer member 78 provided in blade roller 66. The blade body 74 is secured to the roller cage 52 by an internally threaded collar 80 received on the externally threaded portion 76 of blade body 74. The threaded collar also has an externally threaded portion 82 on its upper end. An axially moveable center rod 84 is positioned within body 74 and has an externally threaded portion 86 at its uppermost or distal end from body 74 extending above the threaded collar 80. A blade holder 88 carrying the diamond tipped cutting blade 30 is positioned within body 74 and is secured to the lowermost or proximal end of center rod 84. A drive pin 90 is threaded through the body 74 and is received in a slot 92 provided in center rod 84 to prevent rotational movement of rod 84 while allowing for axial movement of rod 84 so that the cutting blade 30 can be raised and lowered relative to the roller cage assembly 20 and base 14.
A thimble 96 having a knurled outer surface 98 is threaded onto the externally threaded portions 82 and 86 of threaded collar 80 and center rod 84, respectively. The thimble 96 is provided with two internally threaded portions 100 and 102 for receiving such externally threaded portions 82 and 86, respectively. Such an arrangement has been called a "micrometer" thread or a "differential" thread arrangement to allow for precise axial movement of the center rod upon rotational movement of the thimble. The center rod 84 is prevented from being unscrewed from the thimble 96 by use of a retaining screw 104.
By way of example, the internal thread 100 of thimble 96 and the external thread 82 of collar 80 are a metric 5 mm diameter and having a pitch of 0.5. The internal thread 102 of thimble 96 and the external thread 86 of rod 84 are a metric 3.5 mm diameter and having a pitch of 0.6. Therefore, upon clockwise rotation of the roller cage assembly 20 within the trephine 10 but not allowing the thimble 96 itself to turn in the operator's fingers, the center rod 84 and consequently, the blade holder 88 and diamond tipped blade 30 will lowered by 0.096 mm per revolution of the roller cage assembly 20.
The blade mounting mechanism 22 is positioned through the roller cage assembly 20 on an angle to allow for maximum viewing by the surgeon through the center of the device. The blade holder 88 is angled with respect to the center rod 84 so as to present the cutting blade 30 in a vertical orientation to the corneal tissue E to be cut by the trephine. By way of the specific example above, the 0.096 mm of axial movement per revolution of the roller cage assembly 20 will translate into 0.1 mm movement of the blade 30 into the corneal tissue.
The roller cage assembly 20 freely rotates within cam 18 of trephine 10 on spring loaded rollers 54 and 56 and the blade roller 66. Since the spring loaded rollers are biased radially outwardly at all times, these rollers force the blade roller 66 to closely follow the inner surface 48 of cam 18. As is shown in FIGS. 4 and 5, it is possible for the inner cam surface to be of various diameter round configurations as shown at 46 in FIG. 4 or to be of an other than round or possibly oval configuration as shown at 48 in FIGS. 2 and 5. In this fashion the blade mounting means 22 and cutting blade 30 will closely follow the geometric pattern provided on the inside surface of cam 18.
Suction ring 12 of trephine 10 functions by virtue of the void space left between inner and outer suction rings 108 and 110, which void space communicates with a tube 112 adapted to be connected to a source of suction. Suction ring 12 may be identical to the one provided in the cutting device disclosed in the aforementioned U.S. Pat. No. 4,423,728, and accordingly may have a frustoconical shape with a constant height throughout. It is also contemplated that the suction ring may be slightly tilted in such a way that its height varies between maximum and minimum values at about 180° opposed locations in order to compensate for the variation in corneal thickness between the inferior (minimum corneal thickness) and superior (maximum corneal thickness) cornea.
The various included pieces and parts of which trephine 10 is comprised may be prepared by conventional methods, for example casting, machining, etc., from a suitable metal or metal alloy (e.g. stainless steel). Alternatively, injection molded plastic pieces and parts may be utilized in a disposable embodiment of the invention.
The operation of trephine 10 will be described with reference to an ophthalmic surgical procedure for removing a piece of corneal tissue in contemplation of a corneal transplant operation. First, the surgeon or operator would grasp the trephine 10 by finger grips 26 and place the suction ring upon the corneal surface E of the eye. An appropriate suction would be applied to suction ring 12 to secure the trephine 10 to the corneal surface. To start an incision, the operator would first rotate the thimble 96 clockwise to its lowest position which would raise the cutting blade 30 to its fully up position. Then, by rotation of course adjustment ring 16, the operator would lower the blade mounting means 22 and diamond tipped blade 30 to a position immediately adjacent to the corneal tissue E. The locking screw 38 would then be secured to prevent further rotation of the adjusting ring 16.
The operator would then grasp the thimble 96 firmly within the fingers of his or her other hand and rotate the roller cage assembly 20 in a clockwise direction about the annular base 14 without allowing the thimble 96 to rotate. Consequently, the blade 30 would be lowered into the corneal tissue 0.1 mm per revolution of the roller cage assembly 20 until the corneal tissue E has been completely dissected. In this manner, the cutting blade 30 of the trephine 10 provides a continuous cutting action of the tissue providing a smooth annular hole therein. To raise the cutting blade 96, the operator would rotate thimble 30 clockwise while holding the roller cage assembly 20 still until the thimble 96 is screwed back down against the roller cage member 52 which would raise the blade 30 back to its original position.
To change from one interchangeable cam 18 to another, the operator would unscrew the locking ring 24 with spanner wrench (not shown). The roller cage assembly 20 would then be removed from the course adjustment ring 16 and set aside. The adjustment ring 16 would then be removed from the annular base 14. The retaining screw (not shown) in the side of ring 16 would be loosened and cam 18 would be removed from the ring 16. A different cam having a different inside dimension could be put back into the ring 16 and the steps outlined above reversed to place the trephine 10 back in working condition.
Thus, the cam-guided trephine in accordance with the present invention provides a technique for allowing a vertically disposed blade 30 to provide an annular cut of essentially any practical shape, diameter and depth. However, it should be noted that while a vertical blade 30 has been shown in use, it would be equally possible to utilize an angled blade to be used in its place. And, although the trephine in accordance with the present invention is disclosed for use in a procedure for a corneal keratoplasty operation, it will be readily apparent to those skilled in the art that other surgical procedures may be performed by the present invention as well.
Although the present invention has been described with respect to a specific embodiment of the apparatus, it is also readily, apparent that modifications, alterations, or changes may be made without departing from the spirit and scope of the invention as defined by the following claims. | A cam guided corneal trephine for selectively cutting a portion of an eye is provided herein. The cam-guided corneal trephine comprises a base, a coarse adjusting ring, interchangeable annular ring, interchangeable annular cams operatively supported by the adjusting ring, the annular cams having various inner round diameters or other than round dimensions, and a roller cage assembly adapted to be disposed and rotated within the annular cam, the roller cage assembly having a blade mounting means disposed therein for providing a continuous cut of the corneal tissue corresponding to the inner shape of the selected cam upon rotation of the roller cage assembly. | 0 |
BACKGROUND OF THE INVENTION
The invention relates to an x-ray examination apparatus comprising a parallelogram type arm whose one end is mounted by a bearing and whose other end bears, via a support-mounting, an x-ray tube with a radiation diaphragm, wherein the parallelogram arm is rotatable about a vertical axis and can be moved in a vertical direction such that the central ray of the x-ray tube retains its direction.
An x-ray examination apparatus of this type is known from the brochure "Nanomobil 2i" of the Siemens firm. This apparatus, which is a mobile x-ray apparatus, is e.g. transported to a patient resting on an examination table for an x-ray photograph. An x-ray cassette is pushed beneath the patient. The parallelogram arm with the x-ray tube is rotated in such a manner that the diaphragmed-in radiation field covers the cassette. When the cassette is brought into another position along the table beneath the patient for an additional photographic exposure, the parallelogram arm must be rotated, and the x-ray tube must be newly adjusted so that the collimated radiation field again coincides with the cassette.
SUMMARY OF THE INVENTION
The object underlying the invention consists in producing an x-ray examination apparatus wherein the adjustment of the x-ray tube, as compared with the known apparatus, is simplified, wherein particularly the x-ray tube can be readily adjusted to a new cassette position when the cassette position is changed in the longitudinal direction of the patient.
In accordance with the invention, this object is achieved by virtue of the fact that guidance means are arranged in the parallelogram arm between the rotary bearing and the x-ray tube support-mounting which, pursuant to turning the parallelogram arm about the vertical axis, displace the x-ray tube in such a manner that the sides of the field collimated by means of the radiation diaphragm undergo parallel-displacement. If the x-ray tube with the diaphragm has once been adjusted to a cassette position, it can be adjusted by means of a simple rotating of the parallelogram arm to a new cassette position at another location of the patient, because the edge positions of the cassette in the different cassette positions in the case of a patient, as a rule, run parallel to one another.
Further details of the invention shall be apparent from the sub-claims.
The invention shall be explained in further detail in the following on the basis of the sample embodiment illustrated in the accompanying sheets of drawings; and other objects, features and advantages will be apparent from this detailed disclosure and from the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a mobile x-ray examination apparatus in accordance with the invention;
FIG. 2 shows a schematic illustration of the x-ray examination apparatus according to FIG. 1 from above; and
FIG. 3 illustrates the carrier arm of the x-ray tube in the apparatus according to FIG. 1.
DETAILED DESCRIPTION
FIG. 1 illustrates a carriage which is provided with four wheels, of which only two wheels 2, 3 are visible. Rear wheel 2 and the opposite, non-visible rear wheel are steerable. On the upper side of wagon 1 there is arranged a rotatably mounted carrier arm 4 whose free end is connected in an articulated (or hinged) fashion with a second carrier arm 5 by means of a pivot shaft 6. Carrier arm 5 bears at its free end a housing 8 containing an x-ray tube 8a with a primary radiation diaphragm 8b. The high voltage generator (single-tank generator) is also disposed in housing 8, whereas the switching and control elements are arranged on carriage 1 in and on its housing.
Carriage 1 has a stage 9 at which the upper side of the carriage 1 rises obliquely in an upward direction and forms an operating panel 10 for the adjustment of the photographic exposure parameters. Carriage 1, in addition, manifests at its upper side a region 7 for receiving housing 8 in a parking position, the region 7 providing a recess into which housing 8 fits, as indicated by the position of parts 5 and 8 illustrated in broken lines. On the one end face 11 of carriage 1, a recess 12 is present in the carriage housing from which recess a steering bar 13 with a handle 14 projects which serves the purpose of steering the motor-driven wheels. There is arranged on handle 14 a non-illustrated operating button for the purpose of switching on and off the motor-driven wheels. The steering bar 13 is pivotally mounted about an axis 15 and can be folded into the recess 12.
In order to transport the x-ray apparatus, housing 8 is pushed into the illustrated parking position such that the x-ray tube, the radiation diaphragm, and the high voltage generator present in housing 8 are protected against inadvertent impact. For an x-ray photograph, housing 8, as shall be described in greater detail in conjunction with FIGS. 2 and 3, can be freely adjusted by means of two handles 4a, 5a, on arms 4, 5. By means of an equilibration (or weight-compensation) device, the weight of arms 4, 5 and of housing 8 with its components is compensated.
FIG. 2 illustrates by a diagrammatic top plan view that the housing 8 with x-ray tube 8a can be adjusted at a specified angle α in relation to carrier arms 4, 5. When carrier arms 4, 5 are rotated about a vertical axis 16, e.g. into the position indicated by broken lines, housing 8 with x-ray tube 8a is displaced by means to be described in greater detail in reference to FIG. 3 in such a fashion that the sides of the field 17, collimated by means of the radiation diaphragm 8b, become parallel-displaced. In the case of a parallel-displacement of a cassette disposed beneath a patient, housing 8 with the x-ray tube 8a and the radiation diaphragm 8b do not need to be reset during the subsequent rotation of the carrier arms 4, 5.
FIG. 3 illustrates that, in the interior of the carrier arms 4, 5, which have a closed construction, a double parallelogram arm is present whose one end is mounted by means of a hollow-cylindrical bearing 18, and whose other end bears, via a support-mounting 19, the housing 8 (not illustrated in FIG. 3) with the x-ray tube 8a and the radiation diaphragm 8b. The bearing 18 is mounted in the carriage 1 schematically illustrated in FIG. 3.
Two upwardly directed lugs, 20, 21 are mounted on the upwardly-directed frontal face of bearing 18, said lugs being disposed opposite one another at the periphery, and between which a shaft 22 is rotatably mounted. In addition, there is rotatably mounted on each extension 20, 21, one of the two arms 23, 24, arranged so as to be mutually parallel, respectively. The arms 23, 24, are connected in an articulated (or hinged) fashion with the shaft 22. Shaft 6 is rotatably mounted on the free ends of arms 23, 24. Two additional arms 25, 26 are rotatably mounted on shaft 6, and have free ends at which an additional shaft 27 is rotatably mounted. In addition, a downwardly directed bracket arm 28 is rotatably arranged on shaft 27. Bracket arm 28 manifests an upwardly-directed extension 29 which is connected, via a rod 30, with an angle-shaped part 31 fixedly arranged on shaft 6. Part 31, moreover, is connected in an articulated fashion via a rod 32 with the lug 20.
The support-mounting 19 for the housing 8 is pivotally mounted by means of a shaft 33, vertically arranged on bracket arm 28, on which shaft 33 a gear wheel 34 is mounted which engages with an additional gear wheel 35. Gear wheel 35 is mounted on shaft 27 and, together with gear wheel 34, forms a bevel gear drive arrangement. Gear wheel 35 manifests an extension 36 which, via a rod 37, is connected in an articulated fashion with an additional angle-shaped part 38 mounted on shaft 6. Part 38, moreover, is connected via an additional rod 39 with one end of an arm 40 mounted on shaft 22. The other end of arm 40 is connected in an articulated fashion via a rod 41, with an extension 42 of a gear wheel 43, arranged in bearing 18, which gear wheel 43 is attached to a shaft 44 rotatably mounted in the bearing.
Gear wheel 43 is in engagement with a gear wheel 45 which is mounted on a vertical shaft 46 which projects downwardly through bearing 18 and is rotatably mounted on carriage 1. Gear wheels 43 and 45 likewise form a bevel gear drive arrangement. There is attached to shaft 46 a plate (or disc) 47 at the periphery of which a stopping device 48, which is mounted on carriage 1, engages.
Thus, plate 47 is capable of being arrested in relation to the carriage. There is secured to gear wheel 43 a flange 49 at the periphery of which a stopping device 50, which is mounted in bearing 18, engages. Flange 49 is capable of being arrested in relation to the bearing 18.
The double-parallelogram arm can be moved in a vertical direction such that the central ray of the x-ray tube is parallel-displaced. The distance of the focus from the x-ray film can thereby be adjusted. The housing 8 with the x-ray tube, which is secured to a holder 51, connected in an articulated (or hinged) fashion with the support-mounting 19, is adjusted in such a fashion that the central ray of the x-ray tube impinges in the center of the cassette at a right angle (or perpendicular) to the latter. When the position of the central ray has been adjusted, the angle between the support-mounting 19 and the holder 51 and hence the position of the central ray can be fixed by means of an arresting device 52. In the case of a height-displacement of housing 8, bracket arm 28 is rotated such that the central ray, in every angular position of arms 25, 26, always impinges vertically on the cassette.
The double-parallelogram arm can also be horizontally displaced about a vertical axis 53. First, the housing 8 with the x-ray tube must be adjusted in relation to the cassette such that the collimated field of the radiation diaphragm covers the cassette and its edges coincide with the cassette edges. This proceeds by means of rotating housing 8 about shaft 33 when arresting devices 48, 50 are released. In so doing, the bevel gearing 34, 35 rotates such that disc 47 is rotated via the drive transmission elements 36, 37, 38, 39, 40, 41, 42, 43, 45, and 46, which form guidance means. Upon reaching the desired housing position, plate 47 is arrested by means of arresting device 48, which is an electrically energized magnetic brake, through actuation of an operating button arranged e.g. on handle 5a (FIG. 1). Pursuant to rotating the parallelogram arm in a horizontal direction, bearing 18 in carriage 1 rotates such that gear wheel 43 is rotated about the arrested gear wheel 45, and rotation of gear wheel 43 moves the guide means in the transmission sequence 42, 41, 40, 39, 38, 37, 36, 35, and 34, and rotates shaft 33 as well as support-mounting 19 in such a manner that the support-mounting 19 with housing 8 describes a parallel movement as illustrated in FIG. 2. When the desired position of housing 8 with the x-ray tube and the radiation diaphragm has been obtained, the parallelogram arm is arrested by means of the arresting device 50 engaging on the flange 49 of gear wheel 43. This device 50 is likewise an electrically energized magnetic brake and can e.g. also be actuated by means of an operating button arranged on handle 5a (FIG. 1).
It will be apparent that many modifications and variations may be effected without departing from the scope of the novel concepts and teachings of the present invention. | A parallelogram arm adjustably supports the x-ray source and has one end in a rotary bearing at the carriage, the other end carrying an x-ray tube with a radiation diaphragm. The parallelogram arm can be turned about a vertical axis by means of the rotary bearing, and can be moved in a vertical direction, while the central ray of the x-ray tube retains its direction.In the parallelogram arm between the rotary bearing and the x-ray tube support-mounting, a guide mechanism is arranged which displaces the x-ray tube, pursuant to rotating the parallelogram arm about the vertical axis, such that the sides of the field collimated by means of the radiation diaphragm are parallel-displaced. | 0 |
Subsets and Splits
No community queries yet
The top public SQL queries from the community will appear here once available.